CN110203977A - A kind of preparation method of the basic nickel carbonate containing sodium - Google Patents
A kind of preparation method of the basic nickel carbonate containing sodium Download PDFInfo
- Publication number
- CN110203977A CN110203977A CN201810167145.9A CN201810167145A CN110203977A CN 110203977 A CN110203977 A CN 110203977A CN 201810167145 A CN201810167145 A CN 201810167145A CN 110203977 A CN110203977 A CN 110203977A
- Authority
- CN
- China
- Prior art keywords
- sodium
- nickel
- basic nickel
- carbonate
- containing sodium
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/20—Carbon compounds
- B01J27/232—Carbonates
- B01J27/236—Hydroxy carbonates
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/50—Solid solutions
- C01P2002/52—Solid solutions containing elements as dopants
- C01P2002/54—Solid solutions containing elements as dopants one element only
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
The invention discloses a kind of preparation methods of basic nickel carbonate containing sodium, sodium carbonate liquor and nickel sulfate solution are added in reactor this method simultaneously, the pH value for passing through the flow control system for adjusting sodium carbonate liquor and nickel sulfate solution in fill process is 8.2~8.8, and reaction obtains basic nickel carbonate；Stop charging, adjusts reaction temperature, the formation of control hydration carbon nickel sodium crystal seed；Reaction after a certain period of time, is fed, and the pH value and reaction temperature of control system again, promotes nucleus growth, obtains the basic nickel carbonate containing sodium；The present invention in the synthesis process, by control feed time, the pH value of reaction system, reaction temperature and reaction time, makes basic carbonate nickel surface form the crystal seed of hydration carbon sodium nickel, and control crystal seed and grow up, obtains the basic nickel carbonate containing sodium；The present invention synthesizes a kind of can stablize and provides the catalyst precursor of sodium content 2~5%.
Description
Technical field
The invention belongs to a kind of industrialized process for preparing of subcarbonate, and in particular to a kind of alkali formula carbon containing sodium
The preparation method of sour nickel.
Background technique
Subcarbonate can be applied to photocatalysis, supercapacitor and secondary cell field；Nickel, cobalt subcarbonate exist
Electrode material, catalyst, electronic material, magnetic material the fields such as additive there is important application.
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；In addition, basic nickel carbonate is also widely used in plating, electroforming, enamel pigment and industry
Catalyst industry etc..
In the prior art, sodium is free of in the subcarbonate usually prepared, and for some special reactions, in reaction process
In, catalyst provide sodium ion to catalysis reaction in electronics transfer have preferable facilitation, still, existing catalyst
In sodium ion be to be adsorbed on plane of crystal, the stability of such sodium ion and crystal combination is poor, be difficult control alkali formula carbon
The content for the sodium ion that phosphate catalyst provides, so that it is difficult to control the stability of the offer sodium content in subcarbonate, from
And influence the catalytic performance of subcarbonate.
Summary of the invention
For overcome the deficiencies in the prior art, the purpose of the present invention is intended to provide a kind of preparation of basic nickel carbonate containing sodium
Method.
The present invention also provides a kind of preparation method of basic nickel carbonate containing sodium, method is implemented by following steps:
Step 1, sodium carbonate liquor and nickel sulfate solution are added in reactor simultaneously, by adjusting carbonic acid in fill process
The pH value of the flow control system of sodium solution and nickel sulfate solution is 8.2~8.3, and reaction obtains basic nickel carbonate；
Step 2, stop that the sodium carbonate liquor and the nickel sulfate solution is added to reactor, by adjusting reaction temperature
The basic nickel carbonate crystal phase transition that the step 1 obtains is controlled, hydration carbon nickel sodium crystal seed is obtained；
Step 3, the sodium carbonate liquor and the nickel sulfate solution is added to reactor again, passes through tune in fill process
The pH value of the flow control system of sodium carbonate liquor and nickel sulfate solution is saved, and controls the step by adjusting reaction temperature
The 2 hydration carbon nickel sodium crystal seed growths obtained, obtain the basic nickel carbonate crude product containing sodium；
Step 4, the basic nickel carbonate crude product containing the sodium step 3 obtained be successively aged, washed, being dried and
Screening obtains the basic nickel carbonate containing sodium.
In above scheme, the concentration of step 1 sodium carbonate liquor is 180~300g/L, and nickel sulfate is molten in the step 1
The concentration of liquid is 60~100g/L.
In above scheme, the flow of sodium carbonate liquor described in fill process is 100~1000L/h, institute in the step 1
The flow for stating nickel sulfate solution is 100~1000L/h.
In above scheme, the reaction temperature in the step 1 is 60~90 DEG C, 20~25h of reaction time.
In above scheme, the reaction temperature in the step 2 is 50~60 DEG C, 30~60min of reaction time.
In above scheme, the pH value of system is controlled 8.5~8.8 in the step 3.
In above scheme, the reaction temperature in the step 3 is 50~60 DEG C, 11~30h of reaction time.
In above scheme, the digestion time in the step 4 is 0.5~3h.
In above scheme, the washing in the step 4 uses pure water, and the temperature of the pure water is 70~85 DEG C, institute
State conductivity≤100 μ s/m of pure water.
In above scheme, the temperature of the drying in the step 4 is 95~105 DEG C, the time of the drying is 2~
3h；The screening in the step 4 uses 200~400 meshes.
Compared with prior art, the invention proposes a kind of preparation method of basic nickel carbonate containing sodium, this method is by carbon
Acid sodium solution and nickel sulfate solution are added in reactor simultaneously, by adjusting sodium carbonate liquor and nickel sulfate solution in fill process
Flow control system pH value be 8.2~8.3, reaction obtain basic nickel carbonate；Stop charging, adjusts reaction temperature, control
It is hydrated the formation of carbon nickel sodium crystal seed；Reaction after a certain period of time, is fed, and the pH value and reaction temperature of control system again, is promoted
Nucleus growth obtains the basic nickel carbonate containing sodium；The present invention in the synthesis process, passes through control feed time, reaction system
PH value, reaction temperature and reaction time make basic carbonate nickel surface form the crystal seed of hydration carbon sodium nickel, and it is long to control crystal seed
Greatly, the basic nickel carbonate containing sodium is obtained；Sodium ion is being embedded in basic nickel carbonate in the basic nickel carbonate containing sodium that the present invention synthesizes
On crystal face, sodium content according to crystal seed amount can stability Calculation to obtain can stablize provide sodium content 2~5% catalyst before
Body is driven, the electronics transfer in catalyst reaction can be effectively facilitated.
Detailed description of the invention
Fig. 1 is a kind of process flow chart of the preparation method of the basic nickel carbonate containing sodium provided in an embodiment of the present invention；
Fig. 2 is a kind of X-ray diffractogram for basic nickel carbonate containing sodium that the embodiment of the present invention 1 provides；
Fig. 3 is a kind of scanning electron microscope (SEM) photograph for basic nickel carbonate containing sodium that the embodiment of the present invention 1 provides.
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, with reference to embodiments, to the present invention
It is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, it is not used to
Limit the present invention.
The embodiment of the present invention provides a kind of preparation method of basic nickel carbonate, process flow chart, as shown in Figure 1, its side
Method is implemented by following steps:
Step 1, by concentration be 180~300g/L sodium carbonate liquor and concentration be 60~100g/L nickel sulfate solution it is same
When be added reactor in, in fill process adjust sodium carbonate liquor flow be 100~1000L/h, nickel sulfate solution flow
For 100~1000L/h, so that the pH value of control system is 8.2~8.3, and 20~25h is reacted at 60~90 DEG C, obtained
Basic nickel carbonate；
Step 2, stop that sodium carbonate liquor and nickel sulfate solution is added to reactor, the basic nickel carbonate for obtaining step 1
30~60min is reacted at 50~60 DEG C, stopping feeding again after reacting leads to surface energy variation, obtains hydration carbon nickel
Sodium crystal seed；
Step 3, sodium carbonate liquor and nickel sulfate solution are added to reactor again, the pH value of control system is 8.5~
8.8, so that hydration carbon nickel sodium crystal seed is reacted 11~30h at 50~60 DEG C, promote nucleus growth, obtains the basic nickel carbonate containing sodium
Crude product；
Step 4, the basic nickel carbonate crude product containing sodium step 3 obtained is successively aged 0.5~3h, then uses conductivity
≤ 100 μ s/m, temperature are that 70~85 DEG C of pure water is washed, then 2~3h is dried at 95~105 DEG C, finally using 200~
The screening of 400 meshes, obtains the basic nickel carbonate containing sodium.
The present invention in the synthesis process, by control feed time, the pH value of reaction system, reaction temperature and reaction when
Between, in such a way that step 2 stops charging, the surface energy of basic nickel carbonate is reduced, is conducive to alkali formula carbon the reaction was continued
The structure of sour nickel is changed into the structure of hydration carbon sodium nickel, to obtain the crystal seed of hydration carbon sodium nickel, also, the present invention containing of synthesizing
Sodium ion is on being embedded in basic nickel carbonate crystal face in sodium basic nickel carbonate, sodium content according to crystal seed amount can stability Calculation to
It obtains to stablize and the catalyst precursor of sodium content 2~5% is provided, the electronics that can be effectively facilitated in catalyst reaction turns
It moves.
Embodiment 1
The embodiment of the present invention 1 provides a kind of preparation method of basic nickel carbonate containing sodium, and method passes through following steps reality
It applies:
Step 1, by concentration be 180g/L sodium carbonate liquor and concentration be 60g/L nickel sulfate solution and meanwhile reaction is added
In device, the flow that sodium carbonate liquor is adjusted in fill process is 100~1000L/h, the flow of nickel sulfate solution be 100~
1000L/h so that the pH value of control system is 8.2, and reacts 25h at 60 DEG C, obtains basic nickel carbonate；
Step 2, stop that sodium carbonate liquor and nickel sulfate solution is added to reactor, the basic nickel carbonate for obtaining step 1
45min is reacted at 55 DEG C, stopping feeding again after reacting leads to surface energy variation, obtains hydration carbon nickel sodium crystal seed；
Step 3, sodium carbonate liquor and nickel sulfate solution is added to reactor again, the pH value of control system is 8.6, makes water
It closes carbon nickel sodium crystal seed and reacts 25h at 55 DEG C, promote nucleus growth, obtain the basic nickel carbonate crude product containing sodium；
Step 4, the basic nickel carbonate crude product containing sodium step 3 obtained is successively aged 1.5h, then using conductivity≤
100 μ s/m, the pure water that temperature is 80 DEG C are washed, then dry 2h at 100 DEG C, are finally sieved using 200~400 meshes,
Obtain the basic nickel carbonate containing sodium.
The X-ray diffractogram and scanning electron microscope (SEM) photograph for a kind of basic nickel carbonate containing sodium that the embodiment of the present invention 1 provides such as are schemed
Shown in 2 and 3, which is NaNi4(CO3)3(OH)3·3H2O, it can be seen that with the prior art
It compares, the basic nickel carbonate containing sodium obtained using above-mentioned synthesis technology, sodium content 2.6%.
Embodiment 2
The embodiment of the present invention 2 provides a kind of preparation method of basic nickel carbonate containing sodium, and method passes through following steps reality
It applies:
Step 1, by concentration be 180g/L sodium carbonate liquor and concentration be 60g/L nickel sulfate solution and meanwhile reaction is added
In device, the flow that sodium carbonate liquor is adjusted in fill process is 100~1000L/h, the flow of nickel sulfate solution be 100~
1000L/h so that the pH value of control system is 8.3, and reacts 22h at 75 DEG C, obtains basic nickel carbonate；
Step 2, stop that sodium carbonate liquor and nickel sulfate solution is added to reactor, the basic nickel carbonate for obtaining step 1
45min is reacted at 55 DEG C, stopping feeding again after reacting leads to surface energy variation, obtains hydration carbon nickel sodium crystal seed；
Step 3, sodium carbonate liquor and nickel sulfate solution is added to reactor again, the pH value of control system is 8.6, makes water
It closes carbon nickel sodium crystal seed and reacts 25h at 55 DEG C, promote nucleus growth, obtain the basic nickel carbonate crude product containing sodium；
Step 4, the basic nickel carbonate crude product containing sodium step 3 obtained is successively aged 1.5h, then using conductivity≤
100 μ s/m, the pure water that temperature is 80 DEG C are washed, then dry 2h at 100 DEG C, are finally sieved using 200~400 meshes,
Obtain the basic nickel carbonate containing sodium.
Compared with prior art, the basic nickel carbonate containing sodium obtained using above-mentioned synthesis technology, sodium content 2.7%.
Embodiment 3
The embodiment of the present invention 3 provides a kind of preparation method of basic nickel carbonate containing sodium, and method passes through following steps reality
It applies:
Step 1, by concentration be 180g/L sodium carbonate liquor and concentration be 60g/L nickel sulfate solution and meanwhile reaction is added
In device, the flow that sodium carbonate liquor is adjusted in fill process is 100~1000L/h, the flow of nickel sulfate solution be 100~
1000L/h so that the pH value of control system is 8.3, and reacts 20h at 90 DEG C, obtains basic nickel carbonate；
Step 2, stop that sodium carbonate liquor and nickel sulfate solution is added to reactor, the basic nickel carbonate for obtaining step 1
45min is reacted at 55 DEG C, stopping feeding again after reacting leads to surface energy variation, obtains hydration carbon nickel sodium crystal seed；
Step 3, sodium carbonate liquor and nickel sulfate solution is added to reactor again, the pH value of control system is 8.6, makes water
It closes carbon nickel sodium crystal seed and reacts 25h at 55 DEG C, promote nucleus growth, obtain the basic nickel carbonate crude product containing sodium；
Step 4, the basic nickel carbonate crude product containing sodium step 3 obtained is successively aged 1.5h, then using conductivity≤
100 μ s/m, the pure water that temperature is 80 DEG C are washed, then dry 2h at 100 DEG C, are finally sieved using 200~400 meshes,
Obtain the basic nickel carbonate containing sodium.
Compared with prior art, the basic nickel carbonate containing sodium obtained using above-mentioned synthesis technology, sodium content 2.74%.
Embodiment 4
The embodiment of the present invention 4 provides a kind of preparation method of basic nickel carbonate containing sodium, and method passes through following steps reality
It applies:
Step 1, by concentration be 200g/L sodium carbonate liquor and concentration be 80g/L nickel sulfate solution and meanwhile reaction is added
In device, the flow that sodium carbonate liquor is adjusted in fill process is 100~1000L/h, the flow of nickel sulfate solution be 100~
1000L/h so that the pH value of control system is 8.3, and reacts 20h at 60 DEG C, obtains basic nickel carbonate；
Step 2, stop that sodium carbonate liquor and nickel sulfate solution is added to reactor, the basic nickel carbonate for obtaining step 1
60min is reacted at 50 DEG C, stopping feeding again after reacting leads to surface energy variation, obtains hydration carbon nickel sodium crystal seed；
Step 3, sodium carbonate liquor and nickel sulfate solution is added to reactor again, the pH value of control system is 8.6, makes water
It closes carbon nickel sodium crystal seed and reacts 28h at 50 DEG C, promote nucleus growth, obtain the basic nickel carbonate crude product containing sodium；
Step 4, the basic nickel carbonate crude product containing sodium step 3 obtained is successively aged 1.5h, then using conductivity≤
100 μ s/m, the pure water that temperature is 80 DEG C are washed, then dry 2h at 100 DEG C, are finally sieved using 200~400 meshes,
Obtain the basic nickel carbonate containing sodium.
Compared with prior art, the basic nickel carbonate containing sodium obtained using above-mentioned synthesis technology, sodium content 3.5%.
Embodiment 5
The embodiment of the present invention 5 provides a kind of preparation method of basic nickel carbonate containing sodium, and method passes through following steps reality
It applies:
Step 1, by concentration be 200g/L sodium carbonate liquor and concentration be 80g/L nickel sulfate solution and meanwhile reaction is added
In device, the flow that sodium carbonate liquor is adjusted in fill process is 100~1000L/h, the flow of nickel sulfate solution be 100~
1000L/h so that the pH value of control system is 8.3, and reacts 20h at 60 DEG C, obtains basic nickel carbonate；
Step 2, stop that sodium carbonate liquor and nickel sulfate solution is added to reactor, the basic nickel carbonate for obtaining step 1
45min is reacted at 55 DEG C, stopping feeding again after reacting leads to surface energy variation, obtains hydration carbon nickel sodium crystal seed；
Step 3, sodium carbonate liquor and nickel sulfate solution is added to reactor again, the pH value of control system is 8.6, makes water
It closes carbon nickel sodium crystal seed and reacts 20h at 55 DEG C, promote nucleus growth, obtain the basic nickel carbonate crude product containing sodium；
Step 4, the basic nickel carbonate crude product containing sodium step 3 obtained is successively aged 1.5h, then using conductivity≤
100 μ s/m, the pure water that temperature is 80 DEG C are washed, then dry 2h at 100 DEG C, are finally sieved using 200~400 meshes,
Obtain the basic nickel carbonate containing sodium.
Compared with prior art, the basic nickel carbonate containing sodium obtained using above-mentioned synthesis technology, sodium content 3.2%.
Embodiment 6
The embodiment of the present invention 6 provides a kind of preparation method of basic nickel carbonate containing sodium, and method passes through following steps reality
It applies:
Step 1, by concentration be 200g/L sodium carbonate liquor and concentration be 80g/L nickel sulfate solution and meanwhile reaction is added
In device, the flow that sodium carbonate liquor is adjusted in fill process is 100~1000L/h, the flow of nickel sulfate solution be 100~
1000L/h so that the pH value of control system is 8.3, and reacts 20h at 60 DEG C, obtains basic nickel carbonate；
Step 2, stop that sodium carbonate liquor and nickel sulfate solution is added to reactor, the basic nickel carbonate for obtaining step 1
30min is reacted at 60 DEG C, stopping feeding again after reacting leads to surface energy variation, obtains hydration carbon nickel sodium crystal seed；
Step 3, sodium carbonate liquor and nickel sulfate solution is added to reactor again, the pH value of control system is 8.6, makes water
It closes carbon nickel sodium crystal seed and reacts 11h at 60 DEG C, promote nucleus growth, obtain the basic nickel carbonate crude product containing sodium；
Step 4, the basic nickel carbonate crude product containing sodium step 3 obtained is successively aged 1.5h, then using conductivity≤
100 μ s/m, the pure water that temperature is 80 DEG C are washed, then dry 2h at 100 DEG C, are finally sieved using 200~400 meshes,
Obtain the basic nickel carbonate containing sodium.
Compared with prior art, the basic nickel carbonate containing sodium obtained using above-mentioned synthesis technology, sodium content 3.52%.
Embodiment 7
The embodiment of the present invention 7 provides a kind of preparation method of basic nickel carbonate containing sodium, and method passes through following steps reality
It applies:
Step 1, by concentration be 300g/L sodium carbonate liquor and concentration be 100g/L nickel sulfate solution and meanwhile be added anti-
Answer in device, the flow that sodium carbonate liquor is adjusted in fill process is 100~1000L/h, the flow of nickel sulfate solution be 100~
1000L/h so that the pH value of control system is 8.2, and reacts 20h at 80 DEG C, obtains basic nickel carbonate；
Step 2, stop that sodium carbonate liquor and nickel sulfate solution is added to reactor, the basic nickel carbonate for obtaining step 1
60min is reacted at 50 DEG C, stopping feeding again after reacting leads to surface energy variation, obtains hydration carbon nickel sodium crystal seed；
Step 3, sodium carbonate liquor and nickel sulfate solution is added to reactor again, the pH value of control system is 8.6, makes water
It closes carbon nickel sodium crystal seed and reacts 25h at 50 DEG C, promote nucleus growth, obtain the basic nickel carbonate crude product containing sodium；
Step 4, the basic nickel carbonate crude product containing sodium step 3 obtained is successively aged 0.5h, then using conductivity≤
100 μ s/m, the pure water that temperature is 70 DEG C are washed, then dry 3h at 95 DEG C, are finally sieved, are obtained using 200~400 meshes
The basic nickel carbonate of sodium must be contained.
Compared with prior art, the basic nickel carbonate containing sodium obtained using above-mentioned synthesis technology, sodium content 4.9%.
Embodiment 8
The embodiment of the present invention 8 provides a kind of preparation method of basic nickel carbonate containing sodium, and method passes through following steps reality
It applies:
Step 1, by concentration be 300g/L sodium carbonate liquor and concentration be 100g/L nickel sulfate solution and meanwhile be added anti-
Answer in device, the flow that sodium carbonate liquor is adjusted in fill process is 100~1000L/h, the flow of nickel sulfate solution be 100~
1000L/h so that the pH value of control system is 8.2, and reacts 20h at 80 DEG C, obtains basic nickel carbonate；
Step 2, stop that sodium carbonate liquor and nickel sulfate solution is added to reactor, the basic nickel carbonate for obtaining step 1
60min is reacted at 50 DEG C, stopping feeding again after reacting leads to surface energy variation, obtains hydration carbon nickel sodium crystal seed；
Step 3, sodium carbonate liquor and nickel sulfate solution is added to reactor again, the pH value of control system is 8.6, makes water
It closes carbon nickel sodium crystal seed and reacts 25h at 50 DEG C, promote nucleus growth, obtain the basic nickel carbonate crude product containing sodium；
Step 4, the basic nickel carbonate crude product containing sodium step 3 obtained is successively aged 2h, then uses conductivity≤100
μ s/m, the pure water that temperature is 80 DEG C are washed, then dry 3h at 100 DEG C, are finally sieved, are obtained using 200~400 meshes
Basic nickel carbonate containing sodium.
Compared with prior art, the basic nickel carbonate containing sodium obtained using above-mentioned synthesis technology, sodium content 5.0%.
Embodiment 9
The embodiment of the present invention 9 provides a kind of preparation method of basic nickel carbonate containing sodium, and method passes through following steps reality
It applies:
Step 1, by concentration be 300g/L sodium carbonate liquor and concentration be 100g/L nickel sulfate solution and meanwhile be added anti-
Answer in device, the flow that sodium carbonate liquor is adjusted in fill process is 100~1000L/h, the flow of nickel sulfate solution be 100~
1000L/h so that the pH value of control system is 8.2, and reacts 20h at 80 DEG C, obtains basic nickel carbonate；
Step 2, stop that sodium carbonate liquor and nickel sulfate solution is added to reactor, the basic nickel carbonate for obtaining step 1
60min is reacted at 50 DEG C, stopping feeding again after reacting leads to surface energy variation, obtains hydration carbon nickel sodium crystal seed；
Step 3, sodium carbonate liquor and nickel sulfate solution is added to reactor again, the pH value of control system is 8.6, makes water
It closes carbon nickel sodium crystal seed and reacts 25h at 50 DEG C, promote nucleus growth, obtain the basic nickel carbonate crude product containing sodium；
Step 4, the basic nickel carbonate crude product containing sodium step 3 obtained is successively aged 3h, then uses conductivity≤100
μ s/m, the pure water that temperature is 85 DEG C are washed, then dry 2h at 105 DEG C, are finally sieved, are obtained using 200~400 meshes
Basic nickel carbonate containing sodium.
Compared with prior art, the basic nickel carbonate containing sodium obtained using above-mentioned synthesis technology, sodium content 5.1%.
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 the basic nickel carbonate containing sodium, which is characterized in that its method is implemented by following steps:
Step 1, sodium carbonate liquor and nickel sulfate solution are added in reactor simultaneously, it is molten by adjusting sodium carbonate in fill process
The pH value of the flow control system of liquid and nickel sulfate solution is 8.2~8.3, and reaction obtains basic nickel carbonate；
Step 2, stop that the sodium carbonate liquor and the nickel sulfate solution is added to reactor, by adjusting reaction temperature control
The basic nickel carbonate crystal phase transition that the step 1 obtains obtains hydration carbon nickel sodium crystal seed；
Step 3, the sodium carbonate liquor and the nickel sulfate solution is added to reactor again, passes through adjusting carbon in fill process
The pH value of the flow control system of acid sodium solution and nickel sulfate solution, and obtained by adjusting the reaction temperature control step 2
The hydration carbon nickel sodium crystal seed growth obtained, obtains the basic nickel carbonate crude product containing sodium；
Step 4, the basic nickel carbonate crude product containing the sodium step 3 obtained is successively aged, is washed, is dried and is sieved
Point, obtain the basic nickel carbonate containing sodium.
2. a kind of preparation method of basic nickel carbonate containing sodium according to claim 1, which is characterized in that the step 1
The concentration of sodium carbonate liquor is 180~300g/L, and the concentration of nickel sulfate solution is 60~100g/L in the step 1.
3. a kind of preparation method of basic nickel carbonate containing sodium according to claim 3, which is characterized in that the step 1
The flow of sodium carbonate liquor described in middle fill process is 100~1000L/h, the flow of the nickel sulfate solution is 100~
1000L/h。
4. a kind of preparation method of basic nickel carbonate containing sodium according to claim 3, which is characterized in that the step 1
In reaction temperature be 60~90 DEG C, 20~25h of reaction time.
5. a kind of preparation method of basic nickel carbonate containing sodium according to any one of claims 1-4, which is characterized in that
Reaction temperature in the step 2 is 50~60 DEG C, 30~60min of reaction time.
6. a kind of preparation method of basic nickel carbonate containing sodium according to claim 5, which is characterized in that the step 3
The pH value of middle system is controlled 8.5~8.8.
7. a kind of preparation method of basic nickel carbonate containing sodium according to claim 6, which is characterized in that the step 3
In reaction temperature be 50~60 DEG C, 11~30h of reaction time.
8. a kind of preparation method of basic nickel carbonate containing sodium according to claim 7, which is characterized in that the step 4
In digestion time be 0.5~3h.
9. a kind of preparation method of basic nickel carbonate containing sodium according to claim 8, which is characterized in that the step 4
In washing use pure water, the temperature of the pure water is 70~85 DEG C, conductivity≤100 μ s/m of the pure water.
10. a kind of preparation method of basic nickel carbonate containing sodium according to claim 8, which is characterized in that the step 4
In the temperature of the drying be 95~105 DEG C, time of the drying is 2~3h；The screening in the step 4 uses
200~400 meshes.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810167145.9A CN110203977B (en) | 2018-02-28 | 2018-02-28 | Preparation method of sodium-containing basic nickel carbonate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810167145.9A CN110203977B (en) | 2018-02-28 | 2018-02-28 | Preparation method of sodium-containing basic nickel carbonate |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN110203977A true CN110203977A (en) | 2019-09-06 |
| CN110203977B CN110203977B (en) | 2021-09-10 |
Family
ID=67778660
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810167145.9A Active CN110203977B (en) | 2018-02-28 | 2018-02-28 | Preparation method of sodium-containing basic nickel carbonate |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN110203977B (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2023024584A1 (en) * | 2021-08-26 | 2023-03-02 | 广东邦普循环科技有限公司 | Nickel-doped cobalt carbonate, and preparation method therefor and use thereof |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101016173A (en) * | 2006-12-29 | 2007-08-15 | 金川集团有限公司 | Method of preparing electronic grade nickel carbonate by sodium carbonate deposition |
| CN101708868A (en) * | 2009-11-20 | 2010-05-19 | 江西核工业兴中科技有限公司 | Process for rapidly producing basic nickel carbonate or basic cobaltous carbonate |
| CN102923794A (en) * | 2012-11-23 | 2013-02-13 | 长沙矿冶研究院有限责任公司 | Method for continuously compounding high-purity alkali nickel carbonate |
| CN105384199A (en) * | 2015-12-17 | 2016-03-09 | 江西核工业兴中新材料有限公司 | Process for synthesis of basic nickel carbonate from diacidic base |
| US20160090311A1 (en) * | 2014-09-26 | 2016-03-31 | Chung-Yuan Christian University | Method for forming Basic Nickel Carbonate |
-
2018
- 2018-02-28 CN CN201810167145.9A patent/CN110203977B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101016173A (en) * | 2006-12-29 | 2007-08-15 | 金川集团有限公司 | Method of preparing electronic grade nickel carbonate by sodium carbonate deposition |
| CN101708868A (en) * | 2009-11-20 | 2010-05-19 | 江西核工业兴中科技有限公司 | Process for rapidly producing basic nickel carbonate or basic cobaltous carbonate |
| CN102923794A (en) * | 2012-11-23 | 2013-02-13 | 长沙矿冶研究院有限责任公司 | Method for continuously compounding high-purity alkali nickel carbonate |
| US20160090311A1 (en) * | 2014-09-26 | 2016-03-31 | Chung-Yuan Christian University | Method for forming Basic Nickel Carbonate |
| CN105384199A (en) * | 2015-12-17 | 2016-03-09 | 江西核工业兴中新材料有限公司 | Process for synthesis of basic nickel carbonate from diacidic base |
Non-Patent Citations (1)
| Title |
|---|
| 吕文广: "高镍低钠高纯碱式碳酸镍的生产", 《工业催化》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2023024584A1 (en) * | 2021-08-26 | 2023-03-02 | 广东邦普循环科技有限公司 | Nickel-doped cobalt carbonate, and preparation method therefor and use thereof |
| GB2618694A (en) * | 2021-08-26 | 2023-11-15 | Guangdong Brunp Recycling Technology Co Ltd | Nickel-doped cobalt carbonate, and preparation method therefor and use thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN110203977B (en) | 2021-09-10 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101704543B (en) | Method for preparing cerous phosphate nano wire | |
| CN106673073A (en) | Method for preparing small-particle size large-bulk cobalt carbonate | |
| CN113603071B (en) | Nanometer flaky ferric phosphate and preparation method and application thereof | |
| CN103165878A (en) | Preparation method of spherical nickel-manganese binary material | |
| CN110203978A (en) | A kind of preparation method of the basic nickel carbonate of low sodium | |
| CN108328665A (en) | A kind of preparation method of battery grade spherical cobaltosic oxide particle | |
| CN104779388A (en) | Nickel and cobalt binary anode material precursor preparing method and nickel and cobalt binary anode material precursor prepared through method | |
| CN115490273A (en) | Method for continuously preparing large-ratio table ternary precursor and precursor prepared by method | |
| CN110203977A (en) | A kind of preparation method of the basic nickel carbonate containing sodium | |
| CN114524450B (en) | Preparation method of nano cerium oxide ultraviolet absorbent | |
| CN108483478A (en) | A method of preparing three kinds of crystal configuration calcium carbonate granules | |
| CN103628124A (en) | Low-voltage direct-current electrolysis preparation method of calcium carbonate whisker | |
| CN108585018A (en) | A kind of size is less than the Cu of 100nm2The preparation method of O nanospheres | |
| CN107416888A (en) | A kind of preparation method of nano cupric oxide | |
| CN109574056B (en) | Composite inducer for in-situ template-induced synthesis of nano calcium carbonate and application thereof | |
| CN113881952A (en) | Electrolytic synthesis method of high sodium sulfate | |
| CN113415821B (en) | Hollow Zn x Cd 1-x Preparation method and application of S solid solution nanosphere | |
| CN115029724A (en) | Preparation method and application of metal-doped 2H-phase molybdenum disulfide electrocatalyst | |
| CN212632690U (en) | Ternary precursor synthesizer with controllable solid content | |
| CN106241816B (en) | A kind of preparation method of silica dioxide delustring agent | |
| CN103922402A (en) | Method for preparing NH4V3O8 nanoribbon | |
| CN109987651A (en) | A kind of preparation method of high density basic nickel carbonate | |
| CN102863005B (en) | Preparation method of multi-shell core-shell micro/nano structure Cu2O | |
| CN114516624A (en) | Shape-controllable ferric phosphate, preparation method thereof and lithium iron phosphate | |
| CN109987653A (en) | A kind of preparation method of near-spherical basic nickel carbonate |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |