CN110092422A - A kind of minimizing technology for sulfate radical foreign matter in nickelous carbonate - Google Patents

Abstract

The invention discloses a method for removing sulfate impurity in nickel carbonate. The method is realized by the following steps: Step 1, adding liquid caustic soda into nickel carbonate containing sulfate ions and adjusting the pH value to 8.8-10.5 to obtain The nickel carbonate slurry after alkali washing; step 2, adding the above alkali washed nickel carbonate slurry into an aging kettle for 1-20 hours to obtain the aged nickel carbonate slurry; step 3, using pure water to The above-mentioned aged nickel carbonate slurry is rinsed and washed, and then dried to obtain nickel carbonate with sulfate impurity removed. In the present invention, the nickel carbonate containing sulfate ions is washed with liquid alkali with a temperature of 40-70° C. and a mass fraction of 10-32% and aged for 1-20 hours, and then rinsed and washed with pure water, thereby The problems of long washing process, large water consumption, low efficiency and high cost of post-treatment wastewater are effectively avoided, and the content of S element in the obtained nickel carbonate is very small.

Description

A kind of method for removing sulfate impurity in nickel carbonate

technical field

The present invention relates to a kind of removal method for impurities in nickel carbonate, relate to a kind of removal method for sulfate radical impurities in nickel carbonate.

Background technique

Basic nickel carbonate is an important inorganic fine chemical, mainly used for the preparation of various nickel salts. High-purity and refined basic nickel carbonate can be used in smelting, ceramic pigments, glaze ingredients, batteries, contact agents, electroplating nickel and catalysts and other intermediates, which are widely used and in great demand, and belong to the classic catalyst intermediates, with long-term demand and market unsaturation; among them, the traditional washing method adopts a large amount of water washing or ammonia washing and other schemes, although it has a certain effect on washing However, the washing process is too long, inefficient and consumes a lot of washing water, resulting in high cost of post-treatment wastewater, which is not in line with green production.

SUMMARY OF THE INVENTION

In view of this, the main purpose of the present invention is to provide a kind of removal method for sulfate radical impurity in nickel carbonate, solves the problem of long washing process, large water consumption, low efficiency and high cost of post-processing wastewater in the prior art.

For achieving the above object, technical scheme of the present invention is achieved in this way: a kind of removal method for sulfate radical impurity in nickelous carbonate, this method is realized by following steps:

Step 1, adding liquid caustic soda with a mass fraction of 10 to 32% to the nickel carbonate containing sulfate ions and adjusting the pH to 8.8 to 10.5 to obtain the nickel carbonate slurry after alkali washing;

Step 2, adding the alkali-washed nickel carbonate slurry obtained in the step 1 into an aging kettle for aging for 1 to 20 hours to obtain the aged nickel carbonate slurry;

In step 3, pure water is used to rinse and wash the aged nickel carbonate slurry obtained in the step 2, and then oven dry to obtain the nickel carbonate that has removed sulfate impurity.

Preferably, in the step 1, the temperature of the liquid caustic soda is 40-70°C.

Preferably, in the step 1, the flow rate when the liquid caustic soda is added to the nickel carbonate containing sulfate ions is 1 to 10 L/h.

Preferably, in the step 3, the temperature of the pure water is 70-85°C, and the electrical conductivity of the pure water is ≤100 μs/m.

Preferably, in the step 3, the drying temperature is 95-105°C, and the drying time is 2-3 h.

Preferably, in the step 1, the specific preparation method of the nickel carbonate containing sulfate ions is:

Step 1.1, in the solution tank, preparing respectively the sodium carbonate solution that carbonate ion concentration is 100～250g/L, the nickel sulphate solution that nickel ion concentration is 1～2moL/L and the complexing agent that massfraction is 0.1～2%;

Step 1.2, feeding with a metering pump, adding the sodium carbonate solution, nickel sulfate solution and complexing agent described in step 1.1 into the reactor at the same time, keeping the flow rate of the nickel sulfate solution unchanged during the feeding process, and adjusting the sodium carbonate solution. The flow rate of the solution controls the pH value of the system, and the reaction is carried out at 70 to 99 ° C to obtain a mixture containing nickel carbonate;

In step 1.3, the mixture containing nickel carbonate obtained in step 1.2 is put into a centrifuge for centrifugal separation to obtain nickel carbonate containing sulfate ions.

Preferably, in described step 1.1, described complexing agent is at least one in ammonia water complexing agent, EDTA complexing agent.

Preferably, in the step 1.2, when the metering pump feeds, the flow rate of the sodium carbonate solution is 5-1000L/h, the flow rate of the nickel sulfate solution is 50-1000L/h, and the flow rate of the complexing agent is 50-1000L/h. It 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 the prior art, the present invention washes the nickel carbonate containing sulfate ions with liquid alkali with a temperature of 40-70° C. and a mass fraction of 10-32% and ages it for 1-20 hours, and then uses a temperature of Washing and washing with pure water at 70-85°C and electrical conductivity ≤100μs/m can effectively avoid the problems of long washing process, large water consumption, low efficiency and high cost of post-treatment wastewater. The content of S element is very small, which can be well used in smelting, ceramic pigments, glaze ingredients, batteries, electroplating nickel and other industries.

Detailed ways

In order to make the objectives, technical solutions and advantages of the present invention clearer, the present invention will be further described in detail below with reference to the embodiments. It should be understood that the specific embodiments described herein are only used to explain the present invention, but not to limit the present invention.

The embodiment of the present invention provides a kind of removal method for sulfate radical impurity in nickelous carbonate, and this method realizes by following steps:

Step 1, adding liquid caustic soda with a temperature of 40 to 70° C. and a mass fraction of 10 to 32% according to a flow rate of 1 to 10 L/h into nickel carbonate containing sulfate ions and adjusting the pH to 8.8 to 10.5 to obtain alkaline washing. After the nickel carbonate slurry; by first adding liquid caustic soda with a temperature of 40 to 70 ° C and a mass fraction of 10 to 32% and a flow rate of 1 to 10 L/h into the nickel carbonate containing sulfate ions, at this time, carbonic acid The hydroxyl group in nickel adsorbs hydrogen ions in water through hydrogen bonds, and hydrogen ions have a certain attraction to sulfate ions through positive charges. At the same time, sulfate ions are relatively large and easy to adsorb, so that the van der Waals generated by hydrogen bonds and charges can be effectively destroyed by alkali washing. The adsorption force of sulfate ions is greatly weakened, which is more conducive to the removal of sulfate ions;

Wherein, the concrete preparation method of the nickelous carbonate containing sulfate ion is:

Step 1.1, in the solution tank, respectively prepare a sodium carbonate solution with a carbonate ion concentration of 100 to 250g/L, a nickel sulfate solution with a nickel ion concentration of 1 to 2moL/L, and a complexing agent with a mass fraction of 0.1 to 2%; Wherein, the complexing agent is at least one of ammonia water complexing agent and EDTA complexing agent;

Step 1.2, feeding with a metering pump, adding the sodium carbonate solution, nickel sulfate solution and complexing agent described in step 1.1 into the reactor at the same time, keeping the flow rate of the nickel sulfate solution unchanged during the feeding process, and adjusting the sodium carbonate solution. The pH value of the flow control system of the solution is 8.0 to 8.3, and the reaction is carried out at 70 to 99° C. for 5 to 100 hours to obtain a mixture containing nickel carbonate; wherein, when the metering pump feeds, the flow of the sodium carbonate solution is 5 to 1000L /h, the flow rate of nickel sulfate solution is 50~1000L/h, and the flow rate of complexing agent is 0.1~10L/h;

In step 1.3, the mixture containing nickel carbonate obtained in step 1.2 is put into a centrifuge for centrifugal separation to obtain nickel carbonate containing sulfate ions.

Step 2, adding the alkali-washed nickel carbonate slurry obtained in step 1 into an aging kettle for 1-20 hours to obtain the aged nickel carbonate slurry; by aging the alkali-washed nickel carbonate slurry , the purpose is that the hydroxyl group adsorbs hydrogen ions in water and hydrogen ions can have more sufficient time for the adsorption of sulfate ions through positive charges, so that the sulfate radical reaction is complete;

In step 3, the aged nickel carbonate slurry obtained in step 2 is rinsed and washed with pure water with a temperature of 70-85 °C and an electrical conductivity of ≤100 μs/m, and then dried at 95-105 °C for 2- 3h, to obtain nickel carbonate with sulfate impurity removed.

In the present invention, the nickel carbonate containing sulfate ions is washed with liquid alkali with a temperature of 40-70°C and a mass fraction of 10-32%, and then aged for 1-20h, and then washed with a temperature of 70-85°C and an electrical conductivity of 70-85°C. The pure water of ≤100μs/m is used for rinsing and washing, which effectively avoids the problems of long washing process, large water consumption, low efficiency and high cost of post-treatment wastewater, and the content of S element in the obtained nickel carbonate is very small, It can be well used in smelting, ceramic pigments, glaze ingredients, batteries, electroplating nickel and other industries.

Example 1

A method for removing sulfate radical impurities in nickel carbonate, the method is realized by the following steps:

Step 1, adding liquid caustic soda with a temperature of 55°C and a mass fraction of 20% to the nickel carbonate containing sulfate ions according to the flow rate of 5L/h and adjusting the pH value to 9.5 to obtain the nickel carbonate slurry after the alkali washing;

Step 2, adding the alkali-washed nickel carbonate slurry obtained in step 1 into the aging kettle for aging for 10h to obtain the aged nickel carbonate slurry;

In step 3, the aged nickel carbonate slurry obtained in step 2 is rinsed and washed with pure water with a temperature of 88 °C and a conductivity of ≤100 μs/m, and then dried at 100 °C for 2.5 hours to obtain the removal of sulfuric acid. Root impurities of nickel carbonate.

Wherein, the concrete preparation method of the nickelous carbonate containing sulfate ion in step 1 is:

Step 1.1, in solution tank, prepare respectively the sodium carbonate solution of carbonate ion concentration 150g/L, nickel ion concentration be that the nickel chloride solution of 1.5mol/L and massfraction are the ammoniacal complexing agent of 1%;

Step 1.2, with metering pump feeding, sodium carbonate solution, nickel chloride solution and ammonia complexing agent are added in the reactor simultaneously in step 1.1 (this reactor can flow out mother liquor in the reaction process, and ensure that nickel carbonate and mother liquor are formed. The solid content of the reaction system of the The adjustment range of the flow rate is 50-1000L/h) the pH value of the control system is 8.1, and the reaction is carried out at 80°C for 15h to obtain a mixture containing nickel carbonate;

In step 1.3, the mixture containing nickel carbonate obtained in step 1.2 is pumped into a centrifuge for centrifugal separation to obtain nickel carbonate containing sulfate ions.

Example 2

A method for removing sulfate radical impurities in nickel carbonate, the method is realized by the following steps:

Step 1, adding liquid caustic soda with a temperature of 40 ° C and a mass fraction of 32% to the nickel carbonate containing sulfate ions according to the flow rate of 1 L/h and adjusting the pH value to 9.5 to obtain the nickel carbonate slurry after the alkali washing;

Step 2, adding the alkali-washed nickel carbonate slurry obtained in step 1 into the aging kettle for aging for 10h to obtain the aged nickel carbonate slurry;

In step 3, the aged nickel carbonate slurry obtained in step 2 is rinsed and washed with pure water with a temperature of 85° C. and an electrical conductivity of ≤100 μs/m, and then dried at 95° C. for 3 hours to obtain the removal of sulfate radicals. Impurities of nickel carbonate.

Wherein, the concrete preparation method of the nickelous carbonate containing sulfate ion in step 1 is:

Step 1.1, in solution tank, prepare respectively the sodium carbonate solution of carbonate ion concentration 150g/L, nickel ion concentration be that the nickel chloride solution of 1.5mol/L and massfraction are the ammoniacal complexing agent of 1%;

Step 1.2, with metering pump feeding, sodium carbonate solution, nickel chloride solution and ammonia complexing agent are added in the reactor simultaneously in step 1.1 (this reactor can flow out mother liquor in the reaction process, and ensure that nickel carbonate and mother liquor are formed. The solid content of the reaction system of the The adjustment range of the flow rate is 50-1000L/h) the pH value of the control system is 8.1, and the reaction is carried out at 80°C for 15h to obtain a mixture containing nickel carbonate;

In step 1.3, the mixture containing nickel carbonate obtained in step 1.2 is pumped into a centrifuge for centrifugal separation to obtain nickel carbonate containing sulfate ions.

Example 3

A method for removing sulfate radical impurities in nickel carbonate, the method is realized by the following steps:

Step 1, adding the liquid caustic soda with a temperature of 70 ° C and a mass fraction of 10% to the nickel carbonate containing sulfate ions according to the flow rate of 10 L/h and adjusting the pH value to 9.5 to obtain the nickel carbonate slurry after the alkali washing;

Step 2, adding the alkali-washed nickel carbonate slurry obtained in step 1 into the aging kettle for aging for 10h to obtain the aged nickel carbonate slurry;

In step 3, the aged nickel carbonate slurry obtained in step 2 is rinsed and washed with pure water with a temperature of 70° C. and an electrical conductivity of ≤100 μs/m, and then dried at 105° C. for 2 hours to obtain the removal of sulfate radicals. Impurities of nickel carbonate.

Wherein, the concrete preparation method of the nickelous carbonate containing sulfate ion in step 1 is:

Step 1.1, in solution tank, prepare respectively the sodium carbonate solution of carbonate ion concentration 150g/L, nickel ion concentration be that the nickel chloride solution of 1.5mol/L and massfraction are the ammoniacal complexing agent of 1%;

Step 1.2, with metering pump feeding, sodium carbonate solution, nickel chloride solution and ammonia complexing agent are added in the reactor simultaneously in step 1.1 (this reactor can flow out mother liquor in the reaction process, and ensure that nickel carbonate and mother liquor are formed. The solid content of the reaction system of the The adjustment range of the flow rate is 50-1000L/h) the pH value of the control system is 8.1, and the reaction is carried out at 80°C for 15h to obtain a mixture containing nickel carbonate;

In step 1.3, the mixture containing nickel carbonate obtained in step 1.2 is pumped into a centrifuge for centrifugal separation to obtain nickel carbonate containing sulfate ions.

Example 4

A method for removing sulfate radical impurities in nickel carbonate, the method is realized by the following steps:

Step 1, adding liquid caustic soda with a temperature of 55°C and a mass fraction of 20% to the nickel carbonate containing sulfate ions according to the flow rate of 5L/h and adjusting the pH value to 8.8 to obtain the nickel carbonate slurry after the alkali washing;

Step 2, adding the alkali-washed nickel carbonate slurry obtained in step 1 into the aging kettle for aging for 20h to obtain the aged nickel carbonate slurry;

In step 3, the aged nickel carbonate slurry obtained in step 2 is rinsed and washed with pure water with a temperature of 88 °C and a conductivity of ≤100 μs/m, and then dried at 100 °C for 2.5 hours to obtain the removal of sulfuric acid. Root impurities of nickel carbonate.

Wherein, the concrete preparation method of the nickelous carbonate containing sulfate ion in step 1 is:

Step 1.1, in solution tank, prepare respectively the sodium carbonate solution of carbonate ion concentration 150g/L, nickel ion concentration be that the nickel chloride solution of 1.5mol/L and massfraction are the ammoniacal complexing agent of 1%;

Step 1.2, with metering pump feeding, sodium carbonate solution, nickel chloride solution and ammonia complexing agent are added in the reactor simultaneously in step 1.1 (this reactor can flow out mother liquor in the reaction process, and ensure that nickel carbonate and mother liquor are formed. The solid content of the reaction system of the The adjustment range of the flow rate is 50-1000L/h) the pH value of the control system is 8.1, and the reaction is carried out at 80°C for 15h to obtain a mixture containing nickel carbonate;

In step 1.3, the mixture containing nickel carbonate obtained in step 1.2 is pumped into a centrifuge for centrifugal separation to obtain nickel carbonate containing sulfate ions.

Example 5

A method for removing sulfate radical impurities in nickel carbonate, the method is realized by the following steps:

Step 1, adding the liquid caustic soda with a temperature of 40 ° C and a mass fraction of 32% to the nickel carbonate containing sulfate ions according to the flow rate of 1 L/h and adjusting the pH value to 8.8 to obtain the nickel carbonate slurry after the alkali washing;

Step 2, adding the alkali-washed nickel carbonate slurry obtained in step 1 into the aging kettle for aging for 20h to obtain the aged nickel carbonate slurry;

In step 3, the aged nickel carbonate slurry obtained in step 2 is rinsed and washed with pure water with a temperature of 85° C. and an electrical conductivity of ≤100 μs/m, and then dried at 95° C. for 3 hours to obtain the removal of sulfate radicals. Impurities of nickel carbonate.

Wherein, the concrete preparation method of the nickelous carbonate containing sulfate ion in step 1 is:

Step 1.1, in solution tank, prepare respectively the sodium carbonate solution of carbonate ion concentration 150g/L, nickel ion concentration be that the nickel chloride solution of 1.5mol/L and massfraction are the ammoniacal complexing agent of 1%;

Step 1.2, with metering pump feeding, sodium carbonate solution, nickel chloride solution and ammonia complexing agent are added in the reactor simultaneously in step 1.1 (this reactor can flow out mother liquor in the reaction process, and ensure that nickel carbonate and mother liquor are formed. The solid content of the reaction system of the The adjustment range of the flow rate is 50-1000L/h) the pH value of the control system is 8.1, and the reaction is carried out at 80°C for 15h to obtain a mixture containing nickel carbonate;

In step 1.3, the mixture containing nickel carbonate obtained in step 1.2 is pumped into a centrifuge for centrifugal separation to obtain nickel carbonate containing sulfate ions.

Example 6

A method for removing sulfate radical impurities in nickel carbonate, the method is realized by the following steps:

Step 1, adding liquid caustic soda with a temperature of 70°C and a mass fraction of 10% to 10L/h according to the flow rate into the nickel carbonate containing sulfate ions and adjusting the pH value to 8.8 to obtain the nickel carbonate slurry after the alkali washing;

Step 2, adding the alkali-washed nickel carbonate slurry obtained in step 1 into the aging kettle for aging for 20h to obtain the aged nickel carbonate slurry;

In step 3, the aged nickel carbonate slurry obtained in step 2 is rinsed and washed with pure water with a temperature of 70° C. and an electrical conductivity of ≤100 μs/m, and then dried at 105° C. for 2 hours to obtain the removal of sulfate radicals. Impurities of nickel carbonate.

Wherein, the concrete preparation method of the nickelous carbonate containing sulfate ion in step 1 is:

Step 1.1, in solution tank, prepare respectively the sodium carbonate solution of carbonate ion concentration 150g/L, nickel ion concentration be that the nickel chloride solution of 1.5mol/L and massfraction are the ammoniacal complexing agent of 1%;

Step 1.2, with metering pump feeding, sodium carbonate solution, nickel chloride solution and ammonia complexing agent are added in the reactor simultaneously in step 1.1 (this reactor can flow out mother liquor in the reaction process, and ensure that nickel carbonate and mother liquor are formed. The solid content of the reaction system of the The adjustment range of the flow rate is 50-1000L/h) the pH value of the control system is 8.1, and the reaction is carried out at 80°C for 15h to obtain a mixture containing nickel carbonate;

In step 1.3, the mixture containing nickel carbonate obtained in step 1.2 is pumped into a centrifuge for centrifugal separation to obtain nickel carbonate containing sulfate ions.

Example 7

A method for removing sulfate radical impurities in nickel carbonate, the method is realized by the following steps:

Step 1, adding liquid caustic soda with a temperature of 55 ° C and a mass fraction of 20% to the nickel carbonate containing sulfate ions according to the flow rate of 5 L/h and adjusting the pH value to 10.5 to obtain the nickel carbonate slurry after the alkali washing;

Step 2, adding the alkali-washed nickel carbonate slurry obtained in step 1 into the aging kettle for aging for 1 h to obtain the aged nickel carbonate slurry;

In step 3, the aged nickel carbonate slurry obtained in step 2 is rinsed and washed with pure water with a temperature of 88 °C and a conductivity of ≤100 μs/m, and then dried at 100 °C for 2.5 hours to obtain the removal of sulfuric acid. Root impurities of nickel carbonate.

Wherein, the concrete preparation method of the nickelous carbonate containing sulfate ion in step 1 is:

Step 1.1, in solution tank, prepare respectively the sodium carbonate solution of carbonate ion concentration 150g/L, nickel ion concentration be that the nickel chloride solution of 1.5mol/L and massfraction are the ammoniacal complexing agent of 1%;

Step 1.2, with metering pump feeding, sodium carbonate solution, nickel chloride solution and ammonia complexing agent are added in the reactor simultaneously in step 1.1 (this reactor can flow out mother liquor in the reaction process, and ensure that nickel carbonate and mother liquor are formed. The solid content of the reaction system of the The adjustment range of the flow rate is 50-1000L/h) the pH value of the control system is 8.1, and the reaction is carried out at 80°C for 15h to obtain a mixture containing nickel carbonate;

In step 1.3, the mixture containing nickel carbonate obtained in step 1.2 is pumped into a centrifuge for centrifugal separation to obtain nickel carbonate containing sulfate ions.

Example 8

A method for removing sulfate radical impurities in nickel carbonate, the method is realized by the following steps:

Step 1, adding liquid caustic soda with a temperature of 40 ° C and a mass fraction of 32% to the nickel carbonate containing sulfate ions according to the flow rate of 1 L/h and adjusting the pH value to 10.5 to obtain the nickel carbonate slurry after the alkali washing;

Step 2, adding the alkali-washed nickel carbonate slurry obtained in step 1 into the aging kettle for aging for 1 h to obtain the aged nickel carbonate slurry;

In step 3, the aged nickel carbonate slurry obtained in step 2 is rinsed and washed with pure water with a temperature of 85° C. and an electrical conductivity of ≤100 μs/m, and then dried at 95° C. for 3 hours to obtain the removal of sulfate radicals. Impurities of nickel carbonate.

Wherein, the concrete preparation method of the nickelous carbonate containing sulfate ion in step 1 is:

Step 1.1, in solution tank, prepare respectively the sodium carbonate solution of carbonate ion concentration 150g/L, nickel ion concentration be that the nickel chloride solution of 1.5mol/L and massfraction are the ammoniacal complexing agent of 1%;

Step 1.2, with metering pump feeding, sodium carbonate solution, nickel chloride solution and ammonia complexing agent are added in the reactor simultaneously in step 1.1 (this reactor can flow out mother liquor in the reaction process, and ensure that nickel carbonate and mother liquor are formed. The solid content of the reaction system of the The adjustment range of the flow rate is 50-1000L/h) the pH value of the control system is 8.1, and the reaction is carried out at 80°C for 15h to obtain a mixture containing nickel carbonate;

In step 1.3, the mixture containing nickel carbonate obtained in step 1.2 is pumped into a centrifuge for centrifugal separation to obtain nickel carbonate containing sulfate ions.

Example 9

A method for removing sulfate radical impurities in nickel carbonate, the method is realized by the following steps:

Step 1, adding the liquid caustic soda with a temperature of 70 ° C and a mass fraction of 10% to the nickel carbonate containing sulfate ions according to the flow rate of 10 L/h and adjusting the pH value to 10.5 to obtain the nickel carbonate slurry after the alkali washing;

Step 2, adding the alkali-washed nickel carbonate slurry obtained in step 1 into the aging kettle for aging for 1 h to obtain the aged nickel carbonate slurry;

In step 3, the aged nickel carbonate slurry obtained in step 2 is rinsed and washed with pure water with a temperature of 70° C. and an electrical conductivity of ≤100 μs/m, and then dried at 105° C. for 2 hours to obtain the removal of sulfate radicals. Impurities of nickel carbonate.

Wherein, the concrete preparation method of the nickelous carbonate containing sulfate ion in step 1 is:

Step 1.1, in solution tank, prepare respectively the sodium carbonate solution of carbonate ion concentration 150g/L, nickel ion concentration be that the nickel chloride solution of 1.5mol/L and massfraction are the ammoniacal complexing agent of 1%;

Step 1.2, with metering pump feeding, sodium carbonate solution, nickel chloride solution and ammonia complexing agent are added in the reactor simultaneously in step 1.1 (this reactor can flow out mother liquor in the reaction process, and ensure that nickel carbonate and mother liquor are formed. The solid content of the reaction system of the The adjustment range of the flow rate is 50-1000L/h) the pH value of the control system is 8.1, and the reaction is carried out at 80°C for 15h to obtain a mixture containing nickel carbonate;

In step 1.3, the mixture containing nickel carbonate obtained in step 1.2 is pumped into a centrifuge for centrifugal separation to obtain nickel carbonate containing sulfate ions.

Example 10

A method for removing sulfate radical impurities in nickel carbonate, the method is realized by the following steps:

Step 1, adding the liquid caustic soda with a temperature of 40 ° C and a mass fraction of 32% to the nickel carbonate containing sulfate ions according to the flow rate of 5 L/h and adjusting the pH value to 9.0 to obtain the nickel carbonate slurry after the alkali washing;

Step 2, adding the alkali-washed nickel carbonate slurry obtained in step 1 into the aging kettle for aging for 20h to obtain the aged nickel carbonate slurry;

In step 3, the aged nickel carbonate slurry obtained in step 2 is rinsed and washed with pure water with a temperature of 85° C. and an electrical conductivity of ≤100 μs/m, and then dried at 95° C. for 3 hours to obtain the removal of sulfate radicals. Impurities of nickel carbonate.

Wherein, the concrete preparation method of the nickelous carbonate containing sulfate ion in step 1 is:

Step 1.1, in solution tank, prepare respectively the sodium carbonate solution of carbonate ion concentration 150g/L, nickel ion concentration be that the nickel chloride solution of 1.5mol/L and massfraction are the EDTA complexing agent of 1%;

Step 1.2, with metering pump feeding, sodium carbonate solution, nickel chloride solution and ammonia complexing agent are added in the reactor simultaneously in step 1.1 (this reactor can flow out mother liquor in the reaction process, and ensure that nickel carbonate and mother liquor are formed. The solid content of the reaction system of the The adjustment range of the flow rate is 50-1000L/h) the pH value of the control system is 8.1, and the reaction is carried out at 80°C for 15h to obtain a mixture containing nickel carbonate;

In step 1.3, the mixture containing nickel carbonate obtained in step 1.2 is pumped into a centrifuge for centrifugal separation to obtain nickel carbonate containing sulfate ions.

The detection of S content was carried out to the nickel carbonate obtained in Example 1-Example 10 for removing sulfate impurities, and the detection results are shown in Table 1:

The detection data of S content in the nickel carbonate that removes the sulfate radical impurity obtained by the embodiment 1-Example 10 of table 1

S content/% Example 1 0.005% Example 2 0.007% Example 3 0.006% Example 4 0.008% Example 5 0.004% Example 6 0.006% Example 7 0.005% Example 8 0.007% Example 9 0.008% Example 10 0.006% conventional 0.025%

As can be seen from Table 1, in the nickel carbonate for removing sulfate impurity obtained by the present invention, the S content is all less than 0.01%, thus it can be seen that the performance of the nickel carbonate for removing sulfate impurity obtained by the present invention is better than existing Various properties of the basic nickel carbonate obtained by the washing method make it widely used.

The above descriptions are merely preferred embodiments of the present invention, and are not intended to limit the protection 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.