CN113292108A - Preparation process of low-chlorine cobalt carbonate for superfine cobalt powder - Google Patents
Preparation process of low-chlorine cobalt carbonate for superfine cobalt powder Download PDFInfo
- Publication number
- CN113292108A CN113292108A CN202010113493.5A CN202010113493A CN113292108A CN 113292108 A CN113292108 A CN 113292108A CN 202010113493 A CN202010113493 A CN 202010113493A CN 113292108 A CN113292108 A CN 113292108A
- Authority
- CN
- China
- Prior art keywords
- cobalt
- ammonium bicarbonate
- cobalt carbonate
- solid
- bicarbonate solution
- 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.)
- Pending
Links
- ZOTKGJBKKKVBJZ-UHFFFAOYSA-L cobalt(2+);carbonate Chemical compound [Co+2].[O-]C([O-])=O ZOTKGJBKKKVBJZ-UHFFFAOYSA-L 0.000 title claims abstract description 86
- 229910021446 cobalt carbonate Inorganic materials 0.000 title claims abstract description 85
- 239000000460 chlorine Substances 0.000 title claims abstract description 32
- 229910052801 chlorine Inorganic materials 0.000 title claims abstract description 32
- 238000002360 preparation method Methods 0.000 title claims abstract description 31
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 title claims abstract description 25
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 claims abstract description 61
- 229910000013 Ammonium bicarbonate Inorganic materials 0.000 claims abstract description 61
- 235000012538 ammonium bicarbonate Nutrition 0.000 claims abstract description 61
- 239000001099 ammonium carbonate Substances 0.000 claims abstract description 61
- GVPFVAHMJGGAJG-UHFFFAOYSA-L cobalt dichloride Chemical compound [Cl-].[Cl-].[Co+2] GVPFVAHMJGGAJG-UHFFFAOYSA-L 0.000 claims abstract description 61
- 239000007788 liquid Substances 0.000 claims abstract description 36
- 239000002002 slurry Substances 0.000 claims abstract description 35
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 33
- 238000000926 separation method Methods 0.000 claims abstract description 29
- 238000006243 chemical reaction Methods 0.000 claims abstract description 27
- 239000007787 solid Substances 0.000 claims abstract description 27
- 238000003756 stirring Methods 0.000 claims abstract description 25
- 238000001035 drying Methods 0.000 claims abstract description 22
- 238000005406 washing Methods 0.000 claims abstract description 20
- 230000032683 aging Effects 0.000 claims abstract description 15
- 238000000034 method Methods 0.000 claims abstract description 9
- 230000005540 biological transmission Effects 0.000 claims description 44
- 230000000087 stabilizing effect Effects 0.000 claims description 32
- 230000014759 maintenance of location Effects 0.000 claims description 6
- 238000001914 filtration Methods 0.000 claims description 3
- 238000004537 pulping Methods 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims description 2
- 229910000001 cobalt(II) carbonate Inorganic materials 0.000 claims 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 abstract description 22
- 239000002245 particle Substances 0.000 abstract description 7
- 238000001179 sorption measurement Methods 0.000 abstract description 4
- 239000002351 wastewater Substances 0.000 abstract description 3
- 238000009776 industrial production Methods 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 20
- 238000002156 mixing Methods 0.000 description 20
- 238000010438 heat treatment Methods 0.000 description 10
- 238000004806 packaging method and process Methods 0.000 description 10
- 239000000843 powder Substances 0.000 description 10
- 238000012216 screening Methods 0.000 description 10
- 239000002994 raw material Substances 0.000 description 7
- 239000000956 alloy Substances 0.000 description 5
- 229910045601 alloy Inorganic materials 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 238000004321 preservation Methods 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- IKOKHHBZFDFMJW-UHFFFAOYSA-N 2-[4-[2-(2,3-dihydro-1H-inden-2-ylamino)pyrimidin-5-yl]-3-(2-morpholin-4-ylethoxy)pyrazol-1-yl]-1-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)ethanone Chemical compound C1C(CC2=CC=CC=C12)NC1=NC=C(C=N1)C=1C(=NN(C=1)CC(=O)N1CC2=C(CC1)NN=N2)OCCN1CCOCC1 IKOKHHBZFDFMJW-UHFFFAOYSA-N 0.000 description 1
- DHKVCYCWBUNNQH-UHFFFAOYSA-N 2-[5-[2-(2,3-dihydro-1H-inden-2-ylamino)pyrimidin-5-yl]-1,3,4-oxadiazol-2-yl]-1-(1,4,5,7-tetrahydropyrazolo[3,4-c]pyridin-6-yl)ethanone Chemical compound C1C(CC2=CC=CC=C12)NC1=NC=C(C=N1)C1=NN=C(O1)CC(=O)N1CC2=C(CC1)C=NN2 DHKVCYCWBUNNQH-UHFFFAOYSA-N 0.000 description 1
- VCUFZILGIRCDQQ-KRWDZBQOSA-N N-[[(5S)-2-oxo-3-(2-oxo-3H-1,3-benzoxazol-6-yl)-1,3-oxazolidin-5-yl]methyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C1O[C@H](CN1C1=CC2=C(NC(O2)=O)C=C1)CNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F VCUFZILGIRCDQQ-KRWDZBQOSA-N 0.000 description 1
- FHKPLLOSJHHKNU-INIZCTEOSA-N [(3S)-3-[8-(1-ethyl-5-methylpyrazol-4-yl)-9-methylpurin-6-yl]oxypyrrolidin-1-yl]-(oxan-4-yl)methanone Chemical compound C(C)N1N=CC(=C1C)C=1N(C2=NC=NC(=C2N=1)O[C@@H]1CN(CC1)C(=O)C1CCOCC1)C FHKPLLOSJHHKNU-INIZCTEOSA-N 0.000 description 1
- XKMRRTOUMJRJIA-UHFFFAOYSA-N ammonia nh3 Chemical compound N.N XKMRRTOUMJRJIA-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910000428 cobalt oxide Inorganic materials 0.000 description 1
- IVMYJDGYRUAWML-UHFFFAOYSA-N cobalt(ii) oxide Chemical compound [Co]=O IVMYJDGYRUAWML-UHFFFAOYSA-N 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 230000005518 electrochemistry Effects 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000011085 pressure filtration Methods 0.000 description 1
- 238000011946 reduction process Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000004879 turbidimetry Methods 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G51/00—Compounds of cobalt
- C01G51/06—Carbonates
-
- C—CHEMISTRY; METALLURGY
- 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 preparation process of low-chlorine cobalt carbonate for superfine cobalt powder, which comprises the following steps: s1, under the stirring state, adding 78-82 g/L of cobalt chloride solution and 178-182 g/L of ammonium bicarbonate solution into a reaction container containing pure water at a stable and uniform speed, continuously reacting for 6-8 hours at 40-42 ℃, and aging to obtain cobalt carbonate slurry; and S2, carrying out solid-liquid separation on the cobalt carbonate slurry, adding water into the separated solid to carry out slurrying washing, and drying to obtain the low-chlorine cobalt carbonate. According to the invention, the flow and concentration of ammonium bicarbonate and cobalt chloride are controlled, so that the surface smoothness of cobalt carbonate particle growth is controlled from the microscopic morphology, the wrapping and adsorption of chloride ions are controlled, the problems of high chloride ion content and high wastewater amount in cobalt carbonate are effectively solved, and the method is suitable for industrial production.
Description
Technical Field
The invention belongs to the technical field of electrochemistry, and particularly relates to a preparation process of low-chlorine cobalt carbonate for superfine cobalt powder.
Background
The superfine hard alloy has excellent performance and is an important direction for the development of hard alloy. The production of superfine alloy must add superfine cobalt powder, so the high quality superfine cobalt powder is one of the important raw materials for producing superfine hard alloy.
At present, the most common preparation method of cobalt powder is to reduce cobalt oxide or cobalt carbonate, the preparation process is reduced by raising the temperature, but the cobalt carbonate produced by adopting a chloride system at present is difficult to wash chloride ions, the produced wastewater is high, and the content of the chloride ions cannot meet the requirement, namely the cobalt carbonate contains more chloride ions; when the cobalt carbonate is used for preparing cobalt powder, hydrochloric acid generated in the reduction process of downstream cobalt powder products can be caused to corrode equipment, and the high ammonia nitrogen content in the cobalt powder can influence the characteristics of hard alloy. Therefore, the preparation of the low-chlorine cobalt carbonate is necessary.
Disclosure of Invention
In view of the above, the present invention aims to provide a preparation process of low-chlorine cobalt carbonate for superfine cobalt powder, which effectively solves the problems of high chloride ion content and high wastewater amount in cobalt carbonate by controlling the flow rate and concentration of ammonium bicarbonate and cobalt chloride, controlling the surface smoothness of cobalt carbonate particle growth from the micro-morphology, and controlling the wrapping and adsorption of chloride ions.
The technical scheme adopted by the invention is that the preparation process of the low-chlorine cobalt carbonate for the superfine cobalt powder comprises the following steps:
s1, adding a cobalt chloride solution with the mass concentration of 78-82 g/L and an ammonium bicarbonate solution with the mass concentration of 178-182 g/L into a reaction container containing pure water stably at a constant speed in a stirring state, continuously reacting for 6-8 hours at 40-42 ℃, and aging to obtain cobalt carbonate slurry;
wherein the stirring speed is 900-1200 rpm, the feed flow rate of the cobalt chloride solution is 115-125L/h, and the feed flow rate of the ammonium bicarbonate solution is 255-265L/h;
and S2, carrying out solid-liquid separation on the cobalt carbonate slurry obtained in the S1, adding water into the solid obtained after the solid-liquid separation, pulping, washing and drying to obtain the low-chlorine cobalt carbonate.
Preferably, in the S1, the adding amount of water in the reaction vessel is 0.5-0.6 m3The water temperature is 40-42 ℃.
Preferably, the S1 further includes:
and simultaneously starting the transmission of the cobalt chloride solution and the ammonium bicarbonate solution, carrying out a transmission process for stabilizing the flow for 25-35 min, and adding the cobalt chloride solution and the ammonium bicarbonate solution into the reaction container at a constant speed when the flow of the cobalt chloride solution is maintained at 115-125L/h and the flow of the ammonium bicarbonate solution is maintained at 255-265L/h.
Preferably, in the S1, the feed flow rate of the cobalt chloride solution is 118-122L/h, and the feed flow rate of the ammonium bicarbonate solution is 258-262L/h.
Preferably, in S2, in the slurry washing, the ratio of the solid after the solid-liquid separation to water is 1 t: (3 to 5) m3。
Preferably, the equipment used for solid-liquid separation and slurrying washing in the step S2 is a two-in-one equipment for filtering washing.
In a specific embodiment, the two-in-one device is a two-in-one device capable of filtering and washing, and specifically can be a two-in-one device for pressure filtration and washing. Preferably, the number of times of slurry washing in the S2 is 1-3 times.
Preferably, the drying conditions in S2 are as follows: the drying temperature is 140-160 ℃, and the retention time is 30-60 min.
Preferably, in the step S1, the aging time is 10-20 min.
The invention has the beneficial effects that: the method accurately controls the concentration and flow of the ammonium bicarbonate solution and the cobalt chloride solution, and controls the generation and growth of the cobalt carbonate particle seed crystal from the microscopic morphology, so that the surface of the formed cobalt carbonate particle is smooth, and the wrapping and surface adsorption of chloride ions are also controlled; the preparation process controls the wrapping of chloride ions in the cobalt carbonate particles and the modification of the surface of the cobalt carbonate, thereby reducing the wrapping of the chloride ions in the cobalt carbonate and the adsorption of the chloride ions on the surface of the cobalt carbonate, and removing the chloride ions by washing with pure water, wherein the content of the chloride ions in the finally obtained cobalt carbonate is lower than 15 ppm; the preparation process is simple, the conditions are mild, and the preparation of the low-chlorine cobalt carbonate is realized.
Drawings
FIG. 1 is a scanning electron micrograph of cobalt carbonate prepared in example 1 of the present invention;
FIG. 2 is a graph showing the chloride ion content in cobalt carbonate products prepared in examples 1 to 10 and comparative examples 1 to 8 according to the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Example 1
The embodiment provides a preparation process of low-chlorine cobalt carbonate for superfine cobalt powder, which comprises the following steps:
s1, mixing the powder with the grain size of 0.5m3Adding water into the reaction kettle, and heating to 40 ℃;
simultaneously starting the transmission of the cobalt chloride solution and the ammonium bicarbonate solution, and carrying out a transmission process for stabilizing the flow for 30min, namely starting the transmission and maintaining the transmission for 30min for stabilizing the flow, wherein when the flow of the cobalt chloride solution is stabilized at 120L/h and the flow of the ammonium bicarbonate solution is stabilized at 260L/h, the subsequent operation can be carried out;
under the stirring speed of 1000rpm, namely under the continuous stirring state, adding the cobalt chloride solution with the mass concentration of 80g/L and the ammonium bicarbonate solution with the mass concentration of 179g/L which are subjected to the flow stabilizing operation into the reaction container in the S1 in a stable and uniform manner, wherein the feeding flow rate of the cobalt chloride solution is 120L/h, the feeding flow rate of the ammonium bicarbonate solution is 260L/h, and then, after continuously reacting for 6h at 42 ℃, aging for 10min to obtain cobalt carbonate slurry;
s2, performing solid-liquid separation on the cobalt carbonate slurry obtained in the S1 in a two-in-one device, and mixing the solid obtained after the solid-liquid separation with pure water according to the weight ratio of 1 t: 4m3The material-liquid ratio of the raw materials is pulped and washed, the materials are separated in two-in-one equipment after washing, then the solid is transferred to a tray dryer for drying, the drying temperature is 140 ℃, and the retention time is 60 min;
and S3, screening and packaging the dried product of S2 to obtain the low-chlorine cobalt carbonate product.
Example 2
The embodiment provides a preparation process of low-chlorine cobalt carbonate for superfine cobalt powder, which comprises the following steps:
s1, mixing the powder with 0.55m3Adding water into the reaction kettle, and heating to 42 ℃;
simultaneously starting the transmission of the cobalt chloride solution and the ammonium bicarbonate solution, and carrying out a transmission process for stabilizing the flow for 35min, namely starting the transmission and maintaining the transmission for 35min for stabilizing the flow, wherein when the flow of the cobalt chloride solution is stabilized at 118L/h and the flow of the ammonium bicarbonate solution is stabilized at 258L/h, the subsequent operation can be carried out;
under the stirring speed of 1100rpm, namely under the continuous stirring state, adding the cobalt chloride solution with the mass concentration of 81g/L and the ammonium bicarbonate solution with the mass concentration of 181g/L which are subjected to the flow stabilizing operation into the reaction container in the S1 in a stable and uniform manner, wherein the feeding flow rate of the cobalt chloride solution is 118L/h, the feeding flow rate of the ammonium bicarbonate solution is 258L/h, and then after continuously reacting for 7h at 42 ℃, aging for 15min to obtain cobalt carbonate slurry;
s2, performing solid-liquid separation on the cobalt carbonate slurry obtained in the S1 in a two-in-one device, and mixing the solid obtained after the solid-liquid separation with pure water according to the weight ratio of 1 t: 3m3The slurry-liquid ratio of (A) is subjected to slurrying washing, the washed slurry is separated in a two-in-one device, and then the solid is transferredDrying in a tray dryer at 145 deg.C for 50 min;
and S3, screening and packaging the dried product of S2 to obtain the low-chlorine cobalt carbonate product.
Example 3
The embodiment provides a preparation process of low-chlorine cobalt carbonate for superfine cobalt powder, which comprises the following steps:
s1, mixing the powder with 0.6m3Adding water into the reaction kettle, and heating to 40 ℃;
simultaneously starting the transmission of the cobalt chloride solution and the ammonium bicarbonate solution, and carrying out a transmission process for stabilizing the flow for 35min, namely starting the transmission and maintaining the transmission for 35min for stabilizing the flow, wherein when the flow of the cobalt chloride solution is stabilized at 125L/h and the flow of the ammonium bicarbonate solution is stabilized at 265L/h, the subsequent operation can be carried out;
under the stirring speed of 900rpm, namely under the continuous stirring state, adding the cobalt chloride solution with the mass concentration of 82g/L and the ammonium bicarbonate solution with the mass concentration of 182g/L which are subjected to the flow stabilizing operation into the reaction container in the S1 in a stable and uniform manner, wherein the feeding flow rate of the cobalt chloride solution is 125L/h, the feeding flow rate of the ammonium bicarbonate solution is 265L/h, and then, after continuously reacting for 8h at 40 ℃, aging for 20min to obtain cobalt carbonate slurry;
s2, performing solid-liquid separation on the cobalt carbonate slurry obtained in the S1 in a two-in-one device, and mixing the solid obtained after the solid-liquid separation with pure water according to the weight ratio of 1 t: 3m3The material-liquid ratio of the raw materials is pulped and washed, the materials are separated in a two-in-one device after washing, then the solid is transferred to a tray dryer for drying, the drying temperature is 160 ℃, and the retention time is 30 min;
and S3, screening and packaging the dried product of S2 to obtain the low-chlorine cobalt carbonate product.
Example 4
The embodiment provides a preparation process of low-chlorine cobalt carbonate for superfine cobalt powder, which comprises the following steps:
s1, mixing the powder with the grain size of 0.5m3Adding water into the reaction kettle, and heating to 40 ℃;
simultaneously starting the transmission of the cobalt chloride solution and the ammonium bicarbonate solution, and carrying out a transmission process for stabilizing the flow for 25min, namely starting the transmission and maintaining the transmission for 25min for stabilizing the flow, wherein when the flow of the cobalt chloride solution is stabilized at 115L/h and the flow of the ammonium bicarbonate solution is stabilized at 255L/h, the subsequent operation can be carried out;
under the stirring speed of 1200rpm, namely under the continuous stirring state, adding the cobalt chloride solution with the mass concentration of 78g/L and the ammonium bicarbonate solution with the mass concentration of 178g/L which are subjected to the flow stabilizing operation into the reaction container in the S1 in a stable and uniform manner, wherein the feeding flow rate of the cobalt chloride solution is 115L/h, the feeding flow rate of the ammonium bicarbonate solution is 255L/h, and then, after continuously reacting for 6h at 40 ℃, aging for 10min to obtain cobalt carbonate slurry;
s2, performing solid-liquid separation on the cobalt carbonate slurry obtained in the S1 in a two-in-one device, and mixing the solid obtained after the solid-liquid separation with pure water according to the weight ratio of 1 t: 5m3The slurry is washed, the washed materials are separated in a two-in-one device, and then the solid is transferred to a tray dryer to be dried, wherein the drying temperature is 152 ℃, and the heat preservation time is 45 min;
and S3, screening and packaging the dried product of S2 to obtain the low-chlorine cobalt carbonate product.
Example 5
The embodiment provides a preparation process of low-chlorine cobalt carbonate for superfine cobalt powder, which comprises the following steps:
s1, mixing the powder with 0.58m3Adding water into the reaction kettle, and heating to 41 ℃;
simultaneously starting the transmission of the cobalt chloride solution and the ammonium bicarbonate solution, and carrying out a transmission process for stabilizing the flow for 29min, namely starting the transmission and maintaining the transmission for stabilizing the flow for 29min, wherein when the flow of the cobalt chloride solution is stabilized at 117L/h and the flow of the ammonium bicarbonate solution is stabilized at 256L/h, the subsequent operation can be carried out;
under the stirring speed of 950rpm, namely under the continuous stirring state, adding the cobalt chloride solution with the mass concentration of 79g/L and the ammonium bicarbonate solution with the mass concentration of 181g/L which are subjected to the flow stabilizing operation into the reaction container in the S1 in a stable and uniform manner, wherein the feeding flow rate of the cobalt chloride solution is 117L/h, the feeding flow rate of the ammonium bicarbonate solution is 256L/h, and then after continuously reacting for 7h at 40 ℃, aging for 15min to obtain cobalt carbonate slurry;
s2, performing solid-liquid separation on the cobalt carbonate slurry obtained in the S1 in a two-in-one device, and mixing the solid obtained after the solid-liquid separation with pure water according to the weight ratio of 1 t: 3m3The slurry is washed, and then the solid is separated in two-in-one equipment after washing, and then the solid is transferred to a tray dryer for drying, wherein the drying temperature is 140 ℃, and the heat preservation time is 55 min;
and S3, screening and packaging the dried product of S1 to obtain the low-chlorine cobalt carbonate product.
Example 6
The embodiment provides a preparation process of low-chlorine cobalt carbonate for superfine cobalt powder, which comprises the following steps:
s1, mixing the powder with 0.55m3Adding water into the reaction kettle, and heating to 41 ℃;
simultaneously starting the transmission of the cobalt chloride solution and the ammonium bicarbonate solution, and carrying out a transmission process for stabilizing the flow for 30min, namely starting the transmission and maintaining the transmission for 30min for stabilizing the flow, wherein when the flow of the cobalt chloride solution is stabilized at 120L/h and the flow of the ammonium bicarbonate solution is stabilized at 260L/h, the subsequent operation can be carried out;
under the stirring speed of 1050rpm, namely under the continuous stirring state, adding the cobalt chloride solution with the mass concentration of 80g/L and the ammonium bicarbonate solution with the mass concentration of 180g/L which are subjected to the flow stabilizing operation into the reaction container in the S1 in a stable and uniform manner, wherein the feeding flow rate of the cobalt chloride solution is 120L/h, the feeding flow rate of the ammonium bicarbonate solution is 260L/h, and then after continuously reacting for 7h at 41 ℃, aging for 15min to obtain cobalt carbonate slurry;
s2, performing solid-liquid separation on the cobalt carbonate slurry obtained in the S1 in a two-in-one device, and mixing the solid obtained after the solid-liquid separation with pure water according to the weight ratio of 1 t: 4m3The slurry-liquid ratio of the raw materials is pulped and washed, then the raw materials are separated in a two-in-one device, and then the solid is transferred to a tray dryer for pulping and washingDrying at 150 deg.C for 45 min;
and S3, screening and packaging the dried product of S2 to obtain the low-chlorine cobalt carbonate product.
Example 7
The embodiment provides a preparation process of low-chlorine cobalt carbonate for superfine cobalt powder, which comprises the following steps:
s1, mixing the powder with the grain size of 0.5m3Adding water into the reaction kettle, and heating to 42 ℃;
simultaneously starting the transmission of the cobalt chloride solution and the ammonium bicarbonate solution, and carrying out a transmission process for stabilizing the flow for 30min, namely starting the transmission and maintaining the transmission for 30min for stabilizing the flow, wherein when the flow of the cobalt chloride solution is stabilized at 122L/h and the flow of the ammonium bicarbonate solution is stabilized at 257L/h, the subsequent operation can be carried out;
under the stirring speed of 1150rpm, namely under the continuous stirring state, adding the cobalt chloride solution with the mass concentration of 78g/L and the ammonium bicarbonate solution with the mass concentration of 182g/L which are subjected to the flow stabilizing operation into the reaction container in the S1 in a stable and uniform manner, wherein the feeding flow rate of the cobalt chloride solution is 122L/h, the feeding flow rate of the ammonium bicarbonate solution is 257L/h, and then, after continuously reacting for 6h at 42 ℃, aging for 10min to obtain cobalt carbonate slurry;
s2, performing solid-liquid separation on the cobalt carbonate slurry obtained in the S1 in a two-in-one device, and mixing the solid obtained after the solid-liquid separation with pure water according to the weight ratio of 1 t: 5m3The slurry is washed, and then the solid is separated in two-in-one equipment after washing, and then the solid is transferred to a tray dryer for drying, wherein the drying temperature is 145 ℃, and the heat preservation time is 60 min;
and S3, screening and packaging the dried product of S2 to obtain the low-chlorine cobalt carbonate product.
Example 8
The embodiment provides a preparation process of low-chlorine cobalt carbonate for superfine cobalt powder, which comprises the following steps:
s1, mixing the powder with 0.6m3Adding water into the reaction kettle, and heating to 40 ℃;
simultaneously starting the transmission of the cobalt chloride solution and the ammonium bicarbonate solution, and carrying out a transmission process for stabilizing the flow for 25min, namely starting the transmission and maintaining the transmission for 25min for stabilizing the flow, wherein when the flow of the cobalt chloride solution is stabilized at 123L/h and the flow of the ammonium bicarbonate solution is stabilized at 255L/h, the subsequent operation can be carried out;
under the stirring speed of 1200rpm, namely under the continuous stirring state, adding the cobalt chloride solution with the mass concentration of 79g/L and the ammonium bicarbonate solution with the mass concentration of 182g/L which are subjected to the flow stabilizing operation into the reaction container in the S1 in a stable and uniform manner, wherein the feeding flow rate of the cobalt chloride solution is 123L/h, the feeding flow rate of the ammonium bicarbonate solution is 255L/h, and then, after continuously reacting for 6h at 40 ℃, aging for 20min to obtain cobalt carbonate slurry;
s2, performing solid-liquid separation on the cobalt carbonate slurry obtained in the S1 in a two-in-one device, and mixing the solid obtained after the solid-liquid separation with pure water according to the weight ratio of 1 t: 4m3The material-liquid ratio of the raw materials is pulped and washed, the materials are separated in a two-in-one device after washing, then the solid is transferred to a tray dryer for drying, the drying temperature is 160 ℃, and the retention time is 30 min;
and S3, screening and packaging the dried product of S2 to obtain the low-chlorine cobalt carbonate product.
Example 9
The embodiment provides a preparation process of low-chlorine cobalt carbonate for superfine cobalt powder, which comprises the following steps:
s1, mixing the powder with 0.6m3Adding water into the reaction kettle, and heating to 41 ℃;
simultaneously starting the transmission of the cobalt chloride solution and the ammonium bicarbonate solution, and carrying out a transmission process for stabilizing the flow for 25min, namely starting the transmission and maintaining the transmission for 25min for stabilizing the flow, wherein when the flow of the cobalt chloride solution is stabilized at 122L/h and the flow of the ammonium bicarbonate solution is stabilized at 263L/h, the subsequent operation can be carried out;
under the stirring speed of 1200rpm, namely under the continuous stirring state, adding the cobalt chloride solution with the mass concentration of 81g/L and the ammonium bicarbonate solution with the mass concentration of 178g/L which are subjected to the flow stabilizing operation into the reaction vessel in the S1 in a stable and uniform manner, wherein the feeding flow rate of the cobalt chloride solution is 122L/h, the feeding flow rate of the ammonium bicarbonate solution is 263L/h, and then after continuously reacting for 6h at 42 ℃, aging for 15min to obtain cobalt carbonate slurry;
s2, performing solid-liquid separation on the cobalt carbonate slurry obtained in the S1 in a two-in-one device, and mixing the solid obtained after the solid-liquid separation with pure water according to the weight ratio of 1 t: 5m3The material-liquid ratio of the raw materials is pulped and washed, the materials are separated in two-in-one equipment after washing, then the solid is transferred to a tray dryer for drying, the drying temperature is 150 ℃, and the retention time is 30 min;
and S3, screening and packaging the dried product of S2 to obtain the low-chlorine cobalt carbonate product.
Example 10
The embodiment provides a preparation process of low-chlorine cobalt carbonate for superfine cobalt powder, which comprises the following steps:
s1, mixing the powder with the grain size of 0.5m3Adding water into the reaction kettle, and heating to 42 ℃;
simultaneously starting the transmission of the cobalt chloride solution and the ammonium bicarbonate solution, and carrying out a transmission process for stabilizing the flow for 30min, namely starting the transmission and maintaining the transmission for 30min for stabilizing the flow, and carrying out subsequent operation when the flow of the cobalt chloride solution is stabilized at 125L/h and the flow of the ammonium bicarbonate solution is stabilized at 264L/h;
under the stirring speed of 1050rpm, namely under the continuous stirring state, adding the cobalt chloride solution with the mass concentration of 82g/L and the ammonium bicarbonate solution with the mass concentration of 179g/L which are subjected to the flow stabilizing operation into the reaction container in the S1 in a stable and uniform manner, wherein the feeding flow rate of the cobalt chloride solution is 125L/h, the feeding flow rate of the ammonium bicarbonate solution is 264L/h, and then, after continuously reacting for 6h at 42 ℃, aging for 20min to obtain cobalt carbonate slurry;
s2, performing solid-liquid separation on the cobalt carbonate slurry obtained in the S1 in a two-in-one device, and mixing the solid obtained after the solid-liquid separation with pure water according to the weight ratio of 1 t: 5m3The slurry is washed, separated in a two-in-one device, and then the solid is transferred to a tray dryer for drying and drying at high temperatureKeeping the temperature at 155 ℃ for 30 min;
and S3, screening and packaging the dried product of S2 to obtain the low-chlorine cobalt carbonate product.
Comparative example 1
The same preparation method as that of example 1 was repeated, except that the mass concentration of the cobalt chloride solution in S2 was 100 g/L.
Comparative example 2
The mass concentration of the cobalt chloride solution in S2 was 60g/L, which was the same as that in example 1.
Comparative example 3
The mass concentration of the ammonium bicarbonate solution in S2 was 200g/L, which was the same as that in the preparation method of example 1.
Comparative example 4
The mass concentration of the ammonium bicarbonate solution in S2 was 120g/L, which was the same as that in the preparation method of example 1.
Comparative example 5
The same preparation method as in example 1 was repeated, except that the feed rate of the cobalt chloride solution in S2 was 240L/h.
Comparative example 6
The same preparation method as that of example 1 was adopted, except that the feed rate of the cobalt chloride solution in S2 was 100L/h.
Comparative example 7
The same preparation process as in example 1 was repeated except that the feed rate of the ammonium bicarbonate solution in S2 was 500L/h.
Comparative example 8
As in the preparation of example 1, the feed rate of the ammonium bicarbonate solution in S2 was varied to 180L/h.
The cobalt carbonate sample obtained in example 1 is subjected to a scanning electron microscope test, fig. 1 is an SEM image of the sample of example 1, and it can be seen from fig. 1 that the cobalt carbonate particles are uniform and have a smooth surface.
Meanwhile, the cobalt carbonate samples of examples 1 to 10 and comparative examples 1 to 8 were measured for chloride ion content by turbidimetry, table 1 is a table of chloride ion content of the above samples, and fig. 2 is a corresponding content chart.
TABLE 1 examples 1 to 10, comparative examples 1 to 8 cobalt carbonate samples have chloride ion contents
| Group of | Chloride ion content (ppm) |
| Example 1 | 10 |
| Example 2 | 8 |
| Example 3 | 6 |
| Example 4 | 5 |
| Example 5 | 11 |
| Example 6 | 12 |
| Example 7 | 9 |
| Example 8 | 7 |
| Example 9 | 8 |
| Example 10 | 6 |
| Comparative example 1 | 84 |
| Comparative example 2 | 31 |
| Comparative example 3 | 56 |
| Comparative example 4 | 40 |
| Comparative example 5 | 113 |
| Comparative example 6 | 88 |
| Comparative example 7 | 65 |
| Comparative example 8 | 72 |
As can be seen from table 1 and fig. 2, the chloride ion content in the cobalt carbonate samples of comparative examples 1 to 8 is significantly higher than that of the cobalt carbonate samples of examples 1 to 10, indicating that the concentration and addition flow rate of the cobalt chloride solution and the concentration and addition flow rate of the ammonium bicarbonate solution have a great influence on the chloride ion content in the cobalt carbonate samples.
Therefore, as can be seen from fig. 1, fig. 2 and table 1, the present invention is more favorable to control the microstructure of cobalt carbonate by controlling the parameter conditions, and reduces the chloride ions wrapped inside and adsorbed on the surface of cobalt carbonate particles, thereby realizing the preparation of low-chloride cobalt carbonate for ultrafine cobalt powder.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are included in the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.
Claims (9)
1. A preparation process of low-chlorine cobalt carbonate for superfine cobalt powder is characterized by comprising the following steps:
s1, adding a cobalt chloride solution with the mass concentration of 78-82 g/L and an ammonium bicarbonate solution with the mass concentration of 178-182 g/L into a reaction container containing pure water stably at a constant speed in a stirring state, continuously reacting for 6-8 hours at 40-42 ℃, and aging to obtain cobalt carbonate slurry;
wherein the stirring speed is 900-1200 rpm, the feed flow rate of the cobalt chloride solution is 115-125L/h, and the feed flow rate of the ammonium bicarbonate solution is 255-265L/h;
and S2, carrying out solid-liquid separation on the cobalt carbonate slurry obtained in the S1, adding water into the solid obtained after the solid-liquid separation, pulping, washing and drying to obtain the low-chlorine cobalt carbonate.
2. The process of claim 1, wherein the amount of water added to the reaction vessel in S1 is 0.5-0.6 m3The water temperature is 40-42 ℃.
3. The process of claim 1, wherein the step of S1 further comprises:
and simultaneously starting the transmission of the cobalt chloride solution and the ammonium bicarbonate solution, carrying out a transmission process for stabilizing the flow for 25-35 min, and adding the cobalt chloride solution and the ammonium bicarbonate solution into the reaction container at a constant speed when the flow of the cobalt chloride solution is maintained at 115-125L/h and the flow of the ammonium bicarbonate solution is maintained at 255-265L/h.
4. The process of claim 1 or 3, wherein in the step S1, the feeding flow rate of the cobalt chloride solution is 118-122L/h, and the feeding flow rate of the ammonium bicarbonate solution is 258-262L/h.
5. The process of claim 1, wherein in step S2, the slurry-liquid ratio of the solid after solid-liquid separation to water is 1 t: (3 to 5) m3。
6. The process of claim 1 or 5, wherein the solid-liquid separation and slurry washing in S2 is a two-in-one device for filtering and washing.
7. The process of claim 5, wherein the number of times of slurry washing in S2 is 1-3.
8. The process of claim 1, wherein the drying in S2 is performed under the following conditions: the drying temperature is 140-160 ℃, and the retention time is 30-60 min.
9. The process for preparing cobaltous carbonate chloride for superfine cobalt powder as claimed in claim 1, wherein in S1, the aging time is 10-20 min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010113493.5A CN113292108A (en) | 2020-02-24 | 2020-02-24 | Preparation process of low-chlorine cobalt carbonate for superfine cobalt powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010113493.5A CN113292108A (en) | 2020-02-24 | 2020-02-24 | Preparation process of low-chlorine cobalt carbonate for superfine cobalt powder |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN113292108A true CN113292108A (en) | 2021-08-24 |
Family
ID=77317746
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202010113493.5A Pending CN113292108A (en) | 2020-02-24 | 2020-02-24 | Preparation process of low-chlorine cobalt carbonate for superfine cobalt powder |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN113292108A (en) |
Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH07196323A (en) * | 1993-12-28 | 1995-08-01 | Sumitomo Metal Mining Co Ltd | Production of cobalt oxide of low sodium content |
| RU2240287C1 (en) * | 2003-03-17 | 2004-11-20 | Институт химии и технологии редких элементов и минерального сырья им. И.В. Тананаева Кольского научного центра Российской академии наук | Bivalent cobalt carbonate production method |
| 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 |
| CN101293677A (en) * | 2007-04-28 | 2008-10-29 | 北京有色金属研究总院 | Method for preparing cobaltic-cobaltous oxide powder with octahedron shape |
| CN106395916A (en) * | 2015-07-31 | 2017-02-15 | 荆门市格林美新材料有限公司 | Preparation method for ultrapure ultrafine cobalt carbonate |
| CN109319846A (en) * | 2018-12-06 | 2019-02-12 | 怀化学院 | The preparation method of cobalt carbonate and the preparation method of cobaltosic oxide |
| CN109987646A (en) * | 2017-12-29 | 2019-07-09 | 格林美（江苏）钴业股份有限公司 | The method for synthesizing big partial size cobalt carbonate successive reaction |
| CN110759387A (en) * | 2018-07-25 | 2020-02-07 | 荆门市格林美新材料有限公司 | Preparation method of manganese-doped basic cobalt carbonate |
-
2020
- 2020-02-24 CN CN202010113493.5A patent/CN113292108A/en active Pending
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH07196323A (en) * | 1993-12-28 | 1995-08-01 | Sumitomo Metal Mining Co Ltd | Production of cobalt oxide of low sodium content |
| RU2240287C1 (en) * | 2003-03-17 | 2004-11-20 | Институт химии и технологии редких элементов и минерального сырья им. И.В. Тананаева Кольского научного центра Российской академии наук | Bivalent cobalt carbonate production method |
| 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 |
| CN101293677A (en) * | 2007-04-28 | 2008-10-29 | 北京有色金属研究总院 | Method for preparing cobaltic-cobaltous oxide powder with octahedron shape |
| CN106395916A (en) * | 2015-07-31 | 2017-02-15 | 荆门市格林美新材料有限公司 | Preparation method for ultrapure ultrafine cobalt carbonate |
| CN109987646A (en) * | 2017-12-29 | 2019-07-09 | 格林美（江苏）钴业股份有限公司 | The method for synthesizing big partial size cobalt carbonate successive reaction |
| CN110759387A (en) * | 2018-07-25 | 2020-02-07 | 荆门市格林美新材料有限公司 | Preparation method of manganese-doped basic cobalt carbonate |
| CN109319846A (en) * | 2018-12-06 | 2019-02-12 | 怀化学院 | The preparation method of cobalt carbonate and the preparation method of cobaltosic oxide |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| JP7021795B2 (en) | Method for preparing indium oxide spherical powder with controllable grain shape | |
| US7695698B2 (en) | Method of producing iron-arsenic compound excellent in crystallinity | |
| JP2023509676A (en) | Preparation method of nickel-rich ternary precursor in which crystal planes grow preferentially by adjusting and controlling the amount of seed crystals added | |
| CN101234769B (en) | Technique for preparing high purity ultra-fine magnesium hydroxide by sodium hydroxide method | |
| CN113830839B (en) | Preparation method and application of flaky aluminum-doped cobalt carbonate | |
| JP2011057518A (en) | High-density nickel-cobalt-manganese coprecipitation hydroxide and method for producing the same | |
| CN111547742B (en) | Sodium-ion battery positive electrode material, preparation method thereof and sodium-ion battery | |
| CN114180644A (en) | Aluminum-doped cobalt carbonate material, preparation method thereof, aluminum-doped cobaltosic oxide and lithium cobaltate cathode material | |
| WO2023024597A1 (en) | Synthesis method for cobalt hydroxide and cobalt hydroxide | |
| CN113292108A (en) | Preparation process of low-chlorine cobalt carbonate for superfine cobalt powder | |
| CN111774583A (en) | Preparation method of superfine silver powder with high tap mass and high specific surface | |
| CN114031105A (en) | Treatment method of copper-containing etching waste liquid | |
| CN106517289A (en) | Method of using low-grade witherite to produce high-purity barium chloride | |
| CN101481090A (en) | Method for preparing sodium percarbonate | |
| CN1220970A (en) | Technology for producing magnesium sulfate in treatment of titanium white waste sulfuric acid | |
| CN113292110B (en) | Preparation method of superfine and highly dispersed spherical cobalt carbonate | |
| CN111362302B (en) | Method for preparing nano titanium dioxide | |
| CN112592180A (en) | Preparation method of low-fluorine high-purity tantalum pentoxide optical coating material | |
| CN112293721A (en) | Edible refined salt and production method thereof | |
| CN114455641B (en) | Preparation method of cobalt carbonate with low chlorine content | |
| CN112875731B (en) | Preparation method of lithium carbonate | |
| CN117865179A (en) | Small-particle-size lithium fluoride and preparation method thereof | |
| CN113371764B (en) | Preparation method of flower-rod-shaped cobalt carbonate | |
| CN111745164B (en) | Preparation method of superfine spherical platinum powder | |
| CN114349050B (en) | Method for preparing high-purity molybdic acid from calcium molybdate |
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 | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20210824 |