CN115108592A - Production method of high-purity cobalt sulfate - Google Patents
Production method of high-purity cobalt sulfate Download PDFInfo
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- CN115108592A CN115108592A CN202210762697.0A CN202210762697A CN115108592A CN 115108592 A CN115108592 A CN 115108592A CN 202210762697 A CN202210762697 A CN 202210762697A CN 115108592 A CN115108592 A CN 115108592A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G51/00—Compounds of cobalt
- C01G51/10—Sulfates
Abstract
The invention discloses a production method of high-purity cobalt sulfate, which comprises the following steps: adding solid cobalt into a reactor through a feed inlet, wherein the more uniform the material is, the smaller the material block is, the better the gap is, the better the stacking thickness is that air can smoothly pass through, and the feed inlet is sealed after the material is added; starting a solution circulating pump, and adding a dissolving solution into the reactor through a dissolving solution inlet; starting heating equipment, and heating the solution to 40-60 ℃; adding compressed air or oxygen into the reactor through an air inlet, wherein the larger the air volume and the air pressure of the compressed air or oxygen is, the better the air volume and the air pressure of the compressed air or oxygen is, but the basis is that a large amount of acid mist is not generated, and meanwhile, comprehensively adjusting all reaction parameters to ensure that Co at a dissolving liquid outlet is 2+ The concentration reaches the set requirement. The invention aims at the problems of low purity and difficult purification of the cobalt sulfate produced by the existing method.
Description
Technical Field
The invention relates to the technical field of a production method of cobalt sulfate, and particularly relates to a production method of high-purity cobalt sulfate.
Background
The method for producing the cobalt sulfate comprises the following steps: the ore is selected, if sulfide ore is roasted, then sulfuric acid is used to leach metals such as cobalt and nickel in oxide, if oxide ore is directly leached by sulfuric acid to obtain mixed solution of sulfate, then cobalt and other metals are separated by chemical and extraction methods, and the produced cobalt sulfate has low purity and is difficult to purify.
Disclosure of Invention
Aiming at the technical problem, the invention provides a production method of high-purity cobalt sulfate.
In order to achieve the above purpose, the technical scheme of the invention is as follows:
a production method of high-purity cobalt sulfate comprises the following steps: adding solid cobalt into a reactor through a feed inlet, wherein the more uniform the material is, the smaller the material block is, the better the gap is, the better the stacking thickness is that air can smoothly pass through, and the feed inlet is sealed after the material is added; starting a solution circulating pump, and adding a dissolving solution into the reactor through a dissolving solution inlet; starting heating equipment, and heating the solution to 40-60 ℃; adding compressed air or oxygen into the reactor through an air inlet, wherein the larger the air volume and the air pressure of the compressed air or oxygen is, the better the air volume and the air pressure of the compressed air or oxygen is, but the basis is that a large amount of acid mist is not generated, and meanwhile, comprehensively adjusting all reaction parameters to ensure that Co at a dissolving liquid outlet is 2+ The concentration reaches the set requirement.
Wherein SO is added to the air line before air or oxygen is introduced into the reactor 2 And after mixing, adding a dissolving solution together to ensure SO 2 Smoothly added to air or oxygen, SO 2 The pressure should be higher than the air or oxygen pressure, SO 2 The mixing degree with air is more than 98%.
Wherein, SO 2 The addition amount of air and SO 2 The ratio of (A) to (B) is 100: 0.5-3, the oxidation is not obviously improved when the proportion is too low, the reducibility of the solution can occur when the proportion is too high, and the metal cobalt dissolved matter is carried out.
Wherein, SO 2 When the mixture with air is added into the reactor, aeration is needed to make the diameter of the bubbles of the mixed gas less than phi 1mm, so that the specific surface area of the reaction is enlarged, the buoyancy of the bubbles is reduced, the floating speed of the bubbles is reduced, the reaction time is prolonged, the oxidability of the solution is improved, the absorption efficiency is improved, and the productivity is improved.
The invention has the beneficial effects that:
（1）adding 0.5-5% SO before adding air into cobalt dissolving reactor 2 ，SO 2 Dissolved in water and separated out SO 3 2+ ；SO 3 2+ Combined with O2 in air to form SO 5 2+ The oxidation potential of the solution can reach 1200mV at most and is much higher than O 2 400 mV, the oxidation efficiency is improved by more than 2 times, and SO 2 And functions as a catalyst.
（2）SO 2 Adding the dissolved solution together with air, and reacting with Co to generate CoSO 4 The reaction equation is as follows:
Co+SO 2 +O 2 =Co 2 ++SO 4 2- ………… ；
SO 2 the sulfuric acid is finally generated after the dissolution liquid is added and participates in the copper dissolution reaction, no redundant substances are generated in the dissolution liquid, no side reaction is generated, and the consumption of the sulfuric acid can be reduced.
(3) The produced cobalt sulfate has high purity, short flow, no oil and can meet the high-grade requirement.
（4）SO 2 When the mixed gas and air are added into the dissolving solution, aeration is carried out, so that the diameter of bubbles of the mixed gas is less than phi 1mm, the specific surface area of the reaction is improved, the floating speed is reduced, the reaction time is prolonged, and the reaction efficiency is improved.
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 is to be understood that these descriptions are only illustrative and are not intended to limit the scope of the present invention. Moreover, in the following description, descriptions of well-known structures and techniques are omitted so as to not unnecessarily obscure the concepts of the present invention.
Example 1
A production method of high-purity cobalt sulfate comprises the following steps: adding solid cobalt into a reactor through a feed inlet, wherein the more uniform the material is, the smaller the material block is, the better the gap is, the better the stacking thickness is that air can smoothly pass through, and the feed inlet is sealed after the material is added; starting a solution circulating pump, and adding a dissolving solution into the reactor through a dissolving solution inlet;starting heating equipment, and heating the solution to 40 ℃; adding compressed air or oxygen into the reactor through an air inlet, wherein the larger the air volume and the air pressure of the compressed air or oxygen is, the better the air volume and the air pressure of the compressed air or oxygen is, but the basis is that a large amount of acid mist is not generated, and meanwhile, comprehensively adjusting all reaction parameters to ensure that Co at a dissolving liquid outlet is 2+ The concentration reaches the set requirement.
Wherein SO is added to the air line before air or oxygen is introduced into the reactor 2 And after mixing, adding a dissolving solution together to ensure SO 2 Smoothly added to air or oxygen, SO 2 The pressure should be higher than the air or oxygen pressure, SO 2 The mixing degree with air is more than 98%.
Wherein, SO 2 The addition amount of air and SO 2 The ratio of (A) to (B) is 100: 0.5, the oxidizability is not obviously improved when the proportion is too low, the reducibility of the solution can occur when the proportion is too high, and the metal cobalt dissolved matter is carried out.
Wherein, SO 2 When the mixture with air is added into the reactor, aeration is needed to make the diameter of the bubbles of the mixed gas less than phi 1mm, so that the specific surface area of the reaction is enlarged, the buoyancy of the bubbles is reduced, the floating speed of the bubbles is reduced, the reaction time is prolonged, the oxidability of the solution is improved, the absorption efficiency is improved, and the productivity is improved.
Example 2
A production method of high-purity cobalt sulfate comprises the following steps: adding solid cobalt into a reactor through a feed inlet, wherein the more uniform the material is, the smaller the material block is, the better the gap is, the better the stacking thickness is that air can smoothly pass through, and the feed inlet is sealed after the material is added; starting a solution circulating pump, and adding a dissolving solution into the reactor through a dissolving solution inlet; starting heating equipment, and heating the solution to 60 ℃; adding compressed air or oxygen into the reactor through an air inlet, wherein the larger the air volume and the air pressure of the compressed air or oxygen is, the better the air volume and the air pressure of the compressed air or oxygen is, but the basis is that a large amount of acid mist is not generated, and meanwhile, comprehensively adjusting all reaction parameters to ensure that Co at a dissolving liquid outlet is 2+ The concentration reaches the set requirement.
Wherein SO is added to the air line before air or oxygen is introduced into the reactor 2 And after mixingAdding dissolving solution together to ensure SO 2 Smoothly added to air or oxygen, SO 2 The pressure should be higher than the air or oxygen pressure, SO 2 The mixing degree with air is more than 98%.
Wherein, SO 2 The addition amount of air and SO 2 The ratio of (A) to (B) is 100: 3, the oxidizability is not obviously improved when the proportion is too low, the reducibility of the solution can occur when the proportion is too high, and the metal cobalt dissolved matter is carried out.
Wherein, SO 2 When the mixture with air is added into the reactor, aeration is needed to make the diameter of the bubbles of the mixed gas less than phi 1mm, so that the specific surface area of the reaction is enlarged, the buoyancy of the bubbles is reduced, the floating speed of the bubbles is reduced, the reaction time is prolonged, the oxidability of the solution is improved, the absorption efficiency is improved, and the productivity is improved.
Example 3
(1) Adding solid cobalt (cobalt blocks, cobalt skins and cobalt powder) into a reactor, wherein the more uniform the material is, the smaller the material block is, the smaller the gap is, the better the material block is, the stacking thickness is that air can smoothly pass through, then, a feeding opening is closed, the diameter phi of the reactor is 3.5m, the height of the reactor is 5m, the cobalt amount is added once, and 2.5 tons of the material is added;
(2) starting a circulating pump, adding a dissolving solution into the reactor, wherein the components of the dissolving solution comprise sulfuric acid, water, a solution and cobalt sulfate, the concentration of the sulfuric acid is about 50g/L, and Co is 2+ The concentration is about 15g/L, the circulating pump adopts a corrosion-resistant and wear-resistant chemical pump, and the circulating amount is 65m 3/h.
(3) Starting heating equipment, and heating the solution to 50 ℃;
(4) compressed air is introduced into the reactor at a flow rate of 85m 3 H, purifying the air before adding the air;
(5) introducing SO into compressed air 2 Flow rate of 2.2m 3 /h，SO 2 Before the gas is added, the gas is purified,
(6) air and SO 2 Before entering the solution, three-stage mixing is carried out by adopting a Venturi mixer, a swirl mixer and a pipeline mixer to ensure that the mixing degree of the Venturi mixer, the swirl mixer and the pipeline mixer reaches more than 98 percent, the aeration is carried out by adopting the swirl mixer when the solution is added, and the diameter of the added gas bubbles is less than phi 1 mm;
(7) regulating deviceThe flow rate of the whole circulating pump is adjusted to ensure that the outlet Co of the reactor 2+ The content reaches about 120g/L, and the solution is discharged from a solution outlet and enters an evaporator;
(8) the diameter of the evaporator is 1.5m, the evaporation capacity per hour is 8t/h, the evaporator is heated by steam, the working temperature is 170 ℃, and after evaporation and concentration, the solution is sent to crystallization equipment through a pipeline when the specific gravity of the solution reaches 1.65 g/L.
(9) The cobalt sulfate crystallization adopts five-stage continuous crystallization, the diameter of the crystallizer is phi 2m, the height of the crystallizer is 3.5m, the power of a stirring paddle is 18KW, the temperature of each stage of crystallization is 95 ℃, 85 ℃, 70 ℃, 55 ℃ and 40 ℃, and the cobalt sulfate is conveyed into solid-liquid separation equipment through a pipeline after the crystallization is finished.
(10) The solid-liquid separation equipment adopts a continuous discharge centrifuge, 5 tons of cobalt sulfate crystals are separated out every hour, and 15 tons of cobalt sulfate crystals are produced every day by adopting intermittent operation.
(11) And drying the cobalt sulfate crystals by adopting a fluidized bed dryer after the cobalt sulfate crystals are produced, wherein the air inlet temperature of the dryer is 140 ℃, the bed width is 1m, and the length is 6 m. The equipment has low air inlet temperature, is close to static drying, and the dried product has no dehydration phenomenon, small abrasion, crystal surface and clear edges and corners.
(12) And conveying the dried cobalt sulfate to a packaging machine, bagging, weighing, packaging and selling, wherein the yield of the cobalt sulfate is about 15 tons.
(13) The impurity content of the product is as follows: (%)
It is to be understood that the above-described embodiments of the present invention are merely illustrative of or explaining the principles of the invention and are not to be construed as limiting the invention. Therefore, any modification, equivalent replacement, improvement and the like made without departing from the spirit and scope of the present invention should be included in the protection scope of the present invention. Further, it is intended that the appended claims cover all such variations and modifications as fall within the scope and boundaries of the appended claims or the equivalents of such scope and boundaries.
Claims (4)
1. The production method of the high-purity cobalt sulfate is characterized by comprising the following steps: adding solid cobalt into a reactor through a feed inlet, wherein the more uniform the material is, the smaller the material block is, the better the gap is, the better the stacking thickness is that air can smoothly pass through, and the feed inlet is sealed after the material is added; starting a solution circulating pump, and adding a dissolving solution into the reactor through a dissolving solution inlet; starting heating equipment, and heating the solution to 40-60 ℃; adding compressed air or oxygen into the reactor through an air inlet, wherein the larger the air volume and the air pressure of the compressed air or oxygen is, the better the air volume and the air pressure of the compressed air or oxygen is, but the basis is that a large amount of acid mist is not generated, and meanwhile, comprehensively adjusting all reaction parameters to ensure that Co at a dissolving liquid outlet is 2+ The concentration reaches the set requirement.
2. The method for producing high-purity cobalt sulfate according to claim 1, wherein SO is added to the air pipeline before the air or oxygen is introduced into the reactor 2 And after mixing, adding a dissolving solution together to ensure SO 2 Smoothly added to air or oxygen, SO 2 The pressure should be higher than the air or oxygen pressure, SO 2 The mixing degree with air is more than 98%.
3. The method for producing high-purity cobalt sulfate according to claim 2, wherein SO is used as SO 2 The addition amount of air and SO 2 The ratio of (A) to (B) is 100: 0.5-3, the oxidation is not obviously improved when the proportion is too low, the reducibility of the solution can occur when the proportion is too high, and the metal cobalt dissolved matter is carried out.
4. The method for producing high-purity cobalt sulfate according to claim 3, wherein SO is used as SO 2 When the mixture with air is added into the reactor, aeration is needed to make the diameter of the bubbles of the mixed gas less than phi 1mm, so that the specific surface area of the reaction is enlarged, the buoyancy of the bubbles is reduced, the floating speed of the bubbles is reduced, the reaction time is prolonged, the oxidability of the solution is improved, the absorption efficiency is improved, and the productivity is improved.
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| CN202210762697.0A CN115108592A (en) | 2022-06-30 | 2022-06-30 | Production method of high-purity cobalt sulfate |
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| CN202210762697.0A CN115108592A (en) | 2022-06-30 | 2022-06-30 | Production method of high-purity cobalt sulfate |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB350050A (en) * | 1930-03-13 | 1931-06-11 | Metallgesellschaft Ag | Process for the production of sulphates |
| FR1432464A (en) * | 1965-05-11 | 1966-03-18 | Sherritt Gordon Mines Ltd | Treatment of laterites |
| CN101768669A (en) * | 2010-01-28 | 2010-07-07 | 浙江华友钴业股份有限公司 | Method for processing cobalt-copper alloy at room temperature |
| CN105803192A (en) * | 2016-03-01 | 2016-07-27 | 浙江华友钴业股份有限公司 | Method for dissolving heavy metal at low temperature through gas mixture of air and sulfur dioxide |
| CN109911928A (en) * | 2019-03-20 | 2019-06-21 | 金川集团股份有限公司 | A method of fast instant copper |
-
2022
- 2022-06-30 CN CN202210762697.0A patent/CN115108592A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB350050A (en) * | 1930-03-13 | 1931-06-11 | Metallgesellschaft Ag | Process for the production of sulphates |
| FR1432464A (en) * | 1965-05-11 | 1966-03-18 | Sherritt Gordon Mines Ltd | Treatment of laterites |
| CN101768669A (en) * | 2010-01-28 | 2010-07-07 | 浙江华友钴业股份有限公司 | Method for processing cobalt-copper alloy at room temperature |
| CN105803192A (en) * | 2016-03-01 | 2016-07-27 | 浙江华友钴业股份有限公司 | Method for dissolving heavy metal at low temperature through gas mixture of air and sulfur dioxide |
| CN109911928A (en) * | 2019-03-20 | 2019-06-21 | 金川集团股份有限公司 | A method of fast instant copper |
Non-Patent Citations (1)
| Title |
|---|
| 童辉 等: "《无机与分析化学》", 武汉理工大学出版社, pages: 72 * |
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