CN110578052A - Method for reducing calcium content in feed liquid with high calcium sulfate content - Google Patents
Method for reducing calcium content in feed liquid with high calcium sulfate content Download PDFInfo
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- CN110578052A CN110578052A CN201911006905.9A CN201911006905A CN110578052A CN 110578052 A CN110578052 A CN 110578052A CN 201911006905 A CN201911006905 A CN 201911006905A CN 110578052 A CN110578052 A CN 110578052A
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B1/00—Preliminary treatment of ores or scrap
- C22B1/02—Roasting processes
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/22—Treatment or purification of solutions, e.g. obtained by leaching by physical processes, e.g. by filtration, by magnetic means, or by thermal decomposition
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/44—Treatment or purification of solutions, e.g. obtained by leaching by chemical processes
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Abstract
The invention provides a method for reducing the calcium content in feed liquid with high calcium sulfate content, belonging to the technical field of hydrometallurgy. The method for reducing the calcium content in the feed liquid with high calcium sulfate content, provided by the invention, comprises the following steps: mixing the feed liquid with high calcium sulfate content with calcium sulfate crystal seeds, and sequentially carrying out precipitation treatment, aging and solid-liquid separation; wherein the content of calcium sulfate in the feed liquid with high calcium sulfate content is 2.30-2.56 g/L, and the pH value is 4.0-4.5; the particle size of the calcium sulfate seed crystal is 11-18 mu m. According to the invention, calcium sulfate crystal seeds with specific particle sizes are adopted to induce calcium precipitation, so that the content of calcium sulfate in the feed liquid can be effectively reduced, frequent cleaning of calcium sulfate precipitates in the extraction tank in the subsequent calcium extraction and removal process is avoided, manpower and material resources are saved, and the production efficiency is improved. In addition, the method provided by the invention has the advantages of simple steps, strong operability and easiness in large-scale production.
Description
Technical Field
the invention relates to the technical field of wet metallurgy, in particular to a method for reducing the calcium content in feed liquid with high calcium sulfate content.
background
In the process of smelting metals by a wet method, in order to ensure that the smelting process is smoothly carried out, impurity removal needs to be carried out on raw material leaching liquid, and calcium is one of main impurity elements. The existing calcium removal methods mainly comprise fluoride calcium removal and extraction calcium removal. The fluoride calcium removal is to remove copper and iron from the leaching solution, control the system at a specific pH value and temperature, and add fluoride (such as sodium fluoride or ammonium fluoride) to form calcium fluoride precipitate. However, fluorine is remained in the feed liquid after the calcium removal of the fluoride, which pollutes the environment, and the discharge concentration of the fluoride after the treatment of the waste liquid is allowed to be less than 10mg/L by the national Integrated wastewater discharge Standard, so the extraction calcium removal is mainly adopted in the industry at present. The extraction decalcification is to remove copper and iron from the leaching solution, control the system at a specific pH value, and extract and decalcification by using an extractant (such as P204).
The mineral raw materials are leached by using sulfuric acid, and calcium impurities in an obtained system mainly exist in a form of calcium sulfate. At present, in hydrometallurgical production, calcium carbonate is often adopted to adjust the pH value of an acidic leaching material liquid, so that the content of calcium sulfate in a system is too high, a supersaturated calcium sulfate material liquid is formed, and the material liquid after copper and iron removal can form a large amount of calcium sulfate precipitates in an extraction tank in a subsequent calcium extraction and removal process to block pipelines of the extraction tank. Therefore, the calcium sulfate precipitate in the extraction tank needs to be cleaned frequently and regularly, the production is forced to be interrupted, manpower and material resources are wasted, and the production efficiency is reduced.
Disclosure of Invention
The invention aims to provide a method for reducing the calcium content in feed liquid with high calcium sulfate content, which can effectively reduce the calcium sulfate content in the feed liquid, avoid frequently cleaning calcium sulfate precipitates in an extraction tank in the subsequent calcium extraction and removal process, save manpower and material resources and improve the production efficiency.
In order to achieve the above object, the present invention provides the following technical solutions:
The invention provides a method for reducing the calcium content in feed liquid with high calcium sulfate content, which comprises the following steps:
Mixing the feed liquid with high calcium sulfate content with calcium sulfate crystal seeds, and sequentially carrying out precipitation treatment, aging and solid-liquid separation;
Wherein the content of calcium sulfate in the feed liquid with high calcium sulfate content is 2.30-2.56 g/L, and the pH value is 4.0-4.5; the particle size of the calcium sulfate seed crystal is 11-18 mu m.
Preferably, the preparation method of the feed liquid with high calcium sulfate content comprises the following steps:
Providing a raw material leaching liquid, wherein the content of calcium sulfate in the raw material leaching liquid is 1.07-1.52 g/L, and the pH value is 1.5-2.5;
and adjusting the pH value of the raw material leaching liquid by adopting calcium carbonate to carry out copper and iron impurity removal treatment to obtain the high-calcium-sulfate-content liquid.
preferably, the preparation method of the calcium sulfate seed crystal comprises the following steps:
And roasting the calcium sulfate dihydrate or the precipitate obtained by the solid-liquid separation, and sequentially performing ball milling and screening on the obtained roasted material to obtain the calcium sulfate crystal seed.
preferably, the roasting temperature is 100-300 ℃, and the roasting time is 0.5-3 h.
Preferably, the dosage ratio of the feed liquid with high calcium sulfate content to the calcium sulfate seed crystal is 1L: (1-30) g.
Preferably, the precipitation treatment is carried out under the condition of stirring, and the rotating speed of the stirring is 150-240 r/min.
preferably, the time of the precipitation treatment is 0.5-2 h.
Preferably, the aging time is 0.5-4 h.
Preferably, the solid-liquid separation mode is filtration.
The invention provides a method for reducing the calcium content in feed liquid with high calcium sulfate content, which comprises the following steps: mixing the feed liquid with high calcium sulfate content with calcium sulfate crystal seeds, and sequentially carrying out precipitation treatment, aging and solid-liquid separation; wherein the content of calcium sulfate in the feed liquid with high calcium sulfate content is 2.30-2.56 g/L, and the pH value is 4.0-4.5; the particle size of the calcium sulfate seed crystal is 11-18 mu m. According to the invention, calcium sulfate crystal seeds with specific particle sizes are adopted to induce calcium precipitation, so that the content of calcium sulfate in the feed liquid can be effectively reduced, frequent cleaning of calcium sulfate precipitates in the extraction tank in the subsequent calcium extraction and removal process is avoided, manpower and material resources are saved, and the production efficiency is improved. In addition, the method provided by the invention has the advantages of simple steps, strong operability and easiness in large-scale production.
Detailed Description
The invention provides a method for reducing the calcium content in feed liquid with high calcium sulfate content, which comprises the following steps:
mixing the feed liquid with high calcium sulfate content with calcium sulfate crystal seeds, and sequentially carrying out precipitation treatment, aging and solid-liquid separation;
Wherein the content of calcium sulfate in the feed liquid with high calcium sulfate content is 2.30-2.56 g/L, and the pH value is 4.0-4.5; the particle size of the calcium sulfate seed crystal is 11-18 mu m.
in the invention, the content of calcium sulfate in the feed liquid with high content of calcium sulfate is 2.30-2.56 g/L, and the pH value is 4.0-4.5; the preparation method of the feed liquid with high calcium sulfate content preferably comprises the following steps:
providing a raw material leaching liquid, wherein the content of calcium sulfate in the raw material leaching liquid is 1.07-1.52 g/L, and the pH value is 1.5-2.5;
And adjusting the pH value of the raw material leaching liquid by adopting calcium carbonate to carry out copper and iron impurity removal treatment to obtain the high-calcium-sulfate-content liquid.
In the invention, the raw material leaching liquid is preferably a liquid obtained by leaching cobalt concentrate with sulfuric acid; the content of calcium sulfate in the raw material leaching liquid is preferably 1.07-1.52 g/L, more preferably 1.20-1.40 g/L, and the pH value is preferably 1.5-2.5, more preferably 1.7-2.2. The method preferably adopts calcium carbonate to adjust the pH value of the raw material leaching liquid so as to carry out copper and iron impurity removal treatment, and specifically comprises the steps of adding calcium carbonate into the raw material leaching liquid, reacting the calcium carbonate with sulfuric acid in a system to generate calcium sulfate, carbon dioxide and water, raising the pH value of the system to be less than or equal to 3.0, extracting by using an N902 extracting agent to remove copper, adjusting the pH value of raffinate to be 4.0-4.5 by using the calcium carbonate, carrying out precipitation and iron removal, and finally obtaining the high-calcium sulfate content liquid with the pH value of 4.0-4.5.
After the feed liquid with high calcium sulfate content is obtained, the feed liquid with high calcium sulfate content is mixed with the calcium sulfate crystal seeds, and then precipitation treatment, aging and solid-liquid separation are sequentially carried out. In the invention, the particle size of the calcium sulfate seed crystal is 11-18 μm, preferably 11-16 μm, more preferably 11-14 μm, and even more preferably 11-13 μm; according to the invention, by controlling the particle size of the calcium sulfate seed crystal within the above range, the induced nucleation is favorably ensured, the formation of calcium sulfate precipitate is promoted, the surface activity of the seed crystal is low due to the excessively large particle size, and the nucleation and the growth of the seed crystal are not favorably realized due to the excessively small particle size, so that the calcium sulfate removal effect is influenced.
In the present invention, the preparation method of the calcium sulfate seed crystal preferably comprises the following steps:
And roasting the calcium sulfate dihydrate or the precipitate obtained by the solid-liquid separation, and sequentially performing ball milling and screening on the obtained roasted material to obtain the calcium sulfate crystal seed.
In the invention, the roasting temperature is preferably 100-300 ℃, and more preferably 120-180 ℃; the time is preferably 0.5 to 3 hours, and more preferably 1 to 2 hours. The atmosphere conditions in the calcination process are not particularly limited, and the calcination may be carried out in an air atmosphere or under a vacuum condition. The invention preferably carries out roasting under the above conditions, the obtained roasted material is calcium sulfate hemihydrate, the porosity is high, the individual microcrystals are more, the solubility under the room temperature condition is higher than that of calcium sulfate dihydrate, and the calcium sulfate hemihydrate is used as a calcium sulfate crystal seed to treat the feed liquid with high calcium sulfate content, thereby being beneficial to generating the calcium sulfate dihydrate and promoting the calcium sulfate precipitation in the system.
the invention has no special limitation on the ball milling and screening, and can obtain the calcium sulfate crystal seeds with required granularity.
In the invention, the mixing of the feed liquid with high calcium sulfate content and the calcium sulfate seed crystal is preferably to add the calcium sulfate seed crystal into the feed liquid with high calcium sulfate content. In the invention, the dosage ratio of the feed liquid with high calcium sulfate content to the calcium sulfate seed crystal is preferably 1L: (1-30) g, more preferably 1L: (2-20) g, more preferably 1L: (3-10) g. According to the invention, the dosage ratio of the feed liquid with high calcium sulfate content to the calcium sulfate seed crystal is preferably controlled within the above range, so that calcium sulfate can be ensured to gather on the surface of the seed crystal and grow, and the calcium ions and sulfate ions in the feed liquid can be promoted to form precipitate.
In the invention, the precipitation treatment is preferably carried out under the condition of stirring, and the rotating speed of the stirring is preferably 150-240 r/min, and more preferably 170-220 r/min; the time of the precipitation treatment is preferably 0.5-2 h, and more preferably 1-1.5 h; the precipitation treatment is preferably carried out at room temperature, i.e. without additional heating or cooling. In the invention, the aging time is preferably 0.5-4 h, and more preferably 1-2 h; the aging is preferably carried out at room temperature, i.e. without additional heating or cooling. The invention preferably carries out precipitation treatment and aging under the conditions, can ensure that the seed crystals are uniformly dispersed and suspended in the feed liquid, is favorable for providing a growing interface of the seed crystals, promotes calcium ions and sulfate ions in the feed liquid to form precipitate and separate out, and is favorable for successfully removing calcium sulfate through subsequent solid-liquid separation.
The solid-liquid separation method is not particularly limited, and a method known to those skilled in the art may be used. In the present invention, the solid-liquid separation is preferably performed by filtration.
In the invention, after solid-liquid separation, a precipitate and a calcium-removal leaching feed liquid are obtained, wherein the precipitate is a calcium sulfate crystal, namely calcium sulfate dihydrate, and the purity is more than 98% (namely the content of the calcium sulfate dihydrate in the precipitate is more than 98%), and the calcium sulfate crystal seed can be prepared by the method; the calcium content in the decalcified leaching liquid is obviously reduced, calcium sulfate precipitation is favorably reduced in the subsequent extraction decalcifying process, the cleaning period of the extraction tank is prolonged, specifically, if calcium sulfate crystal seeds are not added for treatment, the copper and iron removed leaching liquid is directly subjected to extraction decalcification, and the cleaning period of the extraction tank is about 2 months; after the calcium sulfate crystal seeds are used for treatment by adopting the method provided by the invention, the cleaning period of the extraction tank is about 3.5 months.
The technical solution of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
roasting calcium sulfate dihydrate at 150 ℃ for 2 hours, and performing ball milling and screening on the roasted material to obtain calcium sulfate crystal seeds with the particle size of 11-13 microns;
Leaching cobalt concentrate with sulfuric acid to obtain a raw material leaching liquid (the content of calcium sulfate is 1.3g/L, the pH value is 2.0), adjusting the pH value of the raw material leaching liquid with calcium carbonate to carry out copper and iron impurity removal treatment (specifically, carrying out extraction and copper removal by using an N902 extracting agent) to obtain a high calcium sulfate content liquid (the content of calcium sulfate is 2.56g/L, the pH value is 4.0), adding calcium sulfate seed crystals (3 g of calcium sulfate seed crystals are added in each liter of high calcium sulfate content liquid) under the condition of 200r/min, stirring for 1 hour at room temperature, then aging for 1 hour, and filtering to obtain a precipitate and the calcium removal leaching liquid; wherein the precipitate is calcium sulfate crystal (purity is more than 98%), and the content of calcium sulfate in the calcium-removing leaching liquid is 1.82 g/L.
example 2
Roasting calcium sulfate dihydrate at 150 ℃ for 2 hours, and performing ball milling and screening on the roasted material to obtain calcium sulfate crystal seeds with the particle size of 11-13 microns;
leaching cobalt concentrate with sulfuric acid to obtain a raw material leaching liquid (the content of calcium sulfate is 1.3g/L, the pH value is 2.0), adjusting the pH value of the raw material leaching liquid with calcium carbonate to carry out copper and iron impurity removal treatment (specifically, carrying out extraction and copper removal by using an N902 extracting agent) to obtain a high calcium sulfate content liquid (the content of calcium sulfate is 2.56g/L, the pH value is 4.0), adding calcium sulfate seed crystals (5 g of calcium sulfate seed crystals are added to each liter of high calcium sulfate content liquid) under the condition of 200r/min, stirring for 1.5 hours at room temperature, then aging for 1 hour, and filtering to obtain a precipitate and the calcium removal leaching liquid; wherein the precipitate is calcium sulfate crystal (purity is more than 98%), and the content of calcium sulfate in the calcium-removing leaching liquid is 1.78 g/L.
Example 3
roasting calcium sulfate dihydrate at 105 ℃ for 2 hours, and performing ball milling and screening on the roasted material to obtain calcium sulfate crystal seeds with the particle size of 11-13 microns;
Leaching cobalt concentrate with sulfuric acid to obtain a raw material leaching liquid (the content of calcium sulfate is 1.3g/L, the pH value is 2.0), adjusting the pH value of the raw material leaching liquid with calcium carbonate to carry out copper and iron impurity removal treatment (specifically, carrying out extraction and copper removal by using an N902 extracting agent) to obtain a high calcium sulfate content liquid (the content of calcium sulfate is 2.56g/L, the pH value is 4.0), adding calcium sulfate seed crystals (5 g of calcium sulfate seed crystals are added to each liter of high calcium sulfate content liquid) under the condition of 200r/min, stirring for 1.5 hours at room temperature, then aging for 1 hour, and filtering to obtain a precipitate and the calcium removal leaching liquid; wherein the precipitate is calcium sulfate crystal (purity is more than 98%), and the content of calcium sulfate in the calcium-removing leaching liquid is 1.86 g/L.
example 4
roasting the calcium sulfate crystal obtained in the example 2 at 150 ℃ for 2 hours, and performing ball milling and screening on the roasted material to obtain a calcium sulfate crystal seed with the particle size of 11-13 microns;
Leaching cobalt concentrate with sulfuric acid to obtain a raw material leaching liquid (the content of calcium sulfate is 1.3g/L, the pH value is 2.0), adjusting the pH value of the raw material leaching liquid with calcium carbonate to carry out copper and iron impurity removal treatment (specifically, carrying out extraction and copper removal by using an N902 extracting agent) to obtain a high calcium sulfate content liquid (the content of calcium sulfate is 2.56g/L, the pH value is 4.0), adding calcium sulfate seed crystals (3 g of calcium sulfate seed crystals are added in each liter of high calcium sulfate content liquid) under the condition of 200r/min, stirring for 1.5h at room temperature, then aging for 1h, and filtering to obtain a precipitate and the calcium removal leaching liquid; wherein the precipitate is calcium sulfate crystal (purity is more than 98%), and the content of calcium sulfate in the calcium-removing leaching liquid is 1.79 g/L.
example 5
Roasting calcium sulfate dihydrate at 150 ℃ for 2 hours, and performing ball milling and screening on the roasted material to obtain calcium sulfate crystal seeds with the particle size of 17-18 microns;
Leaching cobalt concentrate with sulfuric acid to obtain a raw material leaching liquid (the content of calcium sulfate is 1.3g/L, the pH value is 2.0), adjusting the pH value of the raw material leaching liquid with calcium carbonate to carry out copper and iron impurity removal treatment (specifically, carrying out extraction and copper removal by using an N902 extracting agent) to obtain a high calcium sulfate content liquid (the content of calcium sulfate is 2.56g/L, the pH value is 4.0), adding calcium sulfate seed crystals (5 g of calcium sulfate seed crystals are added to each liter of high calcium sulfate content liquid) under the condition of 200r/min, stirring for 1.5 hours at room temperature, then aging for 1 hour, and filtering to obtain a precipitate and the calcium removal leaching liquid; wherein the precipitate is calcium sulfate crystal (purity is more than 98%), and the content of calcium sulfate in the calcium-removing leaching liquid is 1.83 g/L.
Example 6
using the precipitate obtained by filtration in example 4 as seed crystal (particle size of 11-13 μm);
leaching cobalt concentrate with sulfuric acid to obtain a raw material leaching liquid (the content of calcium sulfate is 1.3g/L, the pH value is 2.0), adjusting the pH value of the raw material leaching liquid with calcium carbonate to carry out copper and iron impurity removal treatment (specifically, carrying out extraction and copper removal by using an N902 extracting agent) to obtain a high calcium sulfate content liquid (the content of calcium sulfate is 2.56g/L, the pH value is 4.0), adding calcium sulfate seed crystals (5 g of seed crystals are added to each liter of high calcium sulfate content liquid) under the condition of 200r/min, stirring for 1.5 hours at room temperature, then aging for 1 hour, and filtering to obtain a precipitate and the calcium removal leaching liquid; wherein the precipitate is calcium sulfate crystal (purity is more than 98%), and the content of calcium sulfate in the calcium-removing leaching liquid is 1.87 g/L.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (9)
1. a method for reducing the calcium content in feed liquid with high calcium sulfate content is characterized by comprising the following steps:
Mixing the feed liquid with high calcium sulfate content with calcium sulfate crystal seeds, and sequentially carrying out precipitation treatment, aging and solid-liquid separation;
Wherein the content of calcium sulfate in the feed liquid with high calcium sulfate content is 2.30-2.56 g/L, and the pH value is 4.0-4.5; the particle size of the calcium sulfate seed crystal is 11-18 mu m.
2. The method according to claim 1, wherein the preparation method of the feed liquid with high calcium sulfate content comprises the following steps:
Providing a raw material leaching liquid, wherein the content of calcium sulfate in the raw material leaching liquid is 1.07-1.52 g/L, and the pH value is 1.5-2.5;
and adjusting the pH value of the raw material leaching liquid by adopting calcium carbonate to carry out copper and iron impurity removal treatment to obtain the high-calcium-sulfate-content liquid.
3. The method according to claim 1, wherein the preparation method of the calcium sulfate seed crystal comprises the following steps:
And roasting the calcium sulfate dihydrate or the precipitate obtained by the solid-liquid separation, and sequentially performing ball milling and screening on the obtained roasted material to obtain the calcium sulfate crystal seed.
4. The method according to claim 3, wherein the roasting temperature is 100-300 ℃ and the roasting time is 0.5-3 h.
5. The method according to any one of claims 1 to 4, wherein the dosage ratio of the feed liquid with high calcium sulfate content to the calcium sulfate seed crystal is 1L: (1-30) g.
6. The method according to claim 1, wherein the precipitation treatment is carried out under stirring at a rotation speed of 150 to 240 r/min.
7. The method according to claim 1 or 6, wherein the precipitation treatment time is 0.5-2 h.
8. the method according to claim 1, wherein the aging time is 0.5 to 4 hours.
9. The method according to claim 1, wherein the solid-liquid separation is by filtration.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111411226A (en) * | 2020-04-08 | 2020-07-14 | 甘肃稀土新材料股份有限公司 | Method for removing calcium ions in rare earth sulfate extraction separation process |
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Cited By (2)
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| CN111411226A (en) * | 2020-04-08 | 2020-07-14 | 甘肃稀土新材料股份有限公司 | Method for removing calcium ions in rare earth sulfate extraction separation process |
| CN111411226B (en) * | 2020-04-08 | 2022-04-05 | 甘肃稀土新材料股份有限公司 | Method for removing calcium ions in rare earth sulfate extraction separation process |
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Application publication date: 20191217 |
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| RJ01 | Rejection of invention patent application after publication |