CN115744942A - Method for removing lepidolite leaching brine impurities by using lithium precipitation mother liquor - Google Patents
Method for removing lepidolite leaching brine impurities by using lithium precipitation mother liquor Download PDFInfo
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- CN115744942A CN115744942A CN202211498797.3A CN202211498797A CN115744942A CN 115744942 A CN115744942 A CN 115744942A CN 202211498797 A CN202211498797 A CN 202211498797A CN 115744942 A CN115744942 A CN 115744942A
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
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Abstract
The invention discloses a method for removing lepidolite leaching brine impurities by using lithium precipitation mother liquor, and belongs to the technical field of lepidolite lithium precipitation mother liquor and recovery and impurity removal. According to the invention, a large amount of lithium precipitation mother liquor remained in a salt lake brine, spodumene or lepidolite lithium extraction process is fully utilized, sodium carbonate is replaced by the lithium precipitation mother liquor to serve as an impurity removing agent of a lepidolite lithium extraction leaching solution, and a large amount of metal impurity ions in the leaching solution are removed by matching with a heating effect of microwave treatment under high pressure; the process effectively utilizes the lithium deposition mother liquor, has high metal impurity ion removal rate, greatly reduces the subsequent evaporation concentration amount, and achieves the purposes of optimizing the process and saving the cost.
Description
Technical Field
The invention belongs to the technical field of lithium precipitation mother liquor of lepidolite and recovery and impurity removal, and particularly relates to a method for removing impurities in lepidolite leaching brine by using the lithium precipitation mother liquor.
Background
The lithium resource is mainly caused in salt lake brine and granite pegmatite type mineral deposits, wherein the granite pegmatite type mineral deposits are widely distributed and mainly exploit spodumene, lepidolite, petalite and the like. The lepidolite is in the form of short-column, small flake geometry or large plate crystals, wherein Li 2 The theoretical value of the O content is 3.87-5.83%, and the O content simultaneously contains MgO, feO, caO and the like; for example, the polymetallic deposit of tantalum-niobium ore associated with lepidolite, rubidium and cesium in Yichun Jiangxi is the largest associated lepidolite deposit in the world and is the main lithium resource which is being exploited and utilized in ChinaOne of them.
The existing lepidolite lithium extraction and series processes mainly comprises the steps of roasting, leaching, purifying and precipitating the lepidolite to obtain a crude lithium carbonate product and a lithium precipitation mother solution, and further processing the lithium precipitation mother solution to improve the lithium recovery rate. The main problems of the series of processes at present are as follows: the lepidolite has low lithium content, various impurities, multiple lithium extraction process steps, high energy consumption, various and large amount of used substances, and high production cost. The leaching solution after the lepidolite roasting leaching contains a large amount of impurity ions such as iron, manganese, calcium, magnesium and the like, and the impurity ions are mainly removed by adding sodium carbonate or sodium hydroxide at present, but the required dosage is large and partial lithium ion precipitation is easy to remove. Based on this, it is necessary to find another process to replace the subsequent purification treatment of the leachate.
Disclosure of Invention
Aiming at the problem of higher production cost caused by adopting a large amount of carbonate to purify metal impurity ions in the leaching solution in the existing lepidolite lithium extraction process, the invention aims to provide a method for removing lepidolite leaching brine impurities by using a lithium precipitation mother solution. According to the invention, the leachate is subjected to impurity removal by using the carbonate remained in the lithium precipitation mother liquor, so that the lithium precipitation mother liquor can be effectively utilized, and the subsequent evaporation and concentration amount is greatly reduced, thereby achieving the purposes of optimizing the process and saving the cost.
In order to achieve the purpose, the invention specifically adopts the following technical scheme:
the invention provides a method for removing lepidolite leaching brine impurities by using lithium precipitation mother liquor, which comprises the following steps:
step 1): mixing lepidolite ore and sulfate, roasting, grinding and leaching to obtain leached brine;
step 2): transferring the leached brine obtained in the step 1) into a reaction kettle, then gradually pumping lithium precipitation mother liquor into the reaction kettle, continuously stirring under positive pressure and controlled temperature, preserving heat, standing, and filtering to obtain impurity-removed filtrate;
and step 3): and (3) carrying out post-treatment on the impurity-removed filtrate obtained in the step 2) to obtain battery-grade lithium carbonate.
Preferably, the leaching brine in the step 1) contains metal impurity ions of iron, zinc, manganese, calcium and magnesium.
Preferably, the flow rate of the step-by-step pumped lithium precipitation mother liquor in the step 2) is controlled to be 3-7m 3 /h。
Preferably, the lithium precipitation mother liquor is lithium precipitation mother liquor obtained by adding sodium carbonate to react in a process of extracting lithium from salt lake brine, spodumene or lepidolite.
Preferably, the lithium precipitation mother liquor comprises the following main components: 78-110g/L of sulfate ions, 11-18g/L of carbonate ions and 3.3-4.8g/L of lithium oxide.
Preferably, the pressure of the positive pressure in the reaction tank in the step 2) is controlled to be 2 to 10kPa.
Preferably, the reaction kettle in the step 2) is heated by microwaves, and the temperature is kept between 80 and 105 ℃.
Preferably, the removal rate of the metal impurity ions in the impurity-removed filtrate obtained in the step 2) exceeds 96.0%.
Preferably, the post-treatment in step 3) comprises evaporation concentration, ion exchange resin, lithium precipitation, lithium washing, drying and crushing.
Preferably, the purity of the high-purity lithium carbonate obtained in the step 3) is not lower than 99.6%.
Compared with the prior art, the invention has the beneficial effects that:
according to the invention, a large amount of lithium precipitation mother liquor remained in a salt lake brine, spodumene or lepidolite lithium extraction process is fully utilized, sodium carbonate is replaced by the lithium precipitation mother liquor to serve as an impurity removing agent of a lepidolite lithium extraction leaching solution, and a large amount of metal impurity ions in the leaching solution are removed by matching with a heating effect of microwave treatment under high pressure; the process effectively utilizes the lithium precipitation mother liquor, has high metal impurity ion removal rate, greatly reduces the subsequent evaporation concentration amount, and achieves the purposes of optimizing the process and saving the cost.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the technical solutions of the present invention will be clearly and completely described below with reference to the embodiments. The examples, in which specific conditions are not specified, were carried out according to conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are conventional products which are not indicated by manufacturers and are commercially available.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.
Example 1
1. Mixing, roasting, grinding and leaching lepidolite concentrate, sodium sulfate and calcium oxide to obtain lithium sulfate leaching brine with lithium ion concentration of 12 g/L; and detecting metal impurity ions in the leached brine, wherein the concentration of iron ions is 46ppm, the concentration of zinc ions is 35ppm, the concentration of manganese ions is 562ppm, the concentration of calcium ions is 823ppm, and the concentration of magnesium ions is 59ppm.
2. Transferring the lithium sulfate leaching brine into a reaction kettle with a stirring device, adding sodium carbonate into salt lake brine in a lithium extraction process to precipitate lithium to obtain a lithium precipitation mother solution (the main components comprise 85g/L of sulfate ions, 14g/L of carbonate ions and 3.4g/L of lithium oxide), and controlling the flow of the lithium precipitation mother solution by a flow meter to be 4.5m 3 Precisely pumping the mixture into a reaction kettle (controlling the addition of carbonate ions to be 1.6 times of the molar sum of calcium and magnesium ions), pressurizing to 2.5kPa, simultaneously carrying out microwave heating, controlling the temperature to be 95 ℃, continuously stirring for 120min at 60rpm, keeping the temperature, standing for 15min, and filtering to obtain impurity-removed filtrate. And detecting metal impurity ions in the obtained impurity-removed filtrate, wherein the concentration of iron ions is 0.368ppm, the concentration of zinc ions is 0.291ppm, the concentration of manganese ions is 0.095ppm, the concentration of calcium ions is 32.818ppm and the concentration of magnesium ions is 2.330ppm.
3. And (3) carrying out evaporation concentration, ion exchange resin, lithium precipitation, lithium washing, drying and crushing on the impurity-removed filtrate, and packaging the finished product to obtain the battery-grade lithium carbonate. The purity of the cell grade lithium carbonate was measured to be 99.72%.
Example 2
1. Mixing, roasting, grinding and leaching lepidolite concentrate, sodium sulfate and calcium oxide to obtain lithium sulfate leaching brine with the lithium ion concentration of 7 g/L; and detecting metal impurity ions in the leached brine, wherein the concentration of iron ions is 33ppm, the concentration of zinc ions is 82ppm, the concentration of manganese ions is 990ppm, the concentration of calcium ions is 635ppm, and the concentration of magnesium ions is 44ppm.
2. Transferring the lithium sulfate leaching brine into a reaction kettle with a stirring device, taking another lithium precipitation mother liquor (the main components comprise 90g/L of sulfate ions, 17g/L of carbonate ions and 4.4g/L of lithium oxide) obtained by adding sodium carbonate to precipitate lithium in the process of extracting lithium from lepidolite, and controlling the flow of the lithium precipitation mother liquor by a flow meter to be 6.5m 3 Precisely pumping the mixture into a reaction kettle (controlling the addition of carbonate ions to be 1.8 times of the molar sum of the calcium and magnesium ions), pressurizing to 7.5kPa, simultaneously carrying out microwave heating, controlling the temperature to be 100 ℃, continuously stirring for 120min at 60rpm, keeping the temperature, standing for 15min, and filtering to obtain impurity-removed filtrate. And detecting metal impurity ions in the obtained impurity-removed filtrate, wherein the concentration of iron ions is 0.085ppm, the concentration of zinc ions is 0.122ppm, the concentration of manganese ions is 0.054ppm, the concentration of calcium ions is 24.429ppm and the concentration of magnesium ions is 1.488ppm.
3. And (3) evaporating and concentrating the obtained impurity-removed filtrate, performing ion exchange resin, precipitating lithium, washing the lithium, drying and crushing, and packaging finished products to obtain the battery-grade lithium carbonate in the same embodiment 1. The purity of the battery grade lithium carbonate was measured to be 99.81%.
Example 3
1. Mixing, roasting, grinding and leaching lepidolite concentrate, sodium sulfate and calcium oxide to obtain lithium sulfate leaching brine with the lithium ion concentration of 15 g/L; and detecting metal impurity ions in the leached brine, wherein the concentration of iron ions is 78ppm, the concentration of zinc ions is 19ppm, the concentration of manganese ions is 1123ppm, the concentration of calcium ions is 936ppm, and the concentration of magnesium ions is 26ppm.
2. Transferring the lithium sulfate leaching brine into a reaction kettle with a stirring device, adding sodium carbonate into spodumene lithium extraction process to precipitate lithium to obtain lithium precipitation mother liquor (main components including sulfate ions 108g/L, carbonate ions 12g/L and lithium oxide 3.6 g/L), and controlling the flow of the lithium precipitation mother liquor by a flow meter to be 3.5m 3 Precisely pumping the mixture into a reaction kettle (controlling the addition of carbonate ions to be 1.2 times of the molar sum of the calcium and magnesium ions), and pressurizingHeating to 5kPa while controlling the temperature of 95 ℃ by microwave heating, continuously stirring for 120min at 60rpm, keeping the temperature and standing for 15min, and filtering to obtain impurity-removed filtrate. And detecting metal impurity ions in the obtained impurity-removed filtrate, wherein the concentration of iron ions is 0.094ppm, the concentration of zinc ions is 0.175ppm, the concentration of manganese ions is 0.194ppm, the concentration of calcium ions is 32.446ppm, and the concentration of magnesium ions is 1.029ppm.
3. And (3) evaporating and concentrating the obtained impurity-removed filtrate, performing ion exchange resin, precipitating lithium, washing the lithium, drying and crushing, and packaging finished products to obtain the battery-grade lithium carbonate in the same example 1. The purity of the battery grade lithium carbonate was measured to be 99.67%.
Comparative example 1
1. Mixing, roasting, grinding and leaching lepidolite concentrate, sodium sulfate and calcium oxide to obtain lithium sulfate leaching brine with the lithium ion concentration of 12 g/L; and detecting metal impurity ions in the leached brine, wherein the concentration of iron ions is 47ppm, the concentration of zinc ions is 35ppm, the concentration of manganese ions is 566ppm, the concentration of calcium ions is 816ppm, and the concentration of magnesium ions is 60ppm.
2. Transferring the lithium sulfate leaching brine into a reaction kettle with a stirring device, taking sodium carbonate solution (carbonate ion 14 g/L), and controlling the flow rate of the sodium carbonate solution by a flow meter to be 4.5m 3 Precisely pumping the mixture into a reaction kettle (controlling the addition of carbonate ions to be 1.6 times of the molar sum of the calcium and magnesium ions), continuously stirring the mixture for 120min at 60rpm, standing the mixture for 15min, and filtering the mixture to obtain impurity-removed filtrate. And detecting metal impurity ions in the obtained impurity-removed filtrate, wherein the concentration of iron ions is 0.359ppm, the concentration of zinc ions is 0.278ppm, the concentration of manganese ions is 0.122ppm, the concentration of calcium ions is 33.026ppm, and the concentration of magnesium ions is 2.339ppm.
3. And (3) evaporating and concentrating the obtained impurity-removed filtrate, performing ion exchange resin, precipitating lithium, washing the lithium, drying and crushing, and packaging finished products to obtain the battery-grade lithium carbonate in the same example 1. The purity of the battery grade lithium carbonate was measured to be 99.73%.
Comparative example 2
1. Mixing, roasting, grinding and leaching lepidolite concentrate, sodium sulfate and calcium oxide to obtain lithium sulfate leaching brine with lithium ion concentration of 12 g/L; and detecting metal impurity ions in the leached brine, wherein the concentration of iron ions is 46ppm, the concentration of zinc ions is 34ppm, the concentration of manganese ions is 558ppm, the concentration of calcium ions is 824ppm, and the concentration of magnesium ions is 59ppm.
2. Transferring the lithium sulfate leaching brine into a reaction kettle with a stirring device, adding sodium carbonate into another salt lake brine in a lithium extraction process to precipitate lithium to obtain lithium precipitation mother liquor (main components of 85g/L sulfate ions, 14g/L carbonate ions and 3.4g/L lithium oxide), and controlling the flow of the lithium precipitation mother liquor by a flow meter to be 4.5m 3 Precisely pumping the mixture into a reaction kettle (controlling the addition of carbonate ions to be 1.6 times of the molar sum of calcium and magnesium ions), keeping the pressure at normal pressure, simultaneously carrying out microwave heating, controlling the temperature to be 95 ℃, continuously stirring the mixture for 120min at 60rpm, keeping the temperature, standing the mixture for 15min, and filtering the mixture to obtain impurity-removed filtrate. And detecting metal impurity ions in the obtained impurity-removed filtrate, wherein the concentration of iron ions is 0.477ppm, the concentration of zinc ions is 0.364ppm, the concentration of manganese ions is 1.758ppm, the concentration of calcium ions is 37.404ppm, and the concentration of magnesium ions is 2.761ppm.
3. And (3) evaporating and concentrating the obtained impurity-removed filtrate, performing ion exchange resin, precipitating lithium, washing the lithium, drying and crushing, and packaging finished products to obtain the battery-grade lithium carbonate in the same example 1. The purity of the battery grade lithium carbonate was measured to be 98.42%.
Comparative example 3
1. Mixing, roasting, grinding and leaching lepidolite concentrate, sodium sulfate and calcium oxide to obtain lithium sulfate leaching brine with lithium ion concentration of 12 g/L; and detecting metal impurity ions in the leached brine, wherein the concentration of iron ions is 44ppm, the concentration of zinc ions is 34ppm, the concentration of manganese ions is 565ppm, the concentration of calcium ions is 830ppm, and the concentration of magnesium ions is 61ppm.
2. Transferring the lithium sulfate leaching brine into a reaction kettle with a stirring device, adding sodium carbonate into salt lake brine in a lithium extraction process to precipitate lithium to obtain a lithium precipitation mother solution (the main components comprise 85g/L of sulfate ions, 14g/L of carbonate ions and 3.4g/L of lithium oxide), and controlling the flow of the lithium precipitation mother solution by a flow meter to be 4.5m 3 Precisely pumping the mixture into a reaction kettle (controlling the addition of carbonate ions to be 1.6 times of the molar sum of calcium and magnesium ions), pressurizing to 2.5bar, simultaneously carrying out conventional heat conduction heating, controlling the temperature to be 95 ℃, continuously stirring at 60rpm for 120min, keeping the temperature, standing for 15min, and filtering to obtain the calcium magnesium carbonateTo remove impurity and filtrate. And detecting metal impurity ions in the obtained impurity-removed filtrate, wherein the concentration of iron ions is 0.417ppm, the concentration of zinc ions is 0.352ppm, the concentration of manganese ions is 2.702ppm, the concentration of calcium ions is 44.670ppm, and the concentration of magnesium ions is 3.835ppm.
3. And (3) evaporating and concentrating the obtained impurity-removed filtrate, performing ion exchange resin, precipitating lithium, washing the lithium, drying and crushing, and packaging finished products to obtain the battery-grade lithium carbonate in the same embodiment 1. The purity of the battery grade lithium carbonate was measured to be 97.63%.
The embodiments described above merely represent some preferred embodiments of the present invention, which are described in more detail and detail, but are not intended to limit the present invention. It should be understood that various changes and modifications can be made by those skilled in the art, and any modifications, equivalents, improvements, etc. made within the spirit and principle of the invention should be included in the scope of the invention.
Claims (10)
1. A method for removing lepidolite leaching brine impurities by using a lithium precipitation mother liquor is characterized by comprising the following steps:
step 1): mixing lepidolite ore and sulfate, roasting, grinding and leaching to obtain leached brine;
step 2): transferring the leached brine obtained in the step 1) into a reaction kettle, gradually pumping lithium precipitation mother liquor into the reaction kettle, continuously stirring under positive pressure and controlled temperature, keeping the temperature, standing, and filtering to obtain impurity-removed filtrate;
step 3): and (3) carrying out post-treatment on the impurity-removed filtrate obtained in the step 2) to obtain battery-grade lithium carbonate.
2. The method for removing lepidolite leach brine impurities from lithium precipitation mother liquor of claim 1, wherein the leach brine of step 1) contains iron, zinc, manganese, calcium and magnesium metal impurity ions.
3. The method for removing lepidolite leach brine impurities from lithium precipitation mother liquor of claim 1, wherein step 2) is a step-wise pumping of lithium precipitation mother liquorThe flow rate is controlled to be 3-7m 3 /h。
4. The method for removing lepidolite leaching brine impurities by using the lithium precipitation mother liquor according to claim 3, wherein the lithium precipitation mother liquor is obtained by precipitating lithium in salt lake brine, spodumene or a lepidolite lithium extraction process, namely adding sodium carbonate for reaction.
5. The method of claim 4, wherein the lithium precipitation mother liquor is selected from the group consisting of: 78-110g/L of sulfate ions, 11-18g/L of carbonate ions and 3.3-4.8g/L of lithium oxide.
6. The method for removing lepidolite leach brine impurities from lithium precipitation mother liquor of claim 1 wherein the positive pressure in the reaction tank of step 2) is controlled to be 2 to 10kPa.
7. The method for removing lepidolite leaching brine impurities by using lithium precipitation mother liquor as claimed in claim 1, wherein the reaction kettle in step 2) is heated by microwave and the temperature is kept at 80-105 ℃.
8. The method for removing lepidolite leaching brine impurities using lithium precipitation mother liquor according to claim 1, wherein the removal rate of metal impurity ions in the impurity removed filtrate obtained in step 2) is more than 96.0%.
9. The method for removing lepidolite leaching brine impurities by using lithium precipitation mother liquor as claimed in claim 1, wherein the post-treatment of step 3) comprises evaporation concentration, ion exchange resin, lithium precipitation, lithium washing, drying and crushing.
10. The method for removing lepidolite leaching brine impurities from lithium precipitation mother liquor according to claim 1, wherein the purity of the battery grade lithium carbonate obtained in step 3) is not less than 99.6%.
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