CN111807389A - Method for preparing lithium carbonate by using acid-resistant film - Google Patents
Method for preparing lithium carbonate by using acid-resistant film Download PDFInfo
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- CN111807389A CN111807389A CN202010670189.0A CN202010670189A CN111807389A CN 111807389 A CN111807389 A CN 111807389A CN 202010670189 A CN202010670189 A CN 202010670189A CN 111807389 A CN111807389 A CN 111807389A
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- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D15/00—Lithium compounds
- C01D15/08—Carbonates; Bicarbonates
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Abstract
The invention discloses a method for preparing lithium carbonate by utilizing an acid-resistant film, which comprises the following steps: s01: concentrating the lithium-rich solution I through a reverse osmosis membrane to obtain a lithium-rich solution II; s02: filtering the lithium-rich solution II through a nanofiltration membrane to obtain a lithium-rich solution III; s03: adding a pH regulator into the lithium-rich solution III, and regulating the pH to 5-9 to obtain a lithium-rich solution IV; s04: filtering the lithium-rich solution IV through ion exchange resin to obtain a lithium-rich solution V; s05: concentrating the lithium-rich solution V through a high-pressure reverse osmosis membrane to obtain a lithium-rich solution VI; s06: and adding sodium carbonate into the lithium-rich solution VI to separate out lithium carbonate crystals. According to the method for preparing the lithium carbonate by using the acid-resistant film, the problems of concentration and impurity removal of the lithium-rich solution are solved through the acid-resistant film, the addition amount of a medicament can be greatly reduced, and the introduction of impurities is reduced.
Description
Technical Field
The invention relates to the field of lithium ion purification, in particular to a method for preparing lithium carbonate by utilizing an acid-resistant film.
Background
Lithium is the lightest metal element in nature, and is the lightest and most active alkali metal in the group IA alkali metal head position in the periodic table. Because of its wide application field, it is praised as "industrial monosodium glutamate"; lithium is also known as an "energy metal" because it has the highest standard oxidation potential of various elements and is therefore the most undeniable element in the battery and power field.
According to different raw materials, the lithium extraction process can be divided into two process routes of ore lithium extraction and brine lithium extraction. The process route adopted for extracting lithium from ores is the earliest, the total lithium reserve in the ores is small, the energy consumption is large, and high-quality resources are nearly exhausted after being mined for hundreds of years, so that the production cost is high, the lithium resources of salt lake brine account for 71 percent of the lithium resource reserve in China, and the process for extracting lithium from brine is relatively simple and relatively low in cost, so that the process for extracting lithium from brine becomes a mainstream research process.
The lithium content in salt lakes of Qinghai Tibet and other places is high, in the current lithium extraction method, the salt lake of Tibet mainly uses a solar pond method to extract lithium industrially, the production period from salt lake brine to lithium resource products is long, statistics is generally carried out by taking years as units, the consumed time is long, and the lithium extraction efficiency is seriously influenced. The Qinghai salt lake is mainly used for industrially extracting lithium by using an aluminum adsorption method, the method needs to carry out pretreatment such as temperature rise on salt lake brine, more power consumption is inevitably increased by the pretreatment such as temperature rise in a high-altitude low-temperature environment, the concentration of a lithium-containing solution extracted by the method is low, and a multi-step purification process is needed subsequently, so that the whole extraction process is time-consuming and labor-consuming.
Meanwhile, the lithium-rich solution extracted from the salt lake brine contains more metal impurity ions, and in order to change the lithium-rich solution into lithium carbonate, a plurality of precipitants or impurity extracting agents are required to be added to remove the impurity ions, so that the process is complicated, the consumed time is long, and the final yield of the lithium carbonate cannot be ensured. In order to simplify the lithium extraction process of salt lake brine, a method for preparing lithium carbonate suitable for high altitude areas such as Qinghai Tibet and areas with relatively poor industrial foundation needs to be found.
Disclosure of Invention
The invention aims to provide a method for preparing lithium carbonate by using an acid-resistant film, which solves the problems of concentration and impurity removal of a lithium-rich solution through the acid-resistant film, and can greatly reduce the addition amount of a medicament and reduce the introduction of impurities.
In order to achieve the purpose, the invention adopts the following technical scheme: a method for preparing lithium carbonate by utilizing an acid-resistant film comprises the following steps:
s01: concentrating the lithium-rich solution I through a reverse osmosis membrane to obtain a lithium-rich solution II;
s02: filtering the lithium-rich solution II through a nanofiltration membrane to obtain a lithium-rich solution III;
s03: adding a pH regulator into the lithium-rich solution III, and regulating the pH to 5-9 to obtain a lithium-rich solution IV;
s04: filtering the lithium-rich solution IV through ion exchange resin to obtain a lithium-rich solution V;
s05: concentrating the lithium-rich solution V through a high-pressure reverse osmosis membrane to obtain a lithium-rich solution VI;
s06: and adding sodium carbonate into the lithium-rich solution VI to separate out lithium carbonate crystals.
Further, in the step S01, the lithium concentration in the lithium-rich solution i is 1-5g/L, the lithium concentration in the lithium-rich solution ii is 2-10g/L, and the reverse osmosis membrane is an acid-resistant reverse osmosis membrane.
Further, the nanofiltration membrane is an acid-resistant nanofiltration membrane.
Further, in step S03, the pH adjusting agent is sodium hydroxide.
Further, the lithium concentration of the lithium-rich solution VI in the step S06 is 15-25 g/L.
Further, the step S06 specifically includes:
s061: adding sodium carbonate with the molar ratio of Na/Li being 1-1.5 into the lithium-rich solution VI to separate out lithium carbonate crystals;
s062: and (3) filtering the lithium-rich solution VI with the lithium carbonate crystals separated out, and washing the filter residue after filtering with deionized water to obtain the lithium carbonate.
Further, in the step S062, deionized water at the temperature of 60-90 ℃ is adopted to wash the filter residue.
Further, the lithium-rich solution I is obtained by extracting from salt lake brine through an adsorbent, and the specific extraction method comprises the following steps:
t01: allowing the filtered salt lake brine to pass through a manganese-based lithium ion sieve adsorbent so that lithium ions in the salt lake brine are adsorbed on the manganese-based lithium ion sieve adsorbent;
t02: cleaning impurity ions in the manganese-based lithium ion sieve adsorbent by using a cleaning solution;
t03: and washing the manganese-based lithium ion sieve adsorbent by using an eluent to enable lithium ions adsorbed in the manganese-based lithium ion sieve adsorbent to be separated into the eluent, so as to obtain a lithium-rich solution I.
Further, the pH value of the salt lake brine is 5-12, and the lithium ion concentration is more than or equal to 1 ppm.
Further, the temperature range of extracting the lithium-containing solution in the step T01-step T03 is between-20 ℃ below zero and-80 ℃.
The invention has the following beneficial effects: compared with a solar pond method, the method can shorten the production period of extracting lithium from salt lake brine from year to hour, and greatly improves the production efficiency; the invention solves the problems of concentration and impurity removal of the lithium-rich solution through the acid-resistant film, can greatly reduce the addition of the medicament and reduce the introduction of impurities.
Drawings
Fig. 1 is a flow chart of a method for preparing lithium carbonate by using an acid-resistant film according to the invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, embodiments of the present invention are described in detail below with reference to the accompanying drawings.
As shown in fig. 1, the method for preparing lithium carbonate by using an acid-resistant film provided by the invention comprises the following steps:
s01: concentrating the lithium-rich solution I through a reverse osmosis membrane to obtain a lithium-rich solution II; wherein the lithium concentration in the lithium-rich solution I is 1-5g/L, and the lithium concentration in the lithium-rich solution II is 2-10 g/L. The reverse osmosis membrane is an acid-resistant reverse osmosis membrane and can be suitable for an environment with the pH value of 0.5-8. Specific reverse osmosis membrane suppliers include, but are not limited to, DuPont (DuPont), Suez (SUEZ), Koch (Koch), and the like.
S02: filtering the lithium-rich solution II through a nanofiltration membrane to obtain a lithium-rich solution III; the nanofiltration membrane can remove high-valence ions (non-monovalent ions); the nanofiltration membrane in the step is mainly used for removing 80-99.9% of calcium, magnesium, manganese, iron and other impurity ions in the lithium-rich solution II. The nanofiltration membrane is acid-resistant and can be applied in an environment with a pH of 0.5-8, and specific reverse osmosis membrane suppliers include, but are not limited to, DuPont (DuPont), Suez (SUEZ), Koch (Koch), etc.
S03: adding a pH regulator into the lithium-rich solution III, and regulating the pH to 5-9 to obtain a lithium-rich solution IV; the specific pH adjusting agent may be solid sodium hydroxide or a high-concentration sodium hydroxide solution.
S04: filtering the lithium-rich solution IV through ion exchange resin to obtain a lithium-rich solution V; among them, the ion exchange resin is mainly used to remove high-valence impurity ions (non-monovalent ions) such as calcium, magnesium, manganese, iron, etc., and suppliers include, but are not limited to, DuPont (DuPont), Lanxess (Lanxess), and Bronsted (Purolite). In the step, 50-99.9% of impurity ions such as calcium, magnesium, manganese, iron and the like in the lithium-rich solution IV are further removed by ion exchange resin.
S05: concentrating the lithium-rich solution V through a high-pressure reverse osmosis membrane to obtain a lithium-rich solution VI; the high-pressure reverse osmosis membrane has the function of concentrating the lithium-rich solution V, and the lithium concentration in the lithium-rich solution VI obtained after concentration is 15-25 g/L.
S06: adding sodium carbonate into the lithium-rich solution VI to separate out lithium carbonate crystals; the method specifically comprises the following steps:
s061: adding sodium carbonate with the molar ratio of Na/Li being 1-1.5 into the lithium-rich solution VI to separate out lithium carbonate crystals; specifically, after the sodium carbonate is added, the lithium carbonate can be concentrated by adopting methods such as reverse osmosis, nanofiltration, multiple-effect evaporation, MVR (Mechanical vapor recompression), solar heat collection, a solar pond and the like until lithium carbonate crystals are separated out.
S062: filtering the lithium-rich solution VI with the lithium carbonate crystals separated out, and washing filter residues after filtering by deionized water to obtain lithium carbonate; wherein, the filtration can be realized by suction filtration, centrifugation, plate-and-frame filter pressing and the like, and the washing can adopt deionized water with the temperature of 60-90 ℃ to drip wash the filter residue for 1-5 times, thus obtaining the industrial grade lithium carbonate.
It is worth to say that the lithium-rich solution I is obtained by extracting from salt lake brine through an adsorbent, and the extraction method can be applied to the temperature ranging from minus 20 ℃ to minus 80 ℃, and can be directly applied to high-altitude areas such as Qinghai Tibet and the like. The preparation method specifically comprises the following steps:
t01: and (3) passing the filtered salt lake brine through a manganese-based lithium ion sieve adsorbent, so that lithium ions in the salt lake brine are adsorbed on the manganese-based lithium ion sieve adsorbent.
The invention is suitable for any lithium-containing salt lake with the pH value of the salt lake brine in the range of 5-12, and the concentration of lithium ions in the salt lake brine is more than or equal to 1 ppm. Preferably, the salt lake brine is derived from salt lakes in Tibet or Qinghai regions. The manganese-based lithium ion sieve adsorbent can adopt any manganese-based lithium ion sieve adsorbent in the prior art, and specifically can be but not limited to one or more of a porous manganese-based lithium ion sieve adsorbent, a hexagonal flaky manganese-based lithium ion sieve adsorbent and a hexagonal dendritic manganese-based lithium ion sieve adsorbent.
T02: and cleaning the impurity ions in the manganese-based lithium ion sieve adsorbent by using a cleaning solution.
The cleaning solution in this step is deionized water or distilled water or filtered river water, and the purpose of cleaning is to remove impurity ions, such as iron ions, sodium ions, and the like, in the manganese-based lithium ion sieve adsorbent. In the manganese-based lithium ion sieve adsorbent, about 99% of hydrogen ions in the manganese-based lithium ion sieve adsorbent are subjected to ion exchange with lithium ions in salt lake brine, and the rest about 1% of hydrogen ions are subjected to ion exchange with impurity ions in the salt lake brine, wherein the impurity ions have the radius or charge distribution close to that of the lithium ions. Through the reasonable volume of setting up manganese lithium ion sieve adsorbent, can ensure that the lithium ion in salt lake brine is basically all adsorbed in manganese lithium ion sieve adsorbent, at this moment, adopt the washing liquid to wash, can get rid of most other impurity ions except lithium ion.
T03: and (3) cleaning the manganese-based lithium ion sieve adsorbent by using an eluent to enable lithium ions adsorbed in the manganese-based lithium ion sieve adsorbent to be separated into the eluent, so as to obtain a lithium-rich solution I.
The eluent in the invention can be but is not limited to 0.1-2mol/L hydrochloric acid solution or 0.1-2mol/L nitric acid solution or 0.1-2mol/L oxalic acid solution or 0.05-1mol/L phosphoric acid solution or 0.05-1mol/L sulfuric acid solution. In the process of cleaning the manganese-based lithium ion sieve adsorbent by the eluent, the lithium ions adsorbed in the manganese-based lithium ion sieve adsorbent are replaced, and the lithium ions are discharged along with the eluent, wherein the eluent containing the lithium ions is the lithium-enriched solution I.
T04: and cleaning the manganese-based lithium ion sieve adsorbent by using a cleaning solution, and cleaning the eluent in the manganese-based lithium ion sieve adsorbent.
The cleaning solution in this step may be, but is not limited to, deionized water, distilled water, or filtered river water, and the purpose of cleaning is to remove the eluent in the manganese-based lithium ion sieve adsorbent, so as to facilitate the next use.
Compared with a solar pond method, the method can shorten the production period of extracting lithium from salt lake brine from year to hour, and greatly improves the production efficiency; the invention solves the problems of concentration and impurity removal of the lithium-rich solution through the acid-resistant film, can greatly reduce the addition of the medicament and reduce the introduction of impurities.
The above description is only a preferred embodiment of the present invention, and the embodiment is not intended to limit the scope of the present invention, so that all equivalent structural changes made by using the contents of the specification and the drawings of the present invention should be included in the scope of the appended claims.
Claims (10)
1. A method for preparing lithium carbonate by utilizing an acid-resistant film is characterized by comprising the following steps:
s01: concentrating the lithium-rich solution I through a reverse osmosis membrane to obtain a lithium-rich solution II;
s02: filtering the lithium-rich solution II through a nanofiltration membrane to obtain a lithium-rich solution III;
s03: adding a pH regulator into the lithium-rich solution III, and regulating the pH to 5-9 to obtain a lithium-rich solution IV;
s04: filtering the lithium-rich solution IV through ion exchange resin to obtain a lithium-rich solution V;
s05: concentrating the lithium-rich solution V through a high-pressure reverse osmosis membrane to obtain a lithium-rich solution VI;
s06: and adding sodium carbonate into the lithium-rich solution VI to separate out lithium carbonate crystals.
2. The method for preparing lithium carbonate by using the acid-resistant film as claimed in claim 1, wherein the lithium concentration in the lithium-rich solution i in the step S01 is 1-5g/L, the lithium concentration in the lithium-rich solution ii is 2-10g/L, and the reverse osmosis membrane is an acid-resistant reverse osmosis membrane.
3. The method for preparing lithium carbonate by using the acid-resistant film as claimed in claim 1, wherein the nanofiltration membrane is an acid-resistant nanofiltration membrane.
4. The method for preparing lithium carbonate using the acid-resistant film as claimed in claim 1, wherein the pH adjusting agent in step S03 is sodium hydroxide.
5. The method for preparing lithium carbonate by using the acid-resistant film as claimed in claim 1, wherein the lithium concentration in the lithium-rich solution VI in the step S06 is 15-25 g/L.
6. The method for preparing lithium carbonate by using the acid-resistant film as claimed in claim 1, wherein the step S06 specifically comprises:
s061: adding sodium carbonate with the molar ratio of Na/Li being 1-1.5 into the lithium-rich solution VI to separate out lithium carbonate crystals;
s062: and (3) filtering the lithium-rich solution VI with the lithium carbonate crystals separated out, and washing the filter residue after filtering with deionized water to obtain the lithium carbonate.
7. The method for preparing lithium carbonate using the acid-resistant film as claimed in claim 6, wherein the filter residue is washed with deionized water at 60-90 ℃ in the step S062.
8. The method for preparing lithium carbonate by using the acid-resistant film as claimed in claim 1, wherein the lithium-rich solution I is obtained by extracting from salt lake brine by using an adsorbent, and the specific extraction method comprises the following steps:
t01: allowing the filtered salt lake brine to pass through a manganese-based lithium ion sieve adsorbent so that lithium ions in the salt lake brine are adsorbed on the manganese-based lithium ion sieve adsorbent;
t02: cleaning impurity ions in the manganese-based lithium ion sieve adsorbent by using a cleaning solution;
t03: and washing the manganese-based lithium ion sieve adsorbent by using an eluent to enable lithium ions adsorbed in the manganese-based lithium ion sieve adsorbent to be separated into the eluent, so as to obtain a lithium-rich solution I.
9. The method for preparing lithium carbonate by using the acid-resistant film according to claim 8, wherein the salt lake brine has a pH value of 5-12 and a lithium ion concentration of 1ppm or more.
10. The method for preparing lithium carbonate by using the acid-resistant film as claimed in claim 8, wherein the temperature range of the lithium-containing solution extracted in the steps T01-T03 is from-20 ℃ below zero to-80 ℃.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114655970A (en) * | 2022-03-31 | 2022-06-24 | 神华准能资源综合开发有限公司 | Method for preparing lithium carbonate from scale evaporation mother liquor |
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