CN114272961A - Ion exchange resin regeneration method for removing impurities from lithium sulfate solution - Google Patents
Ion exchange resin regeneration method for removing impurities from lithium sulfate solution Download PDFInfo
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Abstract
The invention belongs to the field of lithium carbonate production technology, and particularly relates to a method for regenerating ion exchange resin for removing impurities from a lithium sulfate solution, which comprises the following steps: backwashing the ion exchange resin after adsorption saturation by pure water; resolving the ion exchange resin with dilute sulfuric acid solution; washing the resolved ion exchange resin with pure water; regenerating the washed ion exchange resin by lithium carbonate lithium precipitation mother liquor; and washing the regenerated ion exchange resin with pure water to obtain the regenerated ion exchange resin. The regeneration method of the invention uses dilute sulfuric acid solution for resolution, no chloride ion is introduced, and the lithium precipitation mother solution is used for regeneration, thus saving the use of sodium hydroxide.
Description
Technical Field
The invention belongs to the field of lithium carbonate production technology, and particularly relates to a method for regenerating ion exchange resin for removing impurities from a lithium sulfate solution.
Background
The ion exchange resin is a high molecular compound with a network structure of functional groups. In the preparation process of lithium carbonate, the ion exchange resin is mainly used for removing Ca2+、Mg2+、Al3+、Zn2+Plasma of impurity ions, and the ion exchange resin is easy to useAfter impurity ions are adsorbed, the ion exchange resin is saturated, and in order to save cost, the ion exchange resin needs to be regenerated, and the ions and other impurities adsorbed by the resin are eluted and removed by using a chemical reagent.
The regeneration method of the ion exchange resin commonly used at present uses dilute hydrochloric acid, and the reaction principle is as follows:
adsorption: RCH2NHCH2PO3Na+Ca2+——RCH2NHCH2PO3Ca+Na+
Desorbing: RCH2NHCH2PO3Ca+H+——RCH2NHCH2PO3H+Ca2+
Regeneration: RCH2NHCH2PO3H2+Na++OH-——RCH2NHCH2PO3Na+H2O
Sulfate is generally used in the preparation process of lithium carbonate, and chloride ions are easily introduced into a sulfuric acid system by using hydrochloric acid, so that the pollution of the chloride ions is caused, and the preparation method is not environment-friendly. In addition, in a sulfate system, because calcium sulfate is slightly soluble and is regenerated by sulfuric acid, calcium sulfate particles are deposited inside the resin due to poor control, the internal structure of the porous resin is easily blocked, and the adsorption effect is affected.
Disclosure of Invention
The invention aims to provide a regeneration method of ion exchange resin for removing impurities from a lithium sulfate solution, the regeneration method uses a dilute sulfuric acid solution for analysis, no chloride ion is introduced, lithium precipitation mother liquor is used for regeneration, the use of sodium hydroxide can be saved, the method is green and environment-friendly, the cost is low, and the obtained regenerated ion exchange resin has a good adsorption effect.
The invention provides an ion exchange resin regeneration method for removing impurities from a lithium sulfate solution, which comprises the following specific steps:
s1, backwashing the ion exchange resin after adsorption saturation from bottom to top by using pure water with the volume of 1-5 times of the resin, and performing replacement treatment on substances in the system;
s2, analyzing the ion exchange resin cleaned in the S1 by using a dilute sulfuric acid solution, wherein during analysis, the dilute sulfuric acid solution with the volume 1-5 times of that of the resin is used to ensure that impurity ions are sufficiently analyzed;
s3, washing the ion exchange resin analyzed by the S2 by using pure water with the volume 1-3 times of that of the resin, and replacing a dilute sulfuric acid solution in the system;
s4, regenerating the ion exchange resin washed by the S3 by using lithium carbonate lithium precipitation mother liquor, wherein during regeneration, the lithium precipitation mother liquor with 2-6 times of the volume of the resin is used to ensure that sodium ions are fully regenerated;
and S5, washing the regenerated ion exchange resin of S4 by using pure water with the volume 1-3 times of the resin, and replacing lithium precipitation mother liquor in the system to obtain the regenerated ion exchange resin.
In the technical scheme, pure water is used for backwashing the ion exchange numerical value from bottom to top, so that impurities attached to the surface of the resin can be effectively removed; the low-concentration dilute sulfuric acid solution is used as an analytic solution, and the impurity ions adsorbed on the resin can be effectively removed by controlling the dosage and flow rate of the solution; the lithium precipitation mother liquor after the lithium carbonate is produced is used as the regeneration liquor, the analytic liquor such as sodium hydroxide and the like is not additionally used, the cost can be saved, the sufficient regeneration of sodium type ions can be ensured by controlling the flow rate of the used amount, the regeneration effect is good, meanwhile, the step of decarbonizing the lithium precipitation mother liquor by using sulfuric acid during the production of the lithium carbonate can be saved by using the lithium precipitation mother liquor as the analytic liquor, and the comprehensive cost is saved.
Preferably, in the above technical solution, the ion exchange resin is a macroporous chelating resin. The macroporous chelating resin is a cross-linked functional polymer material capable of forming a multi-coordination complex with metal ions, has the action mechanism that functional atoms on the resin and the metal ions perform a coordination reaction to form a stable structure similar to a micromolecular chelate, has the characteristics of strong bonding force with the metal ions and high selectivity, has a firm structure, good chemical stability, high mesh degree and large chelating capacity, and is mainly used for removing ionic impurities such as calcium, magnesium and the like.
Preferably, in the above technical solution S2, the concentration of the dilute sulfuric acid solution is less than or equal to 7%, and the pH is ensured to be less than or equal to 4 during the circulation process. In the technical scheme, dilute sulfuric acid is selected for resolution, hydrochloric acid is not used, chloride ion impurities can be prevented from being introduced, and the method is more environment-friendly; when preparing the dilute sulfuric acid solution, an acid mixer with an electromagnetic flow meter can be used, and the dilute sulfuric acid solution can also be prepared in a storage tank, but the dilute sulfuric acid solution needs to be accurately measured to ensure the analysis effect.
Preferably, in the technical scheme S2, the flow rate of the dilute sulfuric acid solution passing through the ion exchange resin is 2-6 BV/h. In this technical scheme, select for use low concentration sulphuric acid, control higher flow speed simultaneously, can effectively avoid calcium sulfate deposit in the resin, can not block up poroid resin inner structure, regeneration effect is good.
Preferably, in the technical scheme S4, the lithium precipitation mother liquor is a 1.5-4.5% sodium carbonate solution.
Preferably, in the technical scheme S4, the flow rate of the lithium precipitation mother liquor passing through the resin is 1-5 BV/h. The regeneration liquid with lower flow rate and speed is controlled in the technical scheme, so that the full regeneration of sodium ions is facilitated.
Preferably, in the above technical solution S2, the dilute sulfuric acid solution may be recycled or not, and when the dilute sulfuric acid solution is recycled, a filtering device is required before the recycled dilute sulfuric acid solution enters the resin tank, so as to prevent calcium sulfate particulate matter from entering the resin system. According to the technical scheme, the use amount of the analysis can be saved by recycling the diluted sulfuric acid after the analysis, and the regeneration cost is saved.
Preferably, in the above technical scheme, when the regenerated ion exchange resin is used for removing impurities from a lithium sulfate solution, a single column is used or multiple columns are used in series. According to the technical scheme, the method can select a series connection mode of using a single column, a double column or a three column and the like according to the amount or concentration of impurities in the lithium sulfate solution, so that the impurity removal effect is improved.
Compared with the prior art, the method has the beneficial effects that:
1. according to the method for regenerating the ion exchange resin for removing impurities from the lithium sulfate solution, the dilute sulfuric acid solution is used as the analytic solution, hydrochloric acid is not used, introduction of chloride ions can be avoided, and the method is more green and environment-friendly;
2. according to the invention, the lithium precipitation mother liquor for producing lithium carbonate is used as the regeneration liquor, so that the use of sodium hydroxide can be saved, the use of sulfuric acid in the subsequent decarburization process of the lithium precipitation mother liquor can be saved, and the cost is saved;
3. the invention can effectively avoid the deposition of calcium sulfate in the macroporous resin by optimizing the concentration, flow rate and regeneration flow of the dilute sulfuric acid solution and the lithium precipitation mother solution and strictly controlling the regeneration parameters, and has good regeneration effect.
4. The regeneration method is more environment-friendly and low in cost, and the obtained regenerated ion exchange resin is used for removing impurities from the lithium sulfate solution, the concentration of calcium ions is as low as 1.8ppm, and the adsorption effect is good.
Detailed Description
The technical features of the present invention described above and those described in detail below (as an embodiment) can be combined with each other to form a new or preferred technical solution, but the present invention is not limited to these embodiments, and the embodiments also do not limit the present invention in any way.
The experimental procedures in the following examples are conventional unless otherwise specified. The formulations according to the following examples are all commercially available products and are commercially available, unless otherwise specified.
The present invention is described in further detail below with reference to examples:
example 1
A regeneration method of ion exchange resin for removing impurities from a lithium sulfate solution comprises the following specific steps:
s1, backwashing the ion exchange resin after adsorption saturation by pure water with 5 times of the volume of the resin from bottom to top, and performing replacement treatment on substances in a system;
s2, using a dilute sulfuric acid solution with the concentration of 3% to analyze the ion exchange resin cleaned in the S1, wherein the pH value is ensured to be less than or equal to 4 during analysis, using the dilute sulfuric acid solution with the volume of 5 times of the resin, and ensuring that impurity ions are fully analyzed through the flow rate of the ion exchange resin being 2-6 BV/h;
s3, washing the ion exchange resin analyzed in the S2 by using pure water with the volume of 1 time of the resin, and replacing a dilute sulfuric acid solution in the system;
s4, regenerating the ion exchange resin washed by the S3 by using lithium carbonate lithium precipitation mother liquor, wherein during regeneration, the lithium precipitation mother liquor with 6 times of resin volume is used, and the flow speed of the resin is 1-5BV/h, so that sodium ions are ensured to be fully regenerated; wherein, the lithium precipitation mother liquor is 1.5 percent of sodium carbonate solution;
and S5, washing the regenerated ion exchange resin obtained in the step S4 by using pure water with 2 times of resin volume, and replacing the lithium precipitation mother liquor in the system by using the pure water to obtain the regenerated ion exchange resin.
Example 2
A regeneration method of ion exchange resin for removing impurities from a lithium sulfate solution comprises the following specific steps:
s1, backwashing the ion exchange resin which is adsorbed and saturated from bottom to top by using pure water with the volume of 3 times of the resin, and performing replacement treatment on substances in a system;
s2, using a dilute sulfuric acid solution with the concentration of 5% to analyze the ion exchange resin cleaned in the S1, wherein the pH value is ensured to be less than or equal to 4 during analysis, using the dilute sulfuric acid solution with the volume of 3 times of the resin, and ensuring that impurity ions are fully analyzed through the flow rate of the ion exchange resin being 2-6 BV/h;
s3, washing the ion exchange resin analyzed in the S2 by using pure water with 2 times of the volume of the resin, and replacing a dilute sulfuric acid solution in the system;
s4, regenerating the ion exchange resin washed by the S3 by using lithium carbonate lithium precipitation mother liquor, wherein during regeneration, the lithium precipitation mother liquor with 4 times of resin volume is used, and the flow speed of the resin is 1-5BV/h, so that sodium ions are ensured to be fully regenerated; wherein, the lithium precipitation mother liquor is 3 percent of sodium carbonate solution;
and S5, washing the regenerated ion exchange resin obtained in the step S4 by using pure water with the volume of 1 time of the resin, and replacing the lithium precipitation mother liquor in the system by using the pure water to obtain the regenerated ion exchange resin.
Example 3
A regeneration method of ion exchange resin for removing impurities from a lithium sulfate solution comprises the following specific steps:
s1, backwashing the ion exchange resin after adsorption saturation by using pure water with the volume of 1 time of the resin from bottom to top, and performing replacement treatment on substances in a system;
s2, using a dilute sulfuric acid solution with the concentration of 7% to analyze the ion exchange resin cleaned in the S1, wherein the pH value is ensured to be less than or equal to 4 during analysis, using the dilute sulfuric acid solution with the volume of 2 times of the resin, and ensuring that impurity ions are fully analyzed through the flow rate of the ion exchange resin being 2-6 BV/h;
s3, washing the ion exchange resin analyzed in the S2 by using pure water with 3 times of the volume of the resin, and replacing a dilute sulfuric acid solution in the system;
s4, regenerating the ion exchange resin washed by the S3 by using lithium carbonate lithium precipitation mother liquor, wherein during regeneration, the lithium precipitation mother liquor with 2 times of resin volume is used, and the flow speed of the resin is 1-5BV/h, so that sodium ions are ensured to be fully regenerated; wherein, the lithium precipitation mother liquor is 4.5 percent of sodium carbonate solution;
and S5, washing the regenerated ion exchange resin obtained in the step S4 by using pure water with the volume of 3 times of the resin, and replacing the lithium precipitation mother liquor in the system by using the pure water to obtain the regenerated ion exchange resin.
Test examples
The regenerated ion exchange resin obtained by the method of example 1 and the saturated ion exchange resin before regeneration of example 1 were used to treat lithium sulfate stock solutions containing different calcium ion impurities, respectively, and the results are shown in table 1.
TABLE 1
As can be seen from the results in Table 1, the regenerated ion exchange resin obtained by the regeneration method of the ion exchange resin is used for removing impurities from lithium sulfate stock solution with lower or higher calcium ion concentration, the calcium ion concentration of the regenerated ion exchange resin can be lower than 3.1ppm, and the regenerated ion exchange resin meets the requirement that the calcium ion concentration in the working procedure standard is less than or equal to 8; and the calcium ion concentration of the same lithium sulfate stock solution treated by using the saturated (non-regenerated) ion exchange resin is still 19.4-23.6ppm, which is obviously higher than the process standard and can not meet the requirement. The regenerated ion exchange resin obtained by the regeneration method can well remove calcium ions in the lithium sulfate stock solution, and has good adsorption effect.
Finally, it should be emphasized that the above-described preferred embodiments of the present invention are merely examples of implementations, rather than limitations, and that many variations and modifications of the invention are possible to those skilled in the art, without departing from the spirit and scope of the invention.
Claims (8)
1. The regeneration method of the ion exchange resin for removing impurities from the lithium sulfate solution is characterized by comprising the following specific steps of:
s1, backwashing the ion exchange resin after adsorption saturation from bottom to top by using pure water with the volume of 1-5 times of the resin, and performing replacement treatment on substances in the system;
s2, analyzing the ion exchange resin cleaned in the S1 by using a dilute sulfuric acid solution, wherein during analysis, the dilute sulfuric acid solution with the volume 1-5 times of that of the resin is used to ensure that impurity ions are sufficiently analyzed;
s3, washing the ion exchange resin analyzed by the S2 by using pure water with the volume 1-3 times of that of the resin, and replacing a dilute sulfuric acid solution in the system;
s4, regenerating the ion exchange resin washed by the S3 by using lithium carbonate lithium precipitation mother liquor, wherein during regeneration, the lithium precipitation mother liquor with 2-6 times of the volume of the resin is used to ensure that sodium ions are fully regenerated;
and S5, washing the regenerated ion exchange resin of S4 by using pure water with the volume 1-3 times of the resin, and replacing lithium precipitation mother liquor in the system to obtain the regenerated ion exchange resin.
2. The method of claim 1, wherein the ion exchange resin is a macroporous chelating resin.
3. The method according to claim 1, wherein the dilute sulfuric acid solution has a concentration of 7% or less in S2, and the pH is maintained at 4 or less during the circulation.
4. The method according to claim 1, wherein the flow rate of the dilute sulfuric acid solution through the ion exchange resin in S2 is 2-6 BV/h.
5. The method according to claim 1, wherein in S4, the lithium precipitation mother liquor is 1.5-4.5% sodium carbonate solution.
6. The regeneration method of the ion exchange resin for removing impurities from the lithium sulfate solution, according to claim 1, is characterized in that in S4, the flow rate of the lithium precipitation mother solution passing through the resin is 1-5 BV/h.
7. The method according to claim 1, wherein in S2, the dilute sulfuric acid solution can be recycled or not, and when the dilute sulfuric acid solution is recycled, a filtering device is added before the recycled dilute sulfuric acid solution enters the resin tank to prevent calcium sulfate particulate matters from entering the resin system.
8. The method for regenerating ion exchange resin used for removing impurities from lithium sulfate solution according to claim 1, wherein the regenerated ion exchange resin is used in single column or multiple columns in series when used for removing impurities from lithium sulfate solution.
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| CN116177572A (en) * | 2022-12-05 | 2023-05-30 | 四川国理锂材料有限公司 | Calcium removal production process of lithium sulfate solution |
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