Method for purifying novel chelate resin TP220 in cobaltous sulfate

Abstract

The invention discloses a method for purifying novel chelate resin TP220 in cobaltous sulfate. The method specifically comprises the following steps: filling pretreated TP220 resin into an ion exchange column; the method comprises the following steps: dissolving industrial-grade cobalt sulfate salt to prepare a cobalt salt solution with a certain concentration, and adjusting the cobalt salt solution to a certain pH value; the cobalt salt solution is introduced into a TP220 resin ion exchange column to complete an ion exchange reaction, and an exchanged solution is obtained.The novel chelating resin TP220 is adopted, the treatment depth is high, selectivity is good, impurities such as Cu, Ni, Pb, Zn and Fe in the cobalt sulfate salt solution can be removed at a time, the grade of the high-purity cobalt sulfate salt prepared from the purified solution reaches the battery grade, and the quality of the high-purity cobalt sulfate salt reaches the battery grade. The grade of the prepared high-purity cobalt plate reaches 99.9999% or above, the method is simple and easy to implement, the requirement for equipment is low, compared with an extraction method, the treatment depth is higher than that of the extraction method, and the method is free of pollution and environmentally friendly.

Description

Technical Field

[0001] The invention relates to the field of chemical industry, in particular to a method for purifying a novel chelating resin TP220 in cobalt sulfate. Background Art

[0002] As an important raw material, cobalt sulfate is widely used in the production of synthetic battery materials and electrolytic cobalt. With the rapid development of the battery industry, the requirements for the grade of cobalt sulfate are getting higher and higher, and the purity of cobalt sulfate directly affects the performance of the battery. At the same time, the preparation of high-purity electrolytic cobalt also requires a cobalt sulfate solution with higher purity. The impurity ions in the cobalt sulfate solution mainly include Cu, Ni, Pb, Zn, Fe, etc. The traditional impurity removal methods mainly include precipitation, displacement, extraction, ion exchange, etc. Among them, precipitation and displacement are primary impurity removal methods with low processing depth, which generally cannot meet the requirements of deep processing. Extraction and ion exchange are deep impurity removal methods. The equipment required for the extraction method is large, consumes a lot of organic solvents, has a long processing flow, and has complicated procedures, which has great pollution to the environment. Compared with the extraction method, the ion exchange method has great advantages. The ion exchange method has small equipment volume, short processing flow, clean and environmentally friendly, and no pollution to the environment. However, traditional ion exchange resins can only remove one or two impurities, have poor selectivity, and have a small exchange capacity. They need to be repeatedly cleaned and regenerated, consume a large amount of acid and pure water, and the treatment depth does not meet the required requirements. Summary of the invention

[0003] In order to overcome the above-mentioned shortcomings, the present invention aims to provide a technical solution that can solve the above-mentioned problems.

[0004] A purification method of a novel chelating resin TP220 in cobalt sulfate specifically comprises the following steps: S1, loading the pretreated TP220 resin into an ion exchange column; S2, dissolving industrial-grade cobalt sulfate to prepare a cobalt salt solution of a certain concentration, and adjusting the cobalt salt solution to a certain pH value; S3, passing the cobalt salt solution into a TP220 resin ion exchange column to complete the ion exchange reaction and obtain an exchange liquid.

[0005] As a further solution of the present invention: the cobalt salt solution is a CoSO4 solution.

[0006] As a further solution of the present invention: the working temperature of the above purification method is 20°C-70°C.

[0007] As a further solution of the present invention: the pH value of the cobalt salt solution is adjusted to a range of 1 to 3.

[0008] As a further solution of the present invention: the ion exchange reaction adopts a static adsorption method or a dynamic ion exchange column method.

[0009] The beneficial effects of the present invention are as follows: the present invention adopts a novel chelating resin TP220, which has high processing depth and good selectivity, and can remove impurities such as Cu, Ni, Pb, Zn, Fe and the like in a cobalt sulfate salt solution at one time. The grade of the high-purity cobalt sulfate salt obtained from the purified solution reaches the battery grade, and the grade of the obtained high-purity cobalt plate reaches the level of more than 99.9999%. The method is simple and easy to implement, and has low requirements on equipment. Compared with the extraction method, the present invention not only has a higher processing depth than the extraction method, but also is pollution-free and environmentally friendly.

[0010] Additional aspects and advantages of the present invention will be given in part in the following description and in part will be obvious from the following description, or will be learned through practice of the present invention. BRIEF DESCRIPTION OF THE DRAWINGS

[0011] Figure 1 It is a process flow chart of the present invention. DETAILED DESCRIPTION

[0012] The technical solutions in the embodiments of the present invention are described clearly and completely below. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of them. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0013] Embodiment 1 of the present invention, a method for purifying a novel chelating resin TP220 in cobalt sulfate, comprises the following specific steps: loading 100 mL of the pretreated TP220 resin into an ion exchange column, preparing a cobalt sulfate solution with industrial-grade cobalt sulfate crystals, taking 2000 mL of the cobalt sulfate solution to adjust the pH value of the solution to about 1.5, passing the solution into the ion exchange column, controlling the liquid discharge speed to 2 BV / h, backwashing and regenerating the resin after the exchange, sampling and analyzing the solution after the exchange, and the results are shown in Table 1.

[0014] Table 1 Comparison of solution impurity indicators before and after ion exchange The above solution was placed in a rotary evaporator for evaporation and crystallization to obtain cobalt sulfate crystals. The indicators of the cobalt sulfate crystals are shown in Table 2.

[0015] Table 2 Comparison of sample indicators and refined cobalt sulfate indicators Example 2 of the present invention, the specific steps include placing 100 mL of the pretreated TP220 resin in a conical flask, dissolving industrial-grade cobalt sulfate, taking 500 mL of the cobalt sulfate solution to adjust the pH value of the solution to about 2.5, adding the solution to the conical flask, sealing the conical flask, placing it in a constant temperature oscillator and shaking it for 2 hours, filtering and sampling, and the indicators of the obtained solution are shown in Table 3.

[0016] Table 3 Comparison of solution impurity content before and after ion exchange The above solution was placed in a rotary evaporator for evaporation and crystallization to obtain cobalt sulfate crystals. The indicators of the cobalt sulfate crystals are shown in Table 4.

[0017] Table 4 Comparison table of sample indicators and refined cobalt sulfate indicators Embodiment 3 of the present invention, a method for purifying a novel chelating resin TP220 in cobalt sulfate, comprises the following specific steps: loading 200 mL of the pretreated TP220 resin into an ion exchange column, preparing a cobalt sulfate solution with industrial-grade cobalt sulfate crystals, taking 4000 mL of the cobalt sulfate solution to adjust the pH value of the solution to about 2, passing the solution into the ion exchange column, controlling the liquid discharge speed to 3 BV / h, backwashing and regenerating the resin after the exchange, sampling and analyzing the solution after the exchange, and the results are shown in Table 5.

[0018] Table 5 Comparison of solution impurity content before and after ion exchange The above solution was placed in a beaker, with a titanium plate as cathode and a titanium-coated ruthenium mesh as anode. Power was turned on to start electrolysis, the cell voltage was controlled at 3.0-3.5V, the temperature was around 60°C, the electrolysis cycle was 72h, and after the electrolysis was completed, a high-purity cobalt plate was taken for GDMS testing. The test results are shown in Table 6.

[0019] Table 6 GDMS test report of high purity cobalt plate Test items Test results (ppb) Test items Test results (ppb) Test items Test results (ppb) Test items Test results (ppb) Li 0.1 Cr 0.6 Pb <0.1 Ho <0.1 Be <0.1 Mn 0.2 Ag 4.6 Er <0.1 B <0.1 Fe 27 Cd 0.4 Tm <0.1 C 3.9ppm Ni 529 In 0.1 Yb <0.1 N 220ppm Cu 27 Sn 8.0 Lu <0.1 O 5.6ppm Zn 15 Sb <0.1 Hf <0.1 F 0.7 Ga <0.1 I <0.1 Ta 0.1 Na 18 Ge 0.6 Te 2.7 W <0.1 Mg 0.4 As 47 Cs <0.1 Re <0.1 Al 0.1 Se <0.1 Ba <0.1 Os <0.1 Si 3.5 Br 0.3 La <0.1 Ir 96 P 3.2 R 0.2 Ce <0.1 Pt <0.1 S 84 Sr <0.1 Pr <0.1 Au <0.1 Cl 47 Y <0.1 Nd <0.1 Hg <0.1 K 20 Zr <0.1 Sm <0.1 Tl 0.6 Ca 0.3 Nb <0.1 Eu <0.1 Pb 4.1 Sc <0.1 Mo 2.6 G <0.1 Bi 0.4 Ti 2.7 Ru 16 Tb <0.1 Th <0.1 V <0.1 R <0.1 Dy <0.1 U <0.1 It will be apparent to those skilled in the art that the present invention is not limited to the details of the exemplary embodiments described above and that the present invention can be implemented in other specific forms without departing from the spirit or essential features of the present invention. Therefore, the embodiments should be considered exemplary and non-restrictive in all respects, and the scope of the present invention is defined by the appended claims rather than the above description, and it is intended that all changes falling within the meaning and scope of the equivalent elements of the claims be included in the present invention.

Claims

1. A purification method of novel chelating resin TP220 in cobalt sulfate, characterized in that, The specific steps include: S1, loading the pretreated TP220 resin into an ion exchange column; S2, dissolving industrial-grade cobalt sulfate to prepare a cobalt salt solution of a certain concentration, and adjusting the cobalt salt solution to a certain pH value; S3, passing the cobalt salt solution into a TP220 resin ion exchange column to complete the ion exchange reaction and obtain an exchange liquid.

2. the purification method of novel chelating resin TP220 in cobalt sulfate according to claim 1, is characterized in that, The cobalt salt solution is CoSO4 solution.

3. the purification method of novel chelating resin TP220 in cobalt sulfate according to claim 1, is characterized in that, The working temperature of the above purification method is 20°C-70°C.

4. the purification method of novel chelating resin TP220 in cobalt sulfate according to claim 1, is characterized in that, The pH value of the cobalt salt solution is adjusted to a range of 1 to 3.

5. the purification method of novel chelating resin TP220 in cobalt sulfate according to claim 1 is characterized in that, The ion exchange reaction adopts a static adsorption method or a dynamic ion exchange column method.

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