A method for regenerating a strong alkaline anion resin for separating tungsten and molybdenum
By using Fe-Cl coordination ions formed by dissolving FeCl3 in HCl solution as a regeneration agent, the problems of poor desorption effect and easy damage of strong alkaline anion resin in the tungsten and molybdenum separation process were solved, and efficient regeneration and stable separation of the resin were achieved.
Patent Information
- Application Number
- CN202311251874.X
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2023-09-26
- Publication Date
- 2025-09-23
- Estimated Expiration
- 2043-09-26
AI Technical Summary
In the existing technology, strong alkaline anion resin has poor desorption effect during the tungsten-molybdenum separation process and the resin structure is easily destroyed by oxidation, resulting in unsatisfactory regeneration effect and difficulty in continuous and efficient separation.
FeCl3 dissolved in HCl solution forms Fe-Cl coordination ions with low hydration energy as a regeneration agent. The MoS42- loaded in the resin is exchanged and hydrolyzed into free Fe3+ and Cl- in HCl solution with a pH of 1 to 3, thereby avoiding damage to the resin structure and achieving resin regeneration.
Effectively remove MoS42-, extend resin life, reduce costs, maintain resin regeneration effect and separation efficiency, and avoid damage to resin by oxidants.
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Abstract
Description
Technical Field
[0001] The invention belongs to the technical field of rare metal separation, and in particular relates to a method for regenerating a strong alkaline anion resin for separating tungsten and molybdenum. Background Art
[0002] Tungsten (W) and molybdenum (Mo) are both rare metals belonging to Group VIB, and are located in the sixth and fifth periods, respectively. Tungsten and molybdenum often coexist in minerals and waste materials, and their atomic radius, chemical valence state, and chemical properties in aqueous solutions are extremely similar. Therefore, efficient separation of tungsten and molybdenum is a major challenge in the metallurgical and chemical industries. Reported methods for separating tungsten and molybdenum include extraction, precipitation, ion exchange, and liquid membrane separation. The paper "Research Progress on Tungsten and Molybdenum Separation Processes and Mechanisms" published by Zhao Wendi et al. and the paper "Review of Research Progress in Tungsten and Molybdenum Separation Technologies" published by Sun Zhimin et al. describe existing precipitation, extraction, and ion exchange methods. Extraction requires large amounts of organic extractants, some of which are unstable and prone to loss, resulting in inconsistent separation results. Precipitation is a commonly used method for separating tungsten and molybdenum in industry, but it suffers from limitations such as high precipitant usage and high costs. Ion exchange is a simpler method for separating tungsten and molybdenum, effectively removing impurities, and has garnered significant attention in recent years.
[0003] The ion exchange method uses the characteristics of "tungsten is oxygen-friendly and molybdenum is sulfur-friendly" to first sulfide the tungsten-molybdenum liquid. By controlling the S / Mo ratio and pH and other factors, the Mo in the tungsten-molybdenum liquid can be converted into MoS4. 2- , and W is still WO4 2- exists in the form of MoS4 2- and WO4 2- The difference in physical and chemical properties between tungsten and molybdenum can achieve the separation of tungsten and molybdenum. Existing research shows that quaternary ammonium strong basic anion exchange resin has a strong affinity for MoS4 2- The affinity is much higher than WO4 2- , can be used for the targeted separation of molybdenum from tungsten sulfide molybdenum liquid. However, it is precisely because this type of resin has a strong affinity for MoS4 2- With high selectivity, the adsorbed MoS4 2- It is difficult to desorb, which becomes the main technical bottleneck for the promotion and application of this technology. 2- Desorption, the existing technology uses oxidation technology to desorb MoS4 2- Transformed into MoO4 2- , then use NaCl or NaOH to 2- Desorption regeneration is performed, in which strong oxidants commonly used include H2O2, NaClO, etc. However, these oxidants are not very effective in oxidizing MoS4 2-This process can also easily lead to oxidation and damage to the resin structure, hindering resin regeneration and making it difficult to ensure the resin's continued high-efficiency tungsten-molybdenum separation. Chinese patent application CN 113789442 A discloses a method for separating tungsten and molybdenum from an ammonium tungstate solution using LX363 resin. The method includes resin pretreatment, pretreatment of the ammonium tungstate solution with ammonium sulfide, adsorption on an adsorption column, two-stage, two-stage cyclic desorption using a sodium hydroxide solution, acid washing, and water washing. While this method can achieve tungsten-molybdenum separation, the desorption step is complex and the resin regeneration effect is less than ideal.
[0004] Therefore, it is of great significance to provide a method for regenerating a strong alkaline anion resin that is efficient in desorption and can avoid oxidative damage to the resin structure. Summary of the Invention
[0005] To solve the problems existing in the prior art, the inventors conducted a large number of experiments to study the desorption and regeneration of strong basic anion resins used for tungsten and molybdenum separation. Unexpectedly, they found that by dissolving FeCl3 in HCl solution at a certain molar concentration ratio, low hydration energy Fe-Cl coordination ions were formed as regeneration agents for targeted removal of Mo in tungsten and molybdenum feed solutions; low hydration energy Fe-Cl coordination ions have a high affinity with strong basic anion resins and can be used to exchange MoS4 loaded in the resin. 2- After desorption, the Fe-Cl coordination ions loaded on the resin can be hydrolyzed into free Fe in HCl solution with a pH of 1 to 3. 3+ and Cl - , removing the regeneration agent does not affect the resin's targeted adsorption of MoS4 2- The performance of the present invention can replace the conventional strong oxidant oxidation method, avoid the damage of the resin structure, extend the service life of the resin, have a good regeneration effect, and reduce costs. Based on the above findings, the present invention is completed.
[0006] The purpose of the present invention will be further reflected and explained through the following detailed description.
[0007] The present invention provides a method for regenerating a strong basic anion resin for separating tungsten and molybdenum, comprising the following steps:
[0008] S1, soaking a strong basic anion resin in deionized water to swell it, separating it, washing it with an HCl solution and then a NaOH solution, and drying it to obtain resin A1;
[0009] S2, using a sulfurizing agent to sulfurize the tungsten and molybdenum liquid to obtain a mixed liquid B1;
[0010] S3, adding the resin A1 to the mixed solution B1, shaking and adsorbing, and separating to obtain resin A2;
[0011] S4, dissolving FeCl3 in HCl solution, wherein the molar concentration ratio of HCl to FeCl3 is 3 to 5:1, to obtain a mixed solution B2 containing a regeneration agent;
[0012] S5, adding the resin A2 to the mixed solution B2, shaking and desorbing, and separating to obtain resin A3;
[0013] S6. Dispersing the resin A3 in a HCl solution with a pH of 1 to 3, adding a sodium hydroxide solution dropwise to maintain pH stability, removing the regeneration agent, separating, and repeatedly washing with water, and drying to obtain a regenerated resin A4.
[0014] Preferably, the strong base anion resin is a quaternary ammonium strong base anion resin selected from D201, A-62MP or 1×4.
[0015] Preferably, in step S1, the concentration of the HCl solution is 0.5-2 mol / L, the concentration of the NaOH solution is 0.5-2 mol / L, and the NaOH solution is used for washing until the pH of the separated liquid is 6.5-8.5. More preferably, the soaking and swelling time is 12-24 hours, the volume ratio of the resin to deionized water is 1:(3-5); the solid-liquid ratio of the HCl solution washing is (50-200 g) / 500 mL, and the soaking time is 2-6 hours; the solid-liquid ratio of the NaOH solution washing is (50-200 g) / 500 mL, and the soaking time is 2-6 hours.
[0016] Preferably, in step S2, the sulfurizing agent is selected from Na2S, NaHS, H2S, or (NH4)2S, the mass concentration ratio of WO3 to Mo in the tungsten-molybdenum slurry is 25-75:1, and the sulfurization treatment conditions include: a molar concentration ratio of S to Mo is 4-12:1, and a sulfurization time of 18-24 hours. More preferably, the sulfurization treatment conditions also include: a temperature of 20-30°C and a rotation speed of 150-300 rpm in a constant temperature gas bath oscillator.
[0017] Preferably, the pH of the mixed solution B1 is 7-9.
[0018] Preferably, in step S3, the conditions for the oscillation adsorption include: a solid-liquid ratio of 30-40 g:1 L, a temperature of 20-30° C., a rotation speed of 150-300 rpm, and an adsorption time of 20-30 h. In step S3, the oscillation adsorption of thiomolybdate achieves separation of tungsten and molybdenum.
[0019] Preferably, the FeCl3 is separated from industrial pickling wastewater (containing a large amount of ferrous ions) through simple oxidation.
[0020] Preferably, in step S5, the conditions for oscillation desorption include: a solid-liquid ratio of 10 to 30 g:1 L, a temperature of 20 to 30° C., a rotation speed of 150 to 300 rpm, and a desorption time of 20 to 30 h.
[0021] Preferably, in step S6, water washing is repeated until the pH of the separation liquid is 5.5 to 6.3.
[0022] In step S6, maintaining pH stability means that pH fluctuation is within the range of ±0.2.
[0023] More preferably, the dispersion is static immersion with a solid-liquid ratio of 60 to 100 g:1L.
[0024] Compared with the prior art, the present invention has the following advantages: the present invention provides a method for regenerating a strong basic anion resin for tungsten and molybdenum separation, wherein FeCl3 is dissolved in an HCl solution at a certain molar concentration ratio to form Fe-Cl coordination ions with low hydration energy, which are used as a regeneration agent for targeted removal of Mo in the tungsten and molybdenum feed solution; the low hydration energy Fe-Cl coordination ions have a high affinity with the strong basic anion resin and can be used to exchange the MoS4 loaded in the resin. 2- After desorption, the Fe-Cl coordination ions loaded on the resin can be hydrolyzed into free Fe in HCl solution with a pH of 1 to 3. 3+ and Cl - , removing the regeneration agent does not affect the resin's targeted adsorption of MoS4 2- The performance of the present invention can replace the conventional strong oxidant oxidation method, avoid the damage of the resin structure, extend the service life of the resin, have a good regeneration effect, and reduce costs. Based on the above findings, the present invention is completed. DETAILED DESCRIPTION
[0025] The present invention is further described in detail below through specific examples.
[0026] In the present invention, the materials and equipment involved are all conventional commercially available products, and the relevant methods are performed according to conventional methods in the art or relevant instructions.
[0027] Example 1: Regeneration Method of Strongly Basic Anion Resin for Tungsten-Molybdenum Separation
[0028] A method for regenerating a strong basic anion resin for separating tungsten and molybdenum comprises the following steps:
[0029] S1, 100g D201 strong basic anion resin was soaked and swollen in 4 volumes of deionized water for 24h. After separation, the swollen resin was dispersed in 1mol / L HCl solution and soaked for 4h, washed with deionized water until neutral, and then soaked in 1mol / L NaOH solution for 4h, washed with deionized water until neutral, and placed in an oven to dry to obtain resin A1;
[0030] S2. Weigh 44.8477 g of Na2WO4·2H2O and 1.2609 g of Na2Mo4·2H2O, dissolve them in 250 mL of deionized water, add HCl dropwise to adjust the pH to 7, and prepare a tungsten-molybdenum solution with a WO3 concentration of 100 g / L and a Mo concentration of 2 g / L. Place the solution in a constant temperature oscillator, add 10.0138 g of Na2S·9H2O, and oscillate and sulfide the tungsten-molybdenum solution at 25°C, 250 rpm, and 24 h to obtain a sulfided mixed solution B1.
[0031] S3, 0.6 g of the resin A1 was added to 20 mL of the mixed solution B1, and the mixture was shaken and adsorbed at 25° C. and 250 rpm for 24 h to separate the resin A2. After filtering with a 0.45 μm filter membrane, the concentration of residual tungsten and molybdenum in the filtrate was determined using a German Jena inductively coupled plasma emission spectrometer PQ9000, and the tungsten and molybdenum removal effect was calculated. The results are shown in Table 1;
[0032] S4, prepare 0.5 mol / L FeCl3 and 2 mol / L HCl solutions respectively, mix the two solutions in equal volumes at 200 rpm for 30 min to obtain a mixed solution B2 containing the regeneration agent;
[0033] S5, adding 0.4 g of the dry resin A2 obtained in step S3 to 20 mL of the mixed solution B2, placing it in a constant temperature oscillator and shaking it at 250 rpm for 24 h for desorption, and separating to obtain resin A3;
[0034] S6. Disperse the resin A3 in a HCl solution with a pH of 2 and soak for 2 h. Add NaOH dropwise to maintain pH stability. The solid-liquid ratio of resin A3 to HCl solution is 80 g:1 L. Remove the regeneration agent, filter and separate, and repeatedly wash with water until the pH of the washing solution is 6. After drying, obtain regenerated resin A4.
[0035] The regenerated resin A4 obtained in step S6 replaces the resin A1 in step S3, and the operations of steps S4 to S6 are repeated to perform the first and second regenerations. The tungsten and molybdenum removal effects of the regenerated resin are shown in Table 1.
[0036] Table 1 Separation effect of tungsten and molybdenum of original clean resin and regenerated resin (0.5mol / LFeCl3+2mol / LHCl)
[0037]
[0038] As can be seen from Table 1, the strong alkaline anion resin regeneration method for tungsten-molybdenum separation provided by the present invention does not require the use of a strong oxidant. The original clean resin, the first regenerated resin, and the second regenerated resin can all significantly remove molybdenum, while the loss of tungsten is relatively small, thereby achieving tungsten-molybdenum separation.
[0039] Example 2: Regeneration Method of Strongly Basic Anion Resin for Tungsten-Molybdenum Separation
[0040] A method for regenerating a strong basic anion resin for separating tungsten and molybdenum comprises the following steps:
[0041] S1, 100g D201 strong basic anion resin was soaked and swollen in 4 volumes of deionized water for 24h. After separation, the swollen resin was dispersed in 1mol / L HCl solution and soaked for 4h, washed with deionized water until neutral, and then soaked in 1mol / L NaOH solution for 4h, washed with deionized water until neutral, and placed in an oven to dry to obtain resin A1;
[0042] S2. Weigh 44.8477 g of Na2WO4·2H2O and 1.2609 g of Na2Mo4·2H2O, dissolve them in 250 mL of deionized water, add HCl dropwise to adjust the pH to 7, and prepare a tungsten-molybdenum solution with a WO3 concentration of 100 g / L and a Mo concentration of 2 g / L. Place the solution in a constant temperature oscillator, add 10.0138 g of Na2S·9H2O, and oscillate and sulfide the tungsten-molybdenum solution at 25°C, 250 rpm, and 24 h to obtain a sulfided mixed solution B1.
[0043] S3, 0.6 g of the resin A1 was added to 20 mL of the mixed solution B1, and the mixture was shaken and adsorbed at 25° C. and 250 rpm for 24 h to separate the resin A2. After filtering with a 0.45 μm filter membrane, the concentration of residual tungsten and molybdenum in the filtrate was determined using a German Jena inductively coupled plasma emission spectrometer PQ9000, and the tungsten and molybdenum removal effect was calculated. The results are shown in Table 2;
[0044] S4, prepare 1 mol / L FeCl3 and 4 mol / L HCl solutions respectively, mix the two solutions in equal volumes at 200 rpm for 30 min to obtain a mixed solution B2 containing the regeneration agent;
[0045] S5, adding 0.4 g of the dry resin A2 obtained in step S3 to 20 mL of the mixed solution B2, placing it in a constant temperature oscillator and shaking it at 250 rpm for 24 h for desorption, and separating to obtain resin A3;
[0046] S6. Disperse the resin A3 in a HCl solution with a pH of 2 and soak for 2 h. Add NaOH dropwise to maintain pH stability. The solid-liquid ratio of resin A3 to HCl solution is 80 g:1 L. Remove the regeneration agent, filter and separate, and repeatedly wash with water until the pH of the washing solution is 6. After drying, obtain regenerated resin A4.
[0047] The regenerated resin A4 obtained in step S6 replaces the resin A1 in step S3, and the operations of steps S4 to S6 are repeated to perform the first and second regenerations. The tungsten and molybdenum removal effects of the regenerated resin are shown in Table 2.
[0048] Table 2 Separation effect of tungsten and molybdenum of original clean resin and regenerated resin (1mol / LFeCl3+4mol / LHCl)
[0049]
[0050] As can be seen from Table 2, the strong alkaline anion resin regeneration method for tungsten-molybdenum separation provided by the present invention does not require the use of a strong oxidant. The original clean resin, the first regenerated resin, and the second regenerated resin can all significantly remove molybdenum, while the loss of tungsten is relatively small, thereby achieving tungsten-molybdenum separation.
[0051] Comparative Example 1
[0052] A method for regenerating a strong basic anion resin for separating tungsten and molybdenum comprises the following steps:
[0053] S1, 100g D201 strong basic anion resin was soaked and swollen in 4 volumes of deionized water for 24h. After separation, the swollen resin was dispersed in 1mol / L HCl solution and soaked for 4h, washed with deionized water until neutral, and then soaked in 1mol / L NaOH solution for 4h, washed with deionized water until neutral, and placed in an oven to dry to obtain resin A1;
[0054] S2. Weigh 44.8477 g of Na2WO4·2H2O and 1.2609 g of Na2Mo4·2H2O, dissolve them in 250 mL of deionized water, add HCl dropwise to adjust the pH to 7, and prepare a tungsten-molybdenum solution with a WO3 concentration of 100 g / L and a Mo concentration of 2 g / L. Place the solution in a constant temperature oscillator, add 10.0138 g of Na2S·9H2O, and oscillate and sulfide the tungsten-molybdenum solution at 25°C, 250 rpm, and 24 h to obtain a sulfided mixed solution B1.
[0055] S3, 0.6 g of the resin A1 was added to 20 mL of the mixed solution B1, and the mixture was shaken and adsorbed at 25° C. and 250 rpm for 24 h to separate the resin A2. After filtering with a 0.45 μm filter membrane, the concentration of residual tungsten and molybdenum in the filtrate was determined using a German Jena inductively coupled plasma emission spectrometer PQ9000, and the tungsten and molybdenum removal effect was calculated. The results are shown in Table 3;
[0056] S4, respectively preparing 0.1, 0.5, 1, and 5 mol / L NaNO3 and NaClO4 solutions (low hydration energy) and using them as regeneration solutions (instead of the mixed solution B2 containing the regeneration agent in Example 1);
[0057] S5, adding 0.4 g of the dry resin A2 obtained in step S3 to 20 mL of the regeneration solution, placing it in a constant temperature oscillator and shaking it at 250 rpm for 24 h for desorption, and separating to obtain resin A3;
[0058] S6. The resin A3 is repeatedly washed with water until the pH of the washing solution reaches 6, and then dried to obtain the regenerated resin A4.
[0059] The regenerated resin A4 obtained in step S6 replaces the resin A1 in step S3, and the operations of steps S4 to S6 are repeated for the first time. The tungsten and molybdenum removal effects of the regenerated resin are shown in Table 3.
[0060] Table 3 Separation effect of tungsten and molybdenum of original clean resin and NaNO3, NaClO4 first regeneration resin
[0061]
[0062] As can be seen from Table 3, when low hydration energy NaNO3 and NaClO4 solutions are used as regeneration liquids, the tungsten removal rate of the first regenerated resin in Comparative Example 1 is significantly higher than that of the first regenerated resin in Example 1 of the present invention, and the molybdenum removal rate of the first regenerated resin in Comparative Example 1 (less than 90%) is significantly lower than that of the first regenerated resin in Example 1 of the present invention, and is not suitable for the second regeneration process.
[0063] Comparative Example 2
[0064] A method for regenerating a strong basic anion resin for separating tungsten and molybdenum comprises the following steps:
[0065] S1, soak 100g of strong basic anion resin in 4 volumes of deionized water and swell for 24h. After separation, the swollen resin is dispersed in 1mol / L HCl solution and soaked for 4h, washed with deionized water until neutral, and then soaked in 1mol / L NaOH solution for 4h, washed with deionized water until neutral, and placed in an oven to dry to obtain resin A1;
[0066] S2. Weigh 44.8477 g of Na2WO4·2H2O and 1.2609 g of Na2Mo4·2H2O, dissolve them in 250 mL of deionized water, add HCl dropwise to adjust the pH to 7, and prepare a tungsten-molybdenum solution with a WO3 concentration of 100 g / L and a Mo concentration of 2 g / L. Place the solution in a constant temperature oscillator, add 10.0138 g of Na2S·9H2O, and oscillate and sulfide the tungsten-molybdenum solution at 25°C, 250 rpm, and 24 h to obtain a sulfided mixed solution B1.
[0067] S3, 0.6 g of the resin A1 was added to 20 mL of the mixed solution B1, and the mixture was shaken and adsorbed at 25 ° C. and 250 rpm for 24 h to separate the resin A2. After filtering with a 0.45 μm filter membrane, the concentration of residual tungsten and molybdenum in the filtrate was determined using a German Jena inductively coupled plasma emission spectrometer PQ9000, and the tungsten and molybdenum removal effect was calculated. The results are shown in Table 4;
[0068] S4, respectively prepare 2 mol / L FeCl3 and 0.5 mol / L, and mix the two solutions at equal volumes at 200 rpm for 30 min to obtain a mixed solution B2 containing a regenerant (replacing the mixed solution B2 containing a regenerant in Example 1);
[0069] S5, adding 0.4 g of the dry resin A2 obtained in step S3 to 20 mL of the mixed solution B2, placing it in a constant temperature oscillator and shaking it at 250 rpm for 24 h for desorption, and separating to obtain resin A3;
[0070] S6. The resin A3 was dispersed in HCl solutions with pH values of 1, 2, 3, and 4, respectively, and soaked for 2 h. NaOH was added dropwise to maintain pH stability. The solid-liquid ratio of the resin A3 to the HCl solution was 80 g:1 L. The regeneration agent was removed, and the mixture was filtered and separated, followed by repeated water washing until the pH value of the washing solution reached 6. The regenerated resin A4 was obtained after drying.
[0071] The regenerated resin A4 obtained in step S6 replaces the resin A1 in step S3, and the operations of steps S4 to S6 are repeated to perform the first regeneration. The tungsten and molybdenum removal effects of the regenerated resin are shown in Table 4.
[0072] Table 4 Separation effect of tungsten and molybdenum of the original clean resin and the first regenerated resin (2mol / L FeCl3+0.5mol / L HCl)
[0073]
[0074] As can be seen from Table 4, using mixed solutions of FeCl3 and HCl with different concentrations as the mixed solution B2 containing the regeneration agent, the molybdenum removal rate of the first regenerated resin in Comparative Example 2 (less than 90%) is significantly lower than the removal rate of the first regenerated resin in Example 1 of the present invention, and is not suitable for the second regeneration process.
[0075] The above is a further detailed description of the present invention in conjunction with specific preferred embodiments, and the specific implementation of the present invention should not be considered to be limited to these descriptions. For those skilled in the art of the present invention, without departing from the concept of the present invention, several simple deductions or substitutions can be made, which should be considered to fall within the scope of protection of the present invention.
Claims
1. A method for regenerating a strong basic anion resin for separating tungsten and molybdenum, characterized in that: The steps include: S1, soaking a strong basic anion resin in deionized water to swell it, separating it, washing it with an HCl solution and then a NaOH solution, and drying it to obtain resin A1; S2, using a sulfurizing agent to sulfurize the tungsten and molybdenum liquid to obtain a mixed liquid B1; S3, adding the resin A1 to the mixed solution B1, shaking and adsorbing, and separating to obtain resin A2; S4, dissolving FeCl3 in HCl solution, wherein the molar concentration ratio of HCl to FeCl3 is 3 to 5:1, to obtain a mixed solution B2 containing a regeneration agent; S5, adding the resin A2 to the mixed solution B2, shaking and desorbing, and separating to obtain resin A3; S6. Dispersing the resin A3 in a HCl solution with a pH of 1 to 3, adding a sodium hydroxide solution dropwise to maintain pH stability, removing the regeneration agent, separating, and repeatedly washing with water, and drying to obtain a regenerated resin A4.
2. The method for regenerating a strong basic anion resin for separating tungsten and molybdenum according to claim 1, wherein: The strong base anion resin is a quaternary ammonium strong base anion resin selected from D201 or 1×4.
3. The method for regenerating a strong basic anion resin for separating tungsten and molybdenum according to claim 1 or 2, characterized in that: In step S1, the concentration of the HCl solution is 0.5-2 mol / L, the concentration of the NaOH solution is 0.5-2 mol / L, and the NaOH solution is used for washing until the pH of the separated liquid is 6.5-8.
5.
4. The method for regenerating a strong basic anion resin for separating tungsten and molybdenum according to claim 1 or 2, characterized in that: In step S2, the sulfiding agent is selected from Na2S, NaHS, H2S or (NH4)2S, the mass concentration ratio of WO3 to Mo in the tungsten-molybdenum slurry is 25-75:1, and the sulfiding treatment conditions include: the molar concentration ratio of S to Mo is 4-12:1, and the sulfiding time is 18-24 hours.
5. The method for regenerating a strong basic anion resin for separating tungsten and molybdenum according to claim 1 or 2, characterized in that: The pH of the mixed solution B1 is 7-9.
6. The method for regenerating a strong basic anion resin for separating tungsten and molybdenum according to claim 1 or 2, characterized in that: In step S3, the conditions for oscillation adsorption include: a solid-liquid ratio of 30 to 40 g:1 L, a temperature of 20 to 30° C., a rotation speed of 150 to 300 rpm, and an adsorption time of 20 to 30 h.
7. The method for regenerating a strong basic anion resin for separating tungsten and molybdenum according to claim 1 or 2, characterized in that: In step S5, the conditions for oscillation desorption include: a solid-liquid ratio of 10 to 30 g:1 L, a temperature of 20 to 30° C., a rotation speed of 150 to 300 rpm, and a desorption time of 20 to 30 h.
8. The method for regenerating a strong basic anion resin for separating tungsten and molybdenum according to claim 1 or 2, characterized in that: In step S6, water washing is repeated until the pH of the separated liquid is 5.5-6.3.
Citation Information
Patent Citations
Method for separating tungsten and molybdenum in ammonium tungstate solution by using LX363 resin
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Method for separating molybdenum from tungstate solution through ion exchange
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