Comprehensive recovery method of residual organic phase in alkali extraction strip liquor

Abstract

The invention relates to a comprehensive recovery method of a residual organic phase in an alkali extraction strip liquor. The method comprises the following steps: 1) removing oil by resin adsorption; 2) washing the resin; 3) resin desorption; (4) treating a desorption solution; and 5) washing the resin. The macroporous adsorption resin can be used for adsorbing the residual organic phase in the alkali extraction strip liquor, and the recycling of the organic phase and the recycling of the resin can be realized through the desorption regeneration of the ethanol. The affinity of ethanol to the organic phase is higher than the adsorption capacity of resin to the organic phase, so that the organic phase can be dissolved in ethanol after being removed from the resin, the adsorption performance of the resin is recovered under the condition of keeping the structural integrity of the resin, and the purpose of recycling the resin is achieved. The resin desorption solution is a mixed solution of an organic phase and ethanol, and can be directly mixed into an alkali extraction blank organic phase of an industrial production section according to a certain proportion for recycling.

Description

Technical Field

[0001] The invention belongs to the field of rare metal metallurgy, and in particular relates to a comprehensive recovery method of residual organic phase in alkali extraction stripping solution. Background Art

[0002] In the hydrometallurgical process of tungsten and molybdenum separation, the extraction method is widely used in industry, which can be mainly divided into acid extraction and alkaline extraction. Compared with acid extraction, alkaline extraction is more suitable for complex low-grade high-molybdenum tungsten concentrate smelting system, which can realize the closed process of tungsten and molybdenum leaching-extraction, water and alkali can be recycled, the theoretical sodium salt consumption is zero, and there is no tungsten and molybdenum loss caused by precipitation and impurity removal and water phase opening.

[0003] In the alkaline extraction section, due to the fact that the organic phase itself has a certain degree of hydrophilicity, the oil-water ratio is relatively large during the extraction process, and the clarification time is short, resulting in insufficient phase separation, a trace amount of organic phase will remain in the alkaline extraction stripping solution after extraction-washing-stripping. The residual organic phase not only causes the loss of the organic phase in the alkaline extraction circulation system, but also causes the subsequent production process to produce insoluble oily residues, making equipment cleaning difficult, reducing the yield of tungsten and molybdenum, and increasing production costs, thereby affecting economic benefits. Therefore, it is necessary to recycle the residual organic phase in the alkaline extraction stripping solution. Summary of the invention

[0004] In view of the problems of organic phase loss, production of insoluble oily residue, difficulty in equipment cleaning, loss of valuable metal ions, reduced economic benefits, etc. caused by residual organic phase in alkali extraction stripping solution in the current alkaline extraction process, the present invention provides a comprehensive recovery method for residual organic phase in alkali extraction stripping solution.

[0005] The technical solution adopted by the present invention to solve the technical problem is as follows: A comprehensive recovery method for residual organic phase in an alkali extraction stripping solution comprises the following steps: 1) Resin adsorption and oil removal: The macroporous adsorption resin is loaded into the ion exchange column, and the alkaline stripping solution containing trace organic phase is introduced in a top-in and bottom-out manner for dynamic adsorption and oil removal. Under certain temperature conditions, the adsorption flow rate is proportional to the resin volume. When the TOC in the outlet instantaneous alkaline stripping solution is >10mg / L, the adsorption is stopped. At this time, the macroporous adsorption resin adsorbs the organic phase to reach the breakthrough adsorption amount, and the alkaline stripping solution enters the subsequent evaporation and crystallization process; the macroporous adsorption resin that has adsorbed the organic phase to reach the breakthrough adsorption amount is called oil-carrying resin; 2) Resin washing: The oil-carrying resin in step 1 is washed by soaking in pure water, and the washing liquid is discharged to the main system of online alkali extraction and stripping liquid for recycling; 3) Resin desorption: The oil-loaded resin washed in step 2 is dynamically desorbed using ethanol in a bottom-in-top-out manner. Under certain temperature conditions, the desorption flow rate is proportional to the resin volume. The desorption is performed until no oil phase is produced at the outlet sample, and the obtained desorption liquid is an organic phase ethanol mixture; 4) Desorption liquid treatment: The desorption liquid obtained in step 3 is directly mixed into the online alkali extraction blank organic phase according to a certain proportion for recycling; 5) Resin washing: After dynamic desorption in step 3, the macroporous adsorption resin is washed with pure water in a bottom-in and top-out manner. After washing, the macroporous adsorption resin returns to the adsorption link in step 1.

[0006] In the step 1, the adsorption temperature of the macroporous adsorption resin is 20-40° C., and the adsorption flow rate is 2-3 BV / h.

[0007] In the step 1, the penetration adsorption capacity of the macroporous adsorption resin is greater than 0.85 g / ml, and the TOC removal rate is greater than 98.5%.

[0008] In step 2, the amount of pure water used is 1VB, and the soaking time is 30 minutes.

[0009] In the step 3, the ethanol concentration is greater than 90%, the ethanol is prepared from 99.7% analytical pure anhydrous ethanol, and the amount of ethanol used is 2-4VB.

[0010] In the step 3, the desorption temperature of the oil-carrying resin during desorption is 20-40° C., the desorption flow rate is 1-2 BV / h, and the desorption rate is more than 99%.

[0011] In the step 4, the mixing ratio of the desorption liquid and the alkali-extracted blank organic phase is less than 1 / 60; the saturated loaded tungsten and molybdenum content of the organic phase ethanol desorption mixture and the alkali-extracted blank organic phase after mixing is greater than the saturated loaded tungsten and molybdenum content of the blank organic phase.

[0012] In step 5, the pure water washing flow rate is 2BV / h, and the pure water consumption is 4BV.

[0013] Due to the adoption of the above technical solution, the present invention has the following beneficial effects: (1) The present invention is applicable to high-salt solutions with a tungsten content of 110-130 g / L and a molybdenum content of 11-13 g / L. The resin can maintain stable adsorption performance when adsorbing organic phase in high-salt solutions. Multiple simulated cycle tests have verified that the service life of the resin meets the current industrial application cost requirements and can be used for industrial production.

[0014] (2) The macroporous adsorption resin has a good adsorption and oil removal effect. The TOC in the alkaline extraction stripping solution can be reduced from 550-650 mg / L in the inlet water to less than 10 mg / L in the outlet water. The penetration adsorption capacity of the resin is greater than 0.85 g / ml, and the TOC removal rate is above 98.5%. The desorption of the macroporous adsorption resin is simple and energy-saving. The resin can be recycled after desorption and washing, and the resin structure and performance are stable.

[0015] (4) After desorption, the ethanol mixture in the organic phase can be directly mixed and recycled in a certain proportion, and has a positive effect on the alkali extraction system. The entry of ethanol into the system is also beneficial to the phase separation of the alkali extraction organic phase, further reducing the residual organic phase in the alkali extraction stripping liquid.

[0016] (5) It can prevent the subsequent evaporation and crystallization process equipment from being difficult to clean due to the residual organic phase in the alkali extraction and stripping solution, and the subsequent ammonia solution process from producing insoluble oily slag, thereby reducing the difficulty of manual cleaning, improving the tungsten and molybdenum yields, and reducing the cost of treating insoluble oily slag.

[0017] (6) Simple operation, large adsorption processing capacity, high adsorption efficiency, economical and efficient, green and pollution-free. BRIEF DESCRIPTION OF THE DRAWINGS

[0018] Figure 1 It is a schematic diagram of the process of the present invention.

[0019] Figure 2 It is a schematic diagram of the effect of adsorption temperature on the penetration of organic phase into the resin and the TOC removal rate of the alkaline stripping liquid.

[0020] Figure 3 It is a schematic diagram of the effect of adsorption flow rate on the penetration of organic phase into the resin and the TOC removal rate of the alkaline extraction stripping liquid.

[0021] Figure 4 It is a schematic diagram of the relationship between the desorbent ethanol concentration and the ethanol dosage, desorption rate and the resin organic phase penetration adsorption amount.

[0022] Figure 5 It is a schematic diagram of the effect of desorption temperature on ethanol dosage, desorption rate and resin organic phase penetration adsorption.

[0023] Figure 6 It is a schematic diagram of the relationship between desorption flow rate and ethanol dosage, desorption rate and the amount of organic phase penetrating the resin.

[0024] Figure 7 It is a schematic diagram of the effect of cycle number on the penetration adsorption of organic phase into the resin and the TOC removal rate of the alkaline extraction stripping liquid.

[0025] Figure 8 It is a schematic diagram of the ratio of desorption liquid doping to organic phase loading content and load fluctuation ratio. DETAILED DESCRIPTION

[0026] In order to make the purpose, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below in conjunction with the accompanying drawings of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, rather than all of the embodiments.

[0027] Therefore, the detailed description of the embodiments of the present invention provided below is not intended to limit the scope of protection claimed in the present invention, but merely represents selected embodiments of the present invention. Based on the embodiments of the present invention, any modifications, equivalent replacements, improvements, etc. made within the spirit and principles of the present invention should be included in the scope of protection of the present invention. The experimental reagents and materials used in the embodiments of the present invention that are not described in detail are all commercially available, and the technical means used that are not described in detail are prior art.

[0028] The process of the present invention utilizes macroporous adsorption resin to comprehensively recover residual organic phase in alkali extraction stripping solution, which is suitable for high-salt solution with tungsten content of 110-130 g / L and molybdenum content of 11-13 g / L. The macroporous adsorption resin can maintain stable adsorption performance when adsorbing organic phase in high-salt solution. Multiple simulation cycle tests have verified that the service life of the resin meets the current industrial application cost requirements and can be used for industrial production.

[0029] Combined with Figure 1 The comprehensive recovery method of the residual organic phase in the alkali extraction stripping solution comprises the following steps: 1) Resin adsorption and oil removal: The macroporous adsorption resin is loaded into the ion exchange column, and the alkaline stripping solution containing trace organic phase is introduced in a top-in and bottom-out manner for dynamic adsorption and oil removal. The adsorption temperature is 20-40°C, the adsorption flow rate is 2-3BV / h, and the adsorption is stopped when the TOC in the outlet instantaneous sample alkaline stripping solution is >10mg / L. At this time, the macroporous adsorption resin adsorbs the organic phase to reach the breakthrough adsorption amount, and the alkaline stripping solution enters the subsequent evaporation and crystallization process; the breakthrough adsorption amount of the macroporous adsorption resin is greater than 0.85g / ml, and the TOC removal rate is more than 98.5%; the macroporous adsorption resin after adsorbing the organic phase to the breakthrough adsorption amount is called oil-carrying resin; like Figure 2 As shown in the figure, when the temperature is 20℃, the TOC removal rate is 98.9%, and the organic phase penetration adsorption capacity is close to 0.9 g / ml. The TOC removal rate and the organic phase penetration adsorption capacity decrease with the increase of temperature. When the temperature reaches 40℃, the TOC removal rate is 98.64%, and the organic phase penetration adsorption capacity is between 0.87-0.88 g / ml. As the adsorption temperature continues to increase, the conditions that the penetration adsorption capacity of the macroporous adsorption resin is greater than 0.85g / ml and the TOC removal rate is above 98.5% will not be met.

[0030] like Figure 3As shown in the figure, when the adsorption flow rates are 1 and 2 BV / h respectively, the TOC removal rate and the organic phase penetration adsorption amount are not much different, but the adsorption speed is twice as different. In order to improve the adsorption efficiency, the lower limit of the preferred adsorption flow rate is 2BV / h. The TOC removal rate and the organic phase penetration adsorption amount decrease with the increase of the adsorption flow rate. When the adsorption flow rate is lower than 3 BV / h, it will not be able to meet the conditions that the penetration adsorption amount of the macroporous adsorption resin is greater than 0.85g / ml and the TOC removal rate is above 98.5%.

[0031] 2) Resin washing: The oil-loaded resin in step 1 is washed by soaking in pure water, with the amount of pure water being 1VB and the soaking time being 30 minutes; the washing liquid is discharged to the main system of online alkali extraction and stripping liquid for recycling.

[0032] 3) Resin desorption: The oil-loaded resin washed in step 2 is dynamically desorbed using ethanol with a concentration greater than 90% in a bottom-in-top-out manner, with an ethanol dosage of 2-4VB, a desorption temperature of 20-40°C, a desorption flow rate of 1-2BV / h, and desorption until no oil phase is produced in the outlet sample, with a desorption rate of more than 99%, and the resulting desorption liquid is an organic phase ethanol mixture; Ethanol is prepared from 99.7% analytical pure anhydrous ethanol.

[0033] like Figure 4 As shown in the figure, the amount of ethanol used is inversely proportional to its concentration. When the concentration of ethanol is higher than 90%, the desorption rate can reach more than 99%, and the organic phase penetration adsorption amount can be greater than 0.85g / ml. As the ethanol concentration increases, the desorption rate remains basically unchanged, but the organic phase penetration adsorption amount will gradually increase.

[0034] like Figure 5 As shown, the desorption rate, ethanol dosage and organic phase penetration adsorption amount are directly proportional to the desorption temperature. At 20°C, the desorption rate and organic phase penetration adsorption amount have reached the minimum requirements. In order to save energy and not increase energy consumption during the desorption process, room temperature can be selected to complete the desorption.

[0035] like Figure 6 As shown in the figure, when the desorption flow rate is 1-2 BV / h, the desorption rate and the organic phase penetration adsorption amount can reach the minimum requirement. When it exceeds 2 BV / h, the desorption rate and the organic phase penetration adsorption amount decrease rapidly.

[0036] 4) Treatment of desorption liquid: the desorption liquid obtained in step 3 is directly mixed into the online alkaline extraction blank organic phase according to the proportion for recycling; the mixing ratio of the organic phase ethanol desorption mixture, i.e., the desorption liquid and the alkaline extraction blank organic phase, is less than 1 / 60; the saturated loaded tungsten and molybdenum content of the desorption liquid and the alkaline extraction blank organic phase after mixing is greater than the saturated loaded tungsten and molybdenum content of the blank organic phase.

[0037] like Figure 7As shown, assuming that there is no mixing, the volatility of the tungsten and molybdenum content loaded in the organic phase is 0. When the mixing ratio is 1 / 60, the volatility of the tungsten and molybdenum content loaded in the organic phase is close to 0 and does not change much. When the mixing ratio is less than 1 / 60, the volatility of the tungsten and molybdenum content loaded in the organic phase increases, and the tungsten and molybdenum content loaded in the organic phase increases significantly. Moreover, as the mixing ratio decreases, the higher the volatility of the tungsten and molybdenum content loaded in the organic phase, the more the tungsten and molybdenum content loaded in the organic phase increases. When the mixing ratio is greater than 1 / 60, the volatility of the tungsten and molybdenum content loaded in the organic phase decreases significantly, and the tungsten and molybdenum content loaded in the organic phase decreases significantly.

[0038] 5) Resin washing: After dynamic desorption in step 3, the macroporous adsorption resin is washed with pure water in a bottom-in and top-out manner, with a pure water washing flow rate of 2BV / h and a pure water consumption of 4BV. After washing, the macroporous adsorption resin returns to the adsorption link in step 1.

[0039] The present invention utilizes a macroporous adsorption resin to adsorb the residual organic phase in the alkali extraction stripping solution. The macroporous adsorption resin is selected from SD300, SD600, XDA-88, etc., and the organic phase can be recycled and the resin can be used in a circular manner through ethanol desorption and regeneration. The macroporous adsorption resin has a porous network structure and a large specific surface area. The surface adsorption of the organic phase can be achieved by utilizing the comprehensive effects of the lipophilic and hydrophobic properties of the resin through van der Waals forces, hydrogen bonding, electrostatic attraction, solvation, etc. The surface adsorption is reversible. By utilizing the affinity of ethanol for the organic phase being higher than the adsorption force of the resin for the organic phase, the organic phase can be removed from the resin and dissolved in ethanol. Under the condition of maintaining the integrity of the resin structure, its adsorption performance is restored, thereby achieving the purpose of recycling the resin. The resin desorption solution is a mixed solution of the organic phase and ethanol, which can be directly mixed into the alkali extraction blank organic phase of the industrial production section in a certain proportion for recycling.

[0040] The following is attached Figure 1 The present invention is further described in detail with reference to the accompanying drawings and examples. Example

[0041] The alkaline extraction stripping solution in this example comes from a stripping solution containing trace organic phase produced in the alkaline extraction section of a tungsten-molybdenum smelter in Henan Province using low-grade complex scheelite to produce ammonium paratungstate. Samples were taken for testing and found to contain 122.57 g / L tungsten, 12.07 g / L molybdenum, and 592 mg / L TOC.

[0042] 1) Resin adsorption and oil removal: Special modified macroporous adsorption resin is loaded into the ion exchange column, and the alkaline stripping solution containing trace organic phase is introduced in the top-in and bottom-out manner for dynamic adsorption and oil removal. The adsorption flow rate is 2VB / h at room temperature. When TOC>10mg / L in the outlet instantaneous sample alkaline stripping solution, the adsorption is stopped. At this time, the resin adsorbs the organic phase to the breakthrough adsorption amount, which is the oil-loaded resin. The resin organic phase breakthrough adsorption amount is 0.888g / ml, and the TOC removal rate is 98.59%. When the resin adsorbs the organic phase to the breakthrough adsorption amount, it is the oil-loaded resin. After oil removal, the alkaline stripping solution enters the subsequent evaporation and crystallization process; 2) Resin washing: The oil-carrying resin in step 1 is soaked and washed with 1VB pure water for 30 minutes, and the washing liquid is discharged to the main system of online alkali extraction and stripping liquid for recycling; 3) Resin desorption: The oil-carrying resin washed in step 2 is dynamically desorbed using 99.7% analytical pure anhydrous ethanol in a bottom-in and top-out manner, with a desorption flow rate of 1VB / h at room temperature. No oil phase is produced when the outlet sample is desorbed, and the desorption liquid obtained by desorption is an organic phase ethanol mixture. The amount of desorption ethanol used is 2VB, and the desorption rate is 99.67%; 4) Desorption liquid treatment: The desorption liquid obtained in step 3 was directly recycled by doping with the blank organic phase of the online alkaline extraction at 1 / 100. After doping, the tungsten content of the loaded organic phase increased by 2.97% and the molybdenum content increased by 2.62% compared with that without doping; 5) Resin washing: After dynamic desorption in step 3, the resin is washed with pure water in the order of bottom-in and top-out. The pure water washing flow rate is 2BV / h and the pure water consumption is 4BV. After washing, the resin returns to the adsorption link in step 1. Example

[0043] The alkaline extraction stripping solution in this example comes from a stripping solution containing trace organic phase produced in the alkaline extraction section of a tungsten-molybdenum smelter in Henan Province using low-grade complex scheelite to produce ammonium paratungstate. Samples were taken for testing and found to contain 125.76 g / L tungsten, 12.66 g / L molybdenum, and 578 mg / L TOC.

[0044] 1) Resin adsorption and oil removal: Special modified macroporous adsorption resin is loaded into the ion exchange column, and the alkaline stripping solution containing trace organic phase is introduced in the top-in and bottom-out manner for dynamic adsorption and oil removal. The adsorption flow rate is 3VB / h at room temperature. When TOC>10mg / L in the outlet instantaneous sample alkaline stripping solution, the adsorption is stopped. At this time, the resin adsorbs the organic phase to the breakthrough adsorption amount, which is the oil-loaded resin. The resin organic phase breakthrough adsorption amount is 0.874g / ml, and the TOC removal rate is 98.57%. When the resin adsorbs the organic phase to the breakthrough adsorption amount, it is the oil-loaded resin. After oil removal, the alkaline stripping solution enters the subsequent evaporation and crystallization process; 2) Resin washing: The oil-carrying resin in step 1 is soaked and washed with 1VB pure water for 30 minutes, and the washing liquid is discharged to the main system of online alkali extraction and stripping liquid for recycling; 3) Resin desorption: The oil-loaded resin washed in step 2 is dynamically desorbed using 95% ethanol in a bottom-in-top-out manner, with a desorption flow rate of 2VB / h at room temperature. No oil phase is produced when the outlet sample is desorbed, and the desorption liquid obtained by desorption is an organic phase ethanol mixture. The amount of desorption ethanol used is 3VB, and the desorption rate is 99.45%; 4) Desorption liquid treatment: The desorption liquid obtained in step 3 was directly recycled by doping with the blank organic phase of the online alkaline extraction at 1 / 80. After doping, the tungsten content of the loaded organic phase increased by 1.26% and the molybdenum content increased by 1.16% compared with the undoped organic phase; 5) Resin washing: After dynamic desorption in step 3, the resin is washed with pure water in the order of bottom-in and top-out. The pure water washing flow rate is 2BV / h and the pure water consumption is 4BV. After washing, the resin returns to the adsorption link in step 1. Example

[0045] The alkaline extraction stripping solution in this example comes from a stripping solution containing trace organic phase produced in the alkaline extraction section of a tungsten-molybdenum smelter in Henan Province using low-grade complex scheelite to produce ammonium paratungstate. Samples were taken for testing and found to contain 115.98 g / L tungsten, 11.73 g / L molybdenum, and 637 mg / L TOC.

[0046] 1) Resin adsorption and oil removal: Special modified macroporous adsorption resin is loaded into the ion exchange column, and the alkaline stripping solution containing trace organic phase is introduced in a top-in and bottom-out manner for dynamic adsorption and oil removal. The adsorption flow rate is 2VB / h at room temperature. When TOC>10mg / L in the outlet instantaneous sample alkaline stripping solution, the adsorption is stopped. At this time, the resin adsorbs the organic phase to the breakthrough adsorption amount, which is the oil-loaded resin. The resin organic phase breakthrough adsorption amount is 0.896g / ml, and the TOC removal rate is 98.83%. When the resin adsorbs the organic phase to the breakthrough adsorption amount, it is the oil-loaded resin. After oil removal, the alkaline stripping solution enters the subsequent evaporation and crystallization process; 2) Resin washing: The oil-carrying resin in step 1 is soaked and washed with 1VB pure water for 30 minutes, and the washing liquid is discharged to the main system of online alkali extraction and stripping liquid for recycling; 3) Resin desorption: The oil-loaded resin washed in step 2 was dynamically desorbed using 90% ethanol in a bottom-in-top-out manner, with a desorption flow rate of 1VB / h at room temperature. No oil phase was produced at the outlet sample, and the desorption liquid obtained by desorption was an organic phase ethanol mixture. The amount of desorption ethanol used was 3.5VB, and the desorption rate was 99.17%; 4) Desorption liquid treatment: The desorption liquid obtained in step 3 is directly recycled by doping with the blank organic phase of the online alkali extraction at 1 / 60. After doping, the tungsten content of the loaded organic phase increases by 0.38% and the molybdenum content increases by 0.29% compared with the undoped organic phase; 5) Resin washing: After dynamic desorption in step 3, the resin is washed with pure water in the order of bottom-in and top-out. The pure water washing flow rate is 2BV / h and the pure water consumption is 4BV. After washing, the resin returns to the adsorption link in step 1.

[0047] The present invention is suitable for high-salt solution with tungsten content of 110-130g / L and molybdenum content of 11-13g / L. The resin can maintain stable adsorption performance when adsorbing organic phase in high-salt solution. After multiple simulation cycle tests, it is verified that the service life of the resin meets the current industrial application cost requirements and can be used for industrial production. The macroporous adsorption resin has good adsorption and oil removal effect. The TOC in the alkali extraction stripping solution can be reduced from 550-650 mg / L of water inlet to less than 10 mg / L of water outlet. The penetration adsorption amount of the resin is greater than 0.85g / ml, and the TOC removal rate is more than 98.5%; the desorption of the macroporous adsorption resin is simple and energy-saving. The resin can be recycled after desorption and washing, and the resin structure and performance are stable. The organic phase ethanol mixture after desorption can be directly mixed and recycled in a certain proportion, and has a positive effect on the alkali extraction system. The entry of ethanol into the system is also conducive to the phase separation of the alkali extraction organic phase, further reducing the residual organic phase in the alkali extraction stripping solution. It can prevent the subsequent evaporation and crystallization section equipment from being difficult to clean due to the residual organic phase in the alkali extraction and stripping solution, and the subsequent ammonia solution section from producing insoluble oily slag, thereby reducing the difficulty of manual cleaning, improving the tungsten and molybdenum yields, and reducing the cost of treating insoluble oily slag.

Claims

1. A comprehensive recovery method for residual organic phase in alkali extraction stripping solution, characterized in that: The steps include: 1) Resin adsorption and oil removal: The macroporous adsorption resin is loaded into the ion exchange column, and the alkaline stripping solution containing trace organic phase is introduced in a top-in and bottom-out manner for dynamic adsorption and oil removal. Under certain temperature conditions, the adsorption flow rate is proportional to the resin volume. When the TOC in the outlet instantaneous alkaline stripping solution is >10mg / L, the adsorption is stopped. At this time, the macroporous adsorption resin adsorbs the organic phase to reach the breakthrough adsorption amount, and the alkaline stripping solution enters the subsequent evaporation and crystallization process; the macroporous adsorption resin that has adsorbed the organic phase to reach the breakthrough adsorption amount is called oil-carrying resin; 2) Resin washing: The oil-carrying resin in step 1 is washed by soaking in pure water, and the washing liquid is discharged to the main system of online alkali extraction and stripping liquid for recycling; 3) Resin desorption: The oil-loaded resin washed in step 2 is dynamically desorbed using ethanol in a bottom-in-top-out manner. Under certain temperature conditions, the desorption flow rate is proportional to the resin volume. The desorption is performed until no oil phase is produced at the outlet sample, and the obtained desorption liquid is an organic phase ethanol mixture; 4) Desorption liquid treatment: the desorption liquid obtained in step 3 is directly mixed into the online alkali extraction blank organic phase according to a certain proportion for recycling; 5) Resin washing: After dynamic desorption in step 3, the macroporous adsorption resin is washed with pure water in a bottom-in and top-out manner. After washing, the macroporous adsorption resin returns to the adsorption link in step 1.

2. The comprehensive recovery method of residual organic phase in an alkali extraction stripping solution according to claim 1, characterized in that: In the step 1, the adsorption temperature of the macroporous adsorption resin is 20-40° C., and the adsorption flow rate is 2-3 BV / h.

3. The comprehensive recovery method of residual organic phase in an alkali extraction stripping solution according to claim 2, characterized in that: In the step 1, the penetration adsorption capacity of the macroporous adsorption resin is greater than 0.85 g / ml, and the TOC removal rate is greater than 98.5%.

4. The comprehensive recovery method of residual organic phase in an alkali extraction stripping solution according to claim 1, characterized in that: In step 2, the amount of pure water used is 1VB, and the soaking time is 30 minutes.

5. The comprehensive recovery method of residual organic phase in an alkali extraction stripping solution according to claim 1, characterized in that: In the step 3, the ethanol concentration is greater than 90%, the ethanol is prepared from 99.7% analytical pure anhydrous ethanol, and the amount of ethanol used is 2-4VB.

6. The comprehensive recovery method of residual organic phase in an alkali extraction stripping solution according to claim 5, characterized in that: In the step 3, the desorption temperature of the oil-carrying resin during desorption is 20-40° C., the desorption flow rate is 1-2 BV / h, and the desorption rate is more than 99%.

7. The comprehensive recovery method of residual organic phase in an alkali extraction stripping solution according to claim 1, characterized in that: In the step 4, the mixing ratio of the desorption liquid and the alkali-extracted blank organic phase is less than 1 / 60; the saturated loaded tungsten and molybdenum content of the organic phase ethanol desorption mixture and the alkali-extracted blank organic phase after mixing is greater than the saturated loaded tungsten and molybdenum content of the blank organic phase.

8. The comprehensive recovery method of residual organic phase in an alkali extraction stripping solution according to claim 1, characterized in that: In step 5, the pure water washing flow rate is 2BV / h, and the pure water consumption is 4BV.

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