Extracting agent continuous saponification device and saponification method thereof

By designing a continuous saponification device for extractant and using technical means such as multi-tube feeding and steam heating, the existing problems of low saponification reaction efficiency and large waste of liquid and alkali are solved, and efficient saponification and low-cost production are achieved.

CN119793362APending Publication Date: 2025-04-11MCC RAMU NEW ENERGY TECH CO LTD
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Patent Information

Application Number
CN202411732449.7
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2024-11-29
Publication Date
2025-04-11

AI Technical Summary

Technical Problem

In the existing saponification process of extractive agents, the saponification reaction efficiency is low, resulting in waste of liquid and alkali and increase production costs.

Method used

A continuous saponification device for extractant is designed, including a saponification kettle and a saponification clarification tank. The liquid alkali and extractant are pumped into the saponification kettle by multiple feeding methods, and the reaction efficiency is improved through steam heating and stirring devices, and combined with the adjustment of the aqueous phase reflux pipeline, the utilization of liquid alkali is optimized.

Benefits of technology

It improves the efficiency of the saponification reaction of the extractant, reduces the consumption of liquid alkali, reduces production costs, and improves economic benefits.

✦ Generated by Eureka AI based on patent content.

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Abstract

The invention provides a continuous saponification device for an extracting agent. The continuous saponification device comprises a saponification kettle and a saponification clarifying tank, the upper part of the saponification kettle is communicated with the saponification clarification tank through an overflow pipeline; the bottom of the saponification kettle is communicated with the bottom of the saponification clarification tank through a water phase reflux pipeline; a stirring device is arranged in the bottom of the saponification kettle, and a plurality of extracting agent feeding pipes extending near the stirring device are arranged in the middle of the upper part of the saponification kettle; a plurality of liquid caustic soda feeding pipes extending to the vicinity of the stirring device are arranged at the upper part of the saponification kettle and around the extracting agent feeding pipe; the saponification kettle is of an external jacket type structure, the lower part of an interlayer space of the saponification kettle is communicated with a steam inlet, and the upper part of the interlayer space is communicated with a steam outlet; according to the continuous saponification device for the extraction agent and the saponification method of the continuous saponification device for the extraction agent, the saponification efficiency of the extraction agent is high, liquid caustic soda residues are low, and therefore consumption of the liquid caustic soda is correspondingly low, the production cost is low, and economic benefits are good.
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Description

Technical Field

[0001] The invention relates to the technical field of extractant saponification, and in particular to an extractant continuous saponification device and a saponification method thereof. Background Art

[0002] Nickel sulfate is a very important raw material in the lithium battery and electroplating industries. In the process of large-scale production of nickel sulfate, it is often necessary to use organic solvent extraction to purify nickel sulfate. Specifically, in its production, P204 is used for impurity removal, P507 for cobalt and magnesium extraction, and C272 for deep extraction, followed by washing, stripping, regeneration and other processes to remove impurities, separate nickel and cobalt, and finally achieve the purpose of purifying nickel sulfate.

[0003] The extraction line for purifying nickel sulfate usually consists of five parts: saponification, soap conversion, extraction, washing, and stripping. Among them, saponification, as the starting link of extraction production, mainly involves saponification reaction between the extractant and liquid alkali, so that the extractant obtains a post-soap organic phase with load capacity and converts the liquid alkali into a post-soap water phase. In the process of extractant saponification, theoretically, the water phase after the saponification reaction should be close to neutral due to the excess of acidic extractant. However, in the existing process, due to the limitations of the saponification stirring tank structure and the saponification process, the soap conversion efficiency is low, resulting in the residual unreacted liquid alkali in the water phase after the saponification reaction, thereby causing a waste of liquid alkali and increasing production costs.

[0004] Therefore, there is an urgent need for an extractant saponification device and an extractant saponification method having high extractant saponification efficiency and low liquid alkali consumption. Summary of the invention

[0005] The technical problem to be solved by the present invention is to provide an extractant saponification device and a saponification method thereof with high extractant saponification efficiency and low liquid alkali consumption.

[0006] In order to solve the above technical problems, the present invention provides an extractant continuous saponification device, comprising a saponification kettle and a saponification clarification tank;

[0007] The upper part of the saponification kettle is connected to the saponification clarification tank through an overflow pipe, and the bottom of the saponification kettle and the bottom of the saponification clarification tank are connected through a water phase reflux pipe;

[0008] A stirring device is arranged at the bottom of the saponification kettle, and a plurality of extractant feeding pipes extending into the vicinity of the stirring device are arranged at the middle position of the upper part of the saponification kettle;

[0009] A plurality of liquid alkali feed pipes extending into the vicinity of the stirring device are arranged around the extractant feed pipe at the upper part of the saponification kettle;

[0010] The saponification kettle is an external jacket structure, with the lower part of the interlayer space of the saponification kettle connected to the steam inlet and the upper part of the interlayer space connected to the steam outlet;

[0011] The upper part of the saponification clarification tank is provided with a post-soap organic outlet, and the bottom part is provided with a water phase outlet.

[0012] Furthermore, the steam inlet and the steam outlet are connected to a steam supply circulation device, and the water vapor provided by the steam supply circulation device enters the interlayer space of the saponification kettle from the steam inlet to heat the material in the saponification kettle, and then returns to the steam supply circulation device from the steam outlet.

[0013] Furthermore, the stirring device adopts a turbine stirring device, the rotating turbine of the stirring device is connected to the driving motor outside the saponification kettle through a rotating shaft, and the liquid alkali feed pipe and the extractant feed pipe extend into the rotating turbine attachment of the stirring device.

[0014] Furthermore, a valve with adjustable opening is provided on the water phase reflux pipeline.

[0015] Furthermore, the extractant feed pipe is connected to the extractant supply device through a first connecting pipe, and a first flow pump is arranged on the first connecting pipe connecting the extractant feed pipe and the extractant supply device; the liquid alkali feed pipe is connected to the liquid alkali supply device through a second connecting pipe, and a second flow pump is arranged on the second connecting pipe connecting the liquid alkali feed pipe and the liquid alkali supply device.

[0016] The present invention also provides a method for continuous saponification of an extractant, comprising the following steps:

[0017] The liquid caustic soda and the extractant are continuously pumped into the saponification kettle through the liquid caustic soda feeding pipe and the extractant feeding pipe respectively;

[0018] The liquid alkali and the extractant are mixed under the action of a stirring device and heated by steam to cause saponification reaction;

[0019] The saponification mixed liquid produced by the saponification reaction continuously enters the saponification clarification tank from the overflow pipe;

[0020] The saponified mixed liquid entering the saponification clarification tank is phase-separated in the saponification clarification tank;

[0021] The post-soap organic phase produced by phase separation overflows from the post-soap organic outlet;

[0022] When the residual caustic soda does not meet the standard, the water phase generated by the phase separation is returned to the saponification kettle through the water phase reflux pipe to continue to participate in the saponification reaction;

[0023] The water phase produced by phase separation is discharged from the water phase outlet after the residual liquid alkali reaches the standard.

[0024] Furthermore, the liquid alkali is a sodium hydroxide solution with a mass percentage concentration of 30-35%, and the extractant is P204, P507 or C272.

[0025] Furthermore, the flow rate of the extractant pumped into the saponification kettle is controlled at 40-50m 3 / h, the flow rate of liquid alkali pumped into the saponification kettle is controlled at 2-3m 3 / h, and the volume ratio of the extractant to liquid alkali is controlled to be 18:1-22:1.

[0026] Furthermore, when the liquid alkali and the extractant undergo saponification reaction in the saponification kettle, the temperature of the saponification kettle is controlled at 50-65° C. by adjusting the steam flow rate entering the interlayer space of the saponification kettle.

[0027] Furthermore, the stirring speed of the stirring device is controlled at 50-100 r / min.

[0028] The present invention provides an extractant continuous saponification device and a saponification method thereof. Liquid alkali and an extractant are pumped into a saponification kettle by a multi-tube feeding method, and the liquid alkali and the extractant are introduced into an area near a stirring device at the bottom of the saponification kettle. This can not only effectively increase the dispersion speed of the material and improve the dispersibility of the material, but also enable the liquid alkali and the extractant to contact more fully, which is beneficial to the saponification reaction efficiency, can enable the liquid alkali to react more fully, can effectively reduce the consumption of liquid alkali, save costs, and improve economic benefits.

[0029] In addition, the present invention provides a continuous saponification device for an extractant and a saponification method thereof, wherein a jacket structure is arranged outside a saponification kettle, steam is introduced into the interlayer space of the saponification kettle in a bottom-in-top-out manner to heat the saponification kettle, and the heating temperature is controlled by adjusting the flow rate of the incoming steam, thereby stabilizing the heating temperature in the saponification kettle, making the saponification reaction more stable, and improving the efficiency of the saponification reaction of the extractant.

[0030] At the same time, the present invention provides an extractant continuous saponification device and a saponification method thereof. The bottom of the saponification kettle and the bottom of the saponification clarification tank are connected by a water phase reflux pipe. According to the residual liquid alkali in the water phase produced by phase separation, part of the water phase can be returned to the saponification kettle for further reaction by adjusting the valve opening on the reflux pipe, thereby reducing the residual concentration of liquid alkali in the water phase and reducing the loss of liquid alkali.

[0031] In addition, the present invention provides a continuous saponification device for an extractant, wherein the upper part of a saponification kettle is connected to a saponification clarification tank through an overflow pipe. When the extractant is saponified, liquid alkali and the extractant can be continuously pumped into the saponification kettle through a feed pipe. A saponified mixed liquid generated after the liquid alkali and the extractant undergo saponification reaction in the saponification kettle can continuously enter the saponification clarification tank from the overflow pipe for phase separation. A post-soap organic phase generated by the phase separation can continuously overflow from a post-soap organic outlet. When the residual liquid alkali does not meet the standard, the water phase generated by the phase separation can be returned to the saponification kettle from the water phase reflux pipe to continue to participate in the saponification reaction. If the residual liquid alkali in the water phase generated by the phase separation meets the standard, it can be discharged from the water phase outlet, thereby realizing continuous saponification of the extractant and greatly improving the saponification efficiency. BRIEF DESCRIPTION OF THE DRAWINGS

[0032] Figure 1 A schematic structural diagram of a continuous saponification device for an extractant provided in an embodiment of the present invention.

[0033] Reference numerals:

[0034] 1-liquid alkali feed pipe, 2-extractant feed pipe, 3-stirring device, 4-steam inlet, 5-steam outlet, 6-saponification kettle, 7-soap organic outlet, 8-water phase outlet, 9-saponification clarification tank, 10-water phase reflux pipe, 11-overflow pipe, 12-valve. DETAILED DESCRIPTION

[0035] See also Figure 1 The present invention provides a continuous saponification device for extracting agent, comprising a saponification kettle 6 and a saponification clarification tank 9. The upper part of the saponification kettle 6 is connected to the saponification clarification tank 9 through an overflow pipe 11, and the bottom of the saponification kettle 6 and the bottom of the saponification clarification tank 9 are connected through an aqueous phase reflux pipe 10.

[0036] In addition, a stirring device 3 is arranged at the bottom of the saponification kettle 6, and a plurality of extractant feed pipes 2 extending into the vicinity of the stirring device 3 are arranged at the middle position of the upper part of the saponification kettle 6. A plurality of liquid caustic soda feed pipes 1 extending into the vicinity of the stirring device 3 are arranged around the extractant feed pipe 2 at the upper part of the saponification kettle 6.

[0037] The extractant feed pipe 2 is connected to the extractant supply device through a first connecting pipe, and the extract in the extractant supply device can enter the saponification kettle 6 through multiple extractant feed pipes 2. The liquid alkali feed pipe 1 is connected to the liquid alkali supply device through a second connecting pipe, and the liquid alkali in the liquid alkali supply device can enter the saponification kettle 6 through multiple liquid alkali feed pipes 1.

[0038] As a specific embodiment of the present invention, two liquid alkali feed pipes 1 and two extractant feed pipes 2 are respectively arranged on the saponification kettle 6.

[0039] In addition, a first flow pump is provided on the first connecting pipe connecting the extractant feed pipe 2 and the extractant supply device, and the flow rate of the extractant entering the saponification kettle 6 can be controlled by the first flow pump. Similarly, a second flow pump is provided on the second connecting pipe connecting the liquid caustic soda feed pipe 1 and the liquid caustic soda supply device, and the flow rate of the liquid caustic soda entering the saponification kettle 6 can also be controlled by the second flow pump.

[0040] As a specific embodiment of the present invention, the stirring device 3 adopts a turbine stirring device, the rotating turbine of the stirring device 3 is connected to the driving motor outside the saponification kettle 6 through a rotating shaft, and the liquid alkali feed pipe 1 and the extractant feed pipe 2 extend into the rotating turbine attachment of the stirring device 3.

[0041] The present invention provides a continuous saponification device for an extractant and a saponification method thereof. Liquid alkali and an extractant are pumped into a saponification kettle 6 by a multi-tube feeding method, and the liquid alkali and the extractant are introduced into the vicinity of a stirring device 3 at the bottom of the saponification kettle 6 by a flow pump. This can not only effectively improve the dispersion speed of the material, but also improve the dispersibility of the material, and make the liquid alkali and the extractant contact more fully, which is beneficial to the efficiency of the saponification reaction, and can make the saponification reaction of the liquid alkali and the extractant more complete, and can effectively reduce the consumption of liquid alkali, save costs, and improve economic benefits.

[0042] The saponification kettle 6 is an external jacket structure, the lower part of the interlayer space of the saponification kettle 6 is connected to the steam inlet 4, and the upper part of the interlayer space is connected to the steam outlet 5.

[0043] The steam inlet 4 and the steam outlet 5 are connected to a steam supply circulation device. The water vapor provided by the steam supply circulation device enters the interlayer space of the saponification kettle 6 from the steam inlet 4 to heat the material in the saponification kettle 6, and then returns to the steam supply circulation device from the steam outlet 5.

[0044] The present invention provides a continuous saponification device for extractants, in which a jacket structure is arranged outside a saponification kettle, and steam is introduced into the interlayer space of the saponification kettle in a bottom-in-top-out manner to heat the saponification kettle, so that the material at the bottom of the saponification kettle can be heated more fully and saponification reaction can occur more easily. In addition, the present invention can also control the heating temperature by adjusting the flow rate of the steam entering, so that the heating temperature in the saponification kettle can be stabilized, the saponification reaction can be more stable, and the efficiency of the saponification reaction of the extractant can be easily improved.

[0045] The upper part of the saponification clarification tank 9 is provided with a post-soap organic outlet 7, and the bottom part of the saponification clarification tank 9 is provided with a water phase outlet 8.

[0046] When the extractant is saponified, the liquid alkali and the extractant are continuously pumped into the bottom of the saponification kettle 6 through the liquid alkali feed pipe 1 and the extractant feed pipe 2 respectively. Under the stirring action of the stirring device 3, the liquid alkali and the extractant are fully mixed and contacted, and then a saponification reaction occurs in the saponification kettle 6. The generated saponified mixed liquid can continuously enter the saponification clarification tank from the overflow pipe for phase separation. The post-soap organic phase generated by the phase separation can continuously overflow from the post-soap organic outlet 7. When the liquid alkali residue of the water phase generated by the phase separation does not meet the standard, it can be returned to the saponification kettle 6 from the water phase reflux pipe 10 to continue to participate in the saponification reaction. If the liquid alkali residue of the water phase generated by the phase separation meets the standard, it can be discharged from the water phase outlet 8, thereby realizing the continuous saponification of the extractant and greatly improving the saponification efficiency.

[0047] In addition, a valve 12 with an adjustable opening is provided on the water phase reflux pipe 10. When the residual liquid alkali contained in the water phase produced by phase separation in the saponification clarification tank 9 does not meet the standard, part of the water phase can be returned to the saponification kettle to continue the reaction by adjusting the opening of the valve 12 on the reflux pipe 10 according to the residual liquid alkali in the water phase produced by phase separation, thereby reducing the residual concentration of liquid alkali in the water phase and reducing the loss of liquid alkali.

[0048] The present invention also provides a method for continuous saponification of an extractant, comprising the following steps:

[0049] Step 1) Liquid caustic soda and extractant are continuously pumped into the saponification kettle 6 through the liquid caustic soda feed pipe 1 and the extractant feed pipe 2 respectively.

[0050] The liquid alkali is a sodium hydroxide solution with a mass percentage concentration of 30-35%, and the extractant is P204, P507 or C272.

[0051] In order to control the saponification rate and improve the extraction capacity of the extractant after saponification, the flow rate of the extractant entering the saponification kettle 6 is controlled to be 40-50m / s by a first flow pump arranged on the first connecting pipe between the extractant feed pipe 2 and the extractant supply device. 3 / h, and at the same time, the flow rate of the liquid caustic soda entering the saponification kettle 6 is controlled at 2-3m / h by a second flow pump arranged on a second connecting pipe between the liquid caustic soda feeding pipe 1 and the liquid caustic soda supply device. 3 / h.

[0052] Furthermore, in order to facilitate the saponification reaction of the extractant and the liquid alkali, the volume ratio of the extractant to the liquid alkali is controlled to be 18:1-22:1.

[0053] Step 2) The liquid alkali and the extractant pumped into the saponification kettle 6 are fully mixed under the stirring action of the stirring device 3.

[0054] As a specific implementation of the present invention, in order to achieve the best stirring effect, the stirring speed of the stirring device 3 is controlled at 50-100 r / min.

[0055] The stirring device 3 of the saponification kettle 6 is driven by a turbine stirring, which can mix the liquid alkali and the extractant on the one hand, and can also form a negative pressure at the bottom of the saponification kettle 6 during the stirring process. The bottom of the saponification kettle 6 is connected to the bottom of the saponification clarification tank 9 through a water phase reflux pipe 10. By adjusting the opening of a valve 12 on the water phase reflux pipe 10, the height of the water phase in the saponification clarification tank 9 can be controlled to achieve a full reaction of the liquid alkali and the organic phase.

[0056] The outer part of the saponification kettle 6 is provided with a jacket structure, the lower part of the interlayer space of the saponification kettle 6 is connected to the steam inlet 4, and the upper part of the interlayer space is connected to the steam outlet 5. The water vapor provided by the steam supply circulation device enters the interlayer space of the saponification kettle 6 from the steam inlet 4, and can heat the material in the saponification kettle 6, and then the steam returns to the steam supply circulation device from the steam outlet 5. The steam is introduced into the interlayer space of the saponification kettle in a bottom-in-top-out manner to heat the saponification kettle, so that the material at the bottom of the saponification kettle can be heated more fully, and the saponification reaction is more likely to occur. In addition, by adjusting the flow rate of the incoming steam to control the heating temperature, the heating temperature in the saponification kettle can be stabilized, the saponification reaction can be more stable, and the efficiency of the saponification reaction of the extractant can be easily improved.

[0057] As a specific embodiment of the present invention, the temperature in the saponification kettle 6 is controlled at 50-65° C. by adjusting the steam flow rate entering the interlayer space of the saponification kettle 6 .

[0058] The fully mixed liquid alkali and extractant undergo saponification reaction at a constant temperature of 50-65°C to obtain a saponified mixed liquid formed by the saponified organic phase and the water phase. The reaction is as follows:

[0059] HA+NaOH=NaA+H2O.

[0060] Wherein HA is P204, P507 or C272, the organic phase after saponification is NaA, and the aqueous phase is mainly H2O. Due to the incomplete reaction of the two in the saponification kettle, some NaOH is likely to remain in the aqueous phase.

[0061] Step 3) The saponification mixed liquid produced by the saponification reaction continuously overflows from the overflow pipe 11 into the saponification clarification tank 9.

[0062] Step 4) The saponified mixed liquid entering the saponification clarification tank 9 is phase-separated in the saponification clarification tank 9. Since the density of the saponified organic phase NaA is lower than that of the water phase, the phase separation is achieved under the action of the baffle in the saponification clarification tank 9. The post-soap organic phase generated by the phase separation overflows from the post-soap organic outlet 7.

[0063] When the residual caustic soda in the water phase produced by the phase separation does not meet the standard, the water phase can be returned to the saponification kettle 6 from the water phase reflux pipe 10 to continue to participate in the saponification reaction. In addition, according to the residual caustic soda in the water phase, the opening of the valve 12 on the water phase reflux pipe 10 can be adjusted to allow the liquid caustic soda that has not fully reacted in the water phase to return to the saponification kettle 6 to continue the reaction. When the residual caustic soda in the water phase produced by the phase separation meets the standard, the water phase is directly discharged from the water phase outlet 8.

[0064] The following is a specific description of the method for continuous saponification of an extractant provided by the present invention through examples.

[0065] Example 1

[0066] 32% sodium hydroxide solution was mixed with 2.5m 3 / h flow rate, P204 extractant at 45m 3 / h flow rate is continuously pumped into the saponification kettle 6 from the liquid alkali feed pipe 1 and the extractant feed pipe 2 respectively, the stirring speed of the stirring device 3 is 65r / min, and the temperature in the saponification kettle 6 is stably controlled at 55°C by adjusting the steam flow entering the interlayer of the saponification kettle 6. The water phase reflux valve 10 is in a closed state. The liquid alkali entering the saponification kettle 6 and the extractant P204 continuously undergo saponification reaction. The saponified mixed liquid after the reaction continuously enters the saponification clarification tank 9 from the overflow pipe 11, and is phase-separated after the saponification clarification tank 9. The post-soap organic phase produced by the phase separation overflows from the post-soap organic outlet 7. The liquid alkali residue in the water phase produced by the phase separation meets the standard and is directly discharged from the water phase outlet 8.

[0067] After testing, the saponification rate of the saponified organic phase of this embodiment was measured to be 56.4%, and the residual concentration of liquid alkali in the water phase was 0.79 mol / l. This shows that the extractant of the embodiment of the present invention has a high saponification efficiency and low residual liquid alkali, so the consumption of liquid alkali is correspondingly low, so the production cost is low and the economic benefit is good.

[0068] Example 2

[0069] 30% sodium hydroxide solution was added at 3m 3 / h flow rate, P507 extractant at 40m 3 / h flow rate is continuously pumped into the saponification kettle 6 from the liquid alkali feed pipe 1 and the extractant feed pipe 2 respectively, the stirring speed of the stirring device 3 is 50r / min, and the temperature in the saponification kettle 6 is stably controlled at 50°C by adjusting the steam flow entering the interlayer of the saponification kettle 6. The water phase reflux valve 10 is in a closed state. The liquid alkali entering the saponification kettle 6 and the extractant P507 continuously undergo saponification reaction. The saponified mixed liquid after the reaction continuously enters the saponification clarification tank 9 from the overflow pipe 11, and is phase-separated after the saponification clarification tank 9. The post-soap organic phase produced by the phase separation overflows from the post-soap organic outlet 7. The liquid alkali residue in the water phase produced by the phase separation meets the standard and is directly discharged from the water phase outlet 8.

[0070] After testing, the saponification rate of the saponified organic phase of this embodiment was measured to be 57.1%, and the residual concentration of liquid alkali in the water phase was 0.21 mol / l. This shows that the extractant of the embodiment of the present invention has a high saponification efficiency and low residual liquid alkali, so the consumption of liquid alkali is correspondingly low, so the production cost is low and the economic benefit is good.

[0071] Example 3

[0072] 35% sodium hydroxide solution was mixed with 2m 3 / h flow rate, C272 extractant at 50m 3 / h flow rate is continuously pumped into the saponification kettle 6 from the liquid alkali feed pipe 1 and the extractant feed pipe 2 respectively, the stirring speed of the stirring device 3 is 10r / min, and the temperature in the saponification kettle 6 is stably controlled at 65°C by adjusting the steam flow entering the interlayer of the saponification kettle 6. The water phase reflux valve 10 is in a closed state. The liquid alkali entering the saponification kettle 6 and the extractant C272 continuously undergo saponification reaction. The saponified mixed liquid after the reaction continuously enters the saponification clarification tank 9 from the overflow pipe 11, and is phase-separated through the saponification clarification tank 9. The post-soap organic phase produced by the phase separation overflows from the post-soap organic outlet 7. The liquid alkali residue in the water phase produced by the phase separation meets the standard and is directly discharged from the water phase outlet 8.

[0073] After testing, the saponification rate of the saponified organic phase of this embodiment was measured to be 56.9%, and the residual concentration of liquid alkali in the water phase was 0.47 mol / l. This shows that the extractant of the embodiment of the present invention has a high saponification efficiency and low residual liquid alkali, so the consumption of liquid alkali is correspondingly low, so the production cost is low and the economic benefit is good.

[0074] Finally, it should be noted that the above specific implementation methods are only used to illustrate the technical solution of the present invention rather than to limit it. Although the present invention has been described in detail with reference to examples, those skilled in the art should understand that the technical solution of the present invention can be modified or replaced by equivalents without departing from the spirit and scope of the technical solution of the present invention, which should be included in the scope of the claims of the present invention.

Claims

1. A continuous saponification device for an extractant, characterized in that: It comprises a saponification kettle (6) and a saponification clarification tank (9); The upper part of the saponification kettle (6) is connected to the saponification clarification tank (9) through an overflow pipe (11), and the bottom of the saponification kettle (6) and the bottom of the saponification clarification tank (9) are connected through a water phase reflux pipe (10); A stirring device (3) is arranged at the bottom of the saponification kettle (6), and a plurality of extractant feeding pipes (2) extending into the vicinity of the stirring device (3) are arranged at the middle position of the upper part of the saponification kettle (6); A plurality of liquid alkali feed pipes (1) extending into the vicinity of the stirring device (3) are arranged around the extractant feed pipe (2) at the upper part of the saponification kettle (6); The saponification kettle (6) is an external jacket structure, the lower part of the interlayer space of the saponification kettle (6) is connected to the steam inlet (4), and the upper part of the interlayer space is connected to the steam outlet (5); The saponification clarification tank (9) is provided with a post-soap organic outlet (7) at the top and a water phase outlet (8) at the bottom.

2. The continuous saponification device for extracting agent according to claim 1, characterized in that: The steam inlet (4) and the steam outlet (5) are connected to a steam supply circulation device. The water vapor provided by the steam supply circulation device enters the interlayer space of the saponification kettle (6) from the steam inlet (4) to heat the material in the saponification kettle (6), and then returns to the steam supply circulation device from the steam outlet (5).

3. The continuous saponification device for extracting agent according to claim 1, characterized in that: The stirring device (3) is a turbine stirring device, and the rotating turbine of the stirring device (3) is connected to the driving motor outside the saponification kettle (6) through a rotating shaft, and the liquid alkali feed pipe (1) and the extractant feed pipe (2) extend into the rotating turbine attachment of the stirring device (3).

4. The continuous saponification device for extracting agent according to claim 1, characterized in that: The water phase reflux pipeline (10) is provided with a valve (12) with an adjustable opening.

5. The continuous saponification device for extractant according to claim 1, characterized in that: The extractant feed pipe (2) is connected to the extractant supply device via a first connecting pipe, and a first flow pump is arranged on the first connecting pipe connecting the extractant feed pipe (2) and the extractant supply device; the liquid alkali feed pipe (1) is connected to the liquid alkali supply device via a second connecting pipe, and a second flow pump is arranged on the second connecting pipe connecting the liquid alkali feed pipe (1) and the liquid alkali supply device.

6. A method for continuous saponification of an extractant, characterized in that: The steps include: The liquid caustic soda and the extractant are continuously pumped into the saponification kettle (6) through the liquid caustic soda feed pipe (1) and the extractant feed pipe (2) respectively; The liquid alkali and the extractant are mixed under the action of a stirring device (3) and heated by steam to cause a saponification reaction; The saponification mixed liquid produced by the saponification reaction continuously enters the saponification clarification tank (9) from the overflow pipe (11); The saponified mixed liquid entering the saponification clarification tank (9) undergoes phase separation in the saponification clarification tank (9); The post-soap organic phase produced by phase separation overflows from the post-soap organic outlet (7); When the residual caustic soda does not meet the standard, the water phase generated by the phase separation is returned to the saponification kettle (6) through the water phase reflux pipe (10) to continue to participate in the saponification reaction; The water phase produced by phase separation is discharged from the water phase outlet (8) after the residual liquid alkali reaches the standard.

7. The method for continuous saponification of an extractant according to claim 6, characterized in that: The liquid alkali is a sodium hydroxide solution with a mass percentage concentration of 30-35%, and the extractant is P204, P507 or C272.

8. The method for continuous saponification of an extractant according to claim 7, characterized in that: The flow rate of the extractant pumped into the saponification kettle (6) is controlled at 40-50m 3 / h, the flow rate of the liquid alkali pumped into the saponification kettle (6) is controlled at 2-3m 3 / h, and the volume ratio of the extractant to liquid alkali is controlled to be 18:1-22:

1.

9. The method for continuous saponification of an extractant according to claim 6, characterized in that: When the liquid alkali and the extractant undergo saponification reaction in the saponification kettle (6), the temperature of the saponification kettle (6) is controlled at 50-65°C by adjusting the flow rate of steam entering the interlayer space of the saponification kettle.

10. The method for continuous saponification of an extractant according to claim 6, characterized in that: The stirring speed of the stirring device (3) is controlled at 50-100 r / min.

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