Crude dimethyl sulfoxide phosphate radical removal system and process method thereof

Abstract

The invention discloses a crude dimethyl sulfoxide phosphate radical removal system and a process method thereof, and belongs to the technical field of chemical engineering. The system comprises an adsorption unit, a feeding system and a discharging system, the adsorption unit comprises a T-01A adsorption tank, a T-01B adsorption tank and a T-01C adsorption tank; the feeding system comprises a first feeding pipe, a second feeding pipe and a third feeding pipe; the discharging system comprises a first discharging pipe, a second discharging pipe and a third discharging pipe; the system is further provided with a regenerant supply unit, the regenerant supply unit comprises a regenerant buffer tank, the regenerant buffer tank is connected with a feeding pump through a regenerant discharging pipe, and the feeding pump is connected with the discharging pipe of each adsorption tank through an independent pipeline. A'dual-purpose and one-regeneration 'operation mode is adopted, the equipment utilization rate and the production efficiency are improved, and the large-scale industrial continuous production requirement is met; the problems that a traditional single adsorption column or double adsorption columns are discontinuous in operation, incomplete in regeneration and the like are solved.

Description

Technical Field

[0001] This invention belongs to the field of chemical technology, specifically relating to a crude dimethyl sulfoxide dephosphate system and its process. Background Technology

[0002] Crude dimethyl sulfoxide (DMSO) is an important highly polar aprotic solvent and organic synthesis intermediate, widely used in pharmaceuticals, pesticides, electronic chemicals, polymerization reactions, and fine chemicals. Its purity directly affects the performance of end-use applications, especially in high-end fields such as semiconductor cleaning and pharmaceutical synthesis, where extremely stringent requirements are placed on impurity content (such as metal ions, total organic carbon, and phosphate).

[0003] In actual production processes, a certain amount of phosphate ions (PO4) often remain in crude DMSO. 3- H2PO4 - These inorganic anions (such as phosphate ions) not only possess strong coordination abilities but can also act as alkaline catalysts to promote the thermal decomposition of DMSO, leading to a darker product color, decreased stability, and the introduction of byproducts, severely impacting its storage performance and compatibility with subsequent processes. Furthermore, the presence of phosphate ions can interfere with certain catalytic reaction systems, reducing reaction selectivity and yield, thus limiting the application of DMSO in high-value-added fields.

[0004] Currently, commonly used phosphorus removal methods in industry mainly include precipitation, extraction, and single fixed-bed adsorption. Among them, adsorption is widely used due to its simplicity and high selectivity. However, existing technologies mostly rely on a single adsorption column for intermittent treatment, which has obvious limitations: when the adsorption resin is close to saturation, it must be shut down for replacement or regeneration, leading to production interruptions and low efficiency; at the same time, a single adsorption unit is difficult to achieve deep purification and is prone to "breakthrough," affecting the stability of the effluent water quality.

[0005] Therefore, developing an integrated phosphorus removal system that can achieve continuous operation, efficient removal of phosphate ions, and regenerable resin will not only help improve the purification level of crude DMSO and ensure product quality stability, but also significantly improve production continuity and operational economy, which is of great significance for promoting DMSO process technology. Summary of the Invention

[0006] In view of this, the present invention provides a crude dimethyl sulfoxide dephosphate system and its process method. The present invention adopts a "two-use-one-regeneration" operation mode (i.e., two adsorption tanks are connected in series for adsorption, and one adsorption tank is used for regeneration), which improves equipment utilization and production efficiency and meets the needs of large-scale industrial continuous production; it solves the problems of discontinuous operation and incomplete regeneration of traditional single adsorption column or dual adsorption column.

[0007] To achieve the above objectives, the present invention provides the following technical solution:

[0008] This invention provides a crude dimethyl sulfoxide dephosphaterization system, comprising an adsorption unit, a feeding system, and a discharging system;

[0009] The adsorption unit includes a T-01A adsorption tank, a T-01B adsorption tank, and a T-01C adsorption tank, all three of which are filled with phosphorus removal resin for adsorbing phosphate ions.

[0010] The feeding system includes a first feed pipe, a second feed pipe, and a third feed pipe; the first feed pipe is connected to the bottom of the T-01A adsorption tank, the second feed pipe is connected to the bottom of the T-01B adsorption tank, and the third feed pipe is connected to the bottom of the T-01C adsorption tank; the first feed pipe, the second feed pipe, and the third feed pipe are all connected to the main feed pipe.

[0011] The discharge system includes a first discharge pipe, a second discharge pipe, and a third discharge pipe; the first discharge pipe is connected to the top of the T-01A adsorption tank, the second discharge pipe is connected to the top of the T-01B adsorption tank, and the third discharge pipe is connected to the top of the T-01C adsorption tank; the first discharge pipe, the second discharge pipe, and the third discharge pipe are all connected to the main discharge pipe.

[0012] Preferably, the T-01A adsorption tank is connected to the T-01B adsorption tank via a first discharge branch pipe, one end of which is connected to a first discharge pipe and the other end to a second inlet pipe; the T-01B adsorption tank is connected to the T-01C adsorption tank via a second discharge branch pipe, one end of which is connected to a second discharge pipe and the other end to a third inlet pipe; the T-01C adsorption tank is connected to the T-01A adsorption tank via a third discharge branch pipe, one end of which is connected to a third discharge pipe and the other end to a first inlet pipe.

[0013] Preferably, the first feed pipe, the second feed pipe, and the third feed pipe are respectively provided with a first feed pipe switch valve, a second feed pipe switch valve, and a third feed pipe switch valve; the first discharge pipe, the second discharge pipe, and the third discharge pipe are respectively provided with a first discharge pipe switch valve, a second discharge pipe switch valve, and a third discharge pipe switch valve; the first discharge branch pipe, the second discharge branch pipe, and the third discharge branch pipe are respectively provided with a first discharge branch pipe switch valve, a second discharge branch pipe switch valve, and a third discharge branch pipe switch valve.

[0014] Preferably, the system is further configured with a regenerant supply unit, which includes a regenerant buffer tank. One side of the regenerant buffer tank is connected to an alkali inlet pipe and a first inlet pipe. The alkali inlet pipe is equipped with an alkali inlet pipe switch valve, and the first inlet pipe is equipped with an inlet pipe switch valve. The other side of the regenerant buffer tank is connected to a feeding pump through a regenerant discharge pipe. The feeding pump is then connected to the discharge pipe of each adsorption tank (T-01A adsorption tank, T-01B adsorption tank, and T-01C adsorption tank) through independent pipes, and each adsorption tank has a corresponding independent pipe equipped with a switch valve.

[0015] Preferably, the discharge pipes of the T-01A adsorption tank, T-01B adsorption tank and T-01C adsorption tank are also connected to a nitrogen inlet pipe and a second liquid inlet pipe, and both the nitrogen inlet pipe and the second liquid inlet pipe are equipped with a switch valve.

[0016] Preferably, the feed pipes of the T-01A adsorption tank, T-01B adsorption tank, and T-01C adsorption tank are all connected to a wastewater discharge pipeline and a crude dimethyl sulfoxide discharge inlet pipeline; the wastewater discharge pipeline is connected to a waste liquid collection tank, and the crude dimethyl sulfoxide discharge inlet pipeline is connected to a raw material tank.

[0017] This invention also discloses a process for dephosphaterosis of crude dimethyl sulfoxide using the system described above, comprising the following steps:

[0018] S1. Initial adsorption stage:

[0019] Open the first feed pipe valve, the first discharge branch pipe valve, and the second discharge pipe valve, and close the relevant valves of the other adsorption tanks to form a series circuit between adsorption tanks T-01A and T-01B. Feed crude dimethyl sulfoxide (DMSO) material pressurized to 0.4–0.6 MPa into adsorption tank T-01A via the main feed pipe and the first feed pipe. After treatment with the anion exchange resin in adsorption tank T-01A, the material flows into adsorption tank T-01B via the first discharge branch pipe. T-01A serves as the first-stage adsorption tank to remove most of the phosphate ions from the material, while T-01B serves as the second-stage adsorption tank to further remove residual phosphate ions. After adsorption treatment, the material flows into the main discharge pipe via the second discharge pipe for output.

[0020] S2. Operation Switching and Regeneration Startup:

[0021] After the system has been running continuously for a period of time, when the anion exchange resin in the T-01A adsorption tank is close to saturation, the first feed pipe valve, the first discharge branch pipe valve, and the second discharge pipe valve are closed; the second feed pipe valve, the second discharge branch pipe valve, and the third discharge pipe valve are opened, switching to the series operation of the T-01B and T-01C adsorption tanks, entering a new adsorption stage; at this time, T-01B acts as the first-stage adsorption tank, and T-01C acts as the second-stage adsorption tank; simultaneously, the T-01A adsorption tank stops feeding and enters the regeneration stage.

[0022] S3. Switching and Regeneration Cycle:

[0023] After the system continues to run for a period of time, when the anion exchange resin in the T-01B adsorption tank is close to saturation, the second feed pipe switch valve, the second discharge branch pipe switch valve, and the third discharge pipe switch valve are closed; the third feed pipe switch valve, the third discharge branch pipe switch valve, and the first discharge pipe switch valve are opened, switching to the T-01C and T-01A adsorption tanks to operate in series, with T-01C as the first-stage adsorption tank and T-01A as the second-stage adsorption tank; at the same time, the T-01B adsorption tank stops feeding and enters the regeneration stage.

[0024] S4. Switching and regeneration cycle again:

[0025] After the system continues to run for a period of time, when the anion exchange resin in the T-01C adsorption tank is close to saturation, the third feed pipe switch valve, the third discharge branch pipe switch valve, and the first discharge pipe switch valve are closed; the first feed pipe switch valve, the first discharge branch pipe switch valve, and the second discharge pipe switch valve are opened, and the system switches back to the series operation of the T-01A and T-01B adsorption tanks, with T-01A acting as the first-stage adsorption tank and T-01B acting as the second-stage adsorption tank; at the same time, the T-01C adsorption tank 3 stops feeding and enters the regeneration stage.

[0026] S5. Cyclic Operation Mode:

[0027] The above switching process is repeated in sequence, forming a cyclical operation mode of three tanks rotating, two for use and one for regeneration, to ensure continuous and stable operation of the system; after each switch, two adsorption tanks are always in series adsorption state, while the other adsorption tank enters the regeneration process.

[0028] The present invention also discloses the following steps in the regeneration stage of the above-described crude dimethyl sulfoxide phosphate removal process:

[0029] S11. When any adsorption tank (T-01A, T-01B or T-01C) completes adsorption operation and enters the regeneration stage, nitrogen is first used to replace the crude dimethyl sulfoxide raw material remaining in the resin column of the adsorption tank. The material remaining in the resin column is then pushed back to the raw material tank through the "crude dimethyl sulfoxide inlet pipeline" to realize the recycling of the material.

[0030] S12. After the gas top is completed, the alkaline regeneration solution prepared in the regenerator buffer tank is introduced into the adsorption tank from top to bottom. The alkaline solution reacts with the phosphate ions on the anion exchange resin to achieve the desorption of phosphate ions. The waste liquid after the reaction is discharged to the waste liquid collection tank through the "wastewater pipeline".

[0031] S13. After the waste alkaline solution is drained, the resin column is rinsed with pure water or deionized water until the pH value of the effluent drops to 6.5-7.5 and the conductivity tends to stabilize, indicating that the resin has been cleaned. After regeneration, the adsorption tank is ready to be put into the next adsorption cycle.

[0032] Preferably, the purity of the nitrogen gas is ≥99.5%.

[0033] Preferably, the alkaline regeneration solution is a sodium hydroxide aqueous solution with a mass concentration of 2% to 10%, and the flow rate of the alkaline solution is 1 to 3 BV / h (through volume / hour).

[0034] Compared with the prior art, the present invention has the following beneficial effects:

[0035] (1) This invention achieves continuous and stable operation and improves production efficiency by rotating three adsorption tanks, T-01A, T-01B, and T-01C, using a "two-use-one-regeneration" operating mode (i.e., two adsorption tanks are connected in series for adsorption, and one adsorption tank is used for regeneration). Furthermore, each adsorption stage adopts a two-stage series design (such as T-01A+T-01B, T-01B+T-01C, T-01C+T-01A). The first-stage adsorption tank mainly removes most of the phosphate ions, while the second stage performs deep purification. The multi-stage series adsorption results in high removal efficiency, meeting the requirements for phosphate removal from crude dimethyl sulfoxide.

[0036] (2) The regeneration process of this invention adopts a three-step method: "nitrogen gas top + alkaline elution + pure water rinsing".

[0037] (i) The crude dimethyl sulfoxide raw material remaining in the adsorption tank is replaced by high-purity nitrogen (≥99.5%), and the remaining crude DMSO raw material is pushed back to the raw material tank through the "crude dimethyl sulfoxide inlet pipeline", so as to achieve complete recovery of organic media, avoid waste of crude DMSO, effectively prevent organic residue from interfering with the subsequent alkaline regeneration process, and also realize material recycling.

[0038] (ii) An alkaline regenerant solution (2%–10% NaOH aqueous solution) prepared in a regenerant buffer tank is introduced into the adsorption tank from top to bottom, allowing the alkaline solution to react with the phosphate ions (H2PO4) on the anion exchange resin. - HPO4 2-(etc.) allows for a full ion exchange reaction, achieving efficient desorption of phosphate ions. This process can completely restore the OH- ions in the resin. - The functional groups significantly improve the regeneration rate and reusability of the resin; the waste alkaline liquid after the reaction carries desorption products (such as sodium phosphate) and is discharged into the waste liquid collection tank through the "wastewater pipeline", which is conducive to the subsequent centralized treatment or resource recycling of the waste liquid (such as phosphate recovery) and meets environmental emission standards.

[0039] (iii) After the waste alkali solution is discharged, the resin column is thoroughly rinsed with pure water or deionized water until the pH value of the effluent reaches 6.5 to 7.5 (close to neutral) and the conductivity tends to stabilize. This process effectively avoids the influence of alkali residue on the next round of adsorption effect, and ensures the purity of the crude DMSO and the stability of system operation.

[0040] In summary, by rotating the three adsorption tanks (T-01A, T-01B, and T-01C) and using a "two-use, one-regeneration" operation mode, the system can operate continuously without shutdown, significantly improving equipment utilization and production efficiency, and meeting the needs of large-scale industrial continuous production. Simultaneously, the three-step regeneration method—"nitrogen gas top + alkaline elution + pure water rinsing"—achieves organic matter recovery and efficient impurity desorption, ensuring thorough resin cleaning and activity restoration, significantly extending resin lifespan, and reducing operating costs. Attached Figure Description

[0041] Figure 1 This is a schematic diagram of the overall structure of the crude dimethyl sulfoxide dephosphaterization system of the present invention;

[0042] Figure 2 This is a schematic diagram of the regeneration system in the crude dimethyl sulfoxide dephosphate system of the present invention.

[0043] Figure 3 The results of GC-FID analysis of crude DMSO samples before treatment with the crude dimethyl sulfoxide dephosphaterization system of this invention are shown.

[0044] Figure 4 The results of GC-FID analysis of crude DMSO samples after treatment with the crude dimethyl sulfoxide dephosphaterization system of this invention;

[0045] In the diagram: 1T-01A adsorption tank, 11 first inlet pipe, 12 first outlet pipe, 13 first outlet branch pipe, 14 first inlet pipe switch valve, 15 first outlet pipe switch valve, 16 first outlet branch pipe switch valve; 2T-01B adsorption tank, 21 second inlet pipe, 22 second outlet pipe, 23 second outlet branch pipe, 24 second inlet pipe switch valve, 25 second outlet pipe switch valve, 26 second outlet branch pipe switch valve; 3T-01C Adsorption tank, 31 Third feed pipe, 32 Third discharge pipe, 33 Third discharge branch pipe, 34 Third feed pipe switch valve, 35 Third discharge pipe switch valve, 36 Third discharge branch pipe switch valve, 4 Feed main pipe, 5 Discharge main pipe, 6 Regenerator buffer tank, 61 Alkali inlet pipe, 62 First inlet pipe, 63 Alkali inlet pipe switch valve, 64 Inlet pipe switch valve, 65 Regenerator discharge pipe, 7 Feed pump, 8 Nitrogen inlet pipe, 9 Second inlet pipe. Detailed Implementation

[0046] The technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.

[0047] In the description of this invention, it should be noted that the terms "upper," "lower," "left," "right," "inner," and "outer," etc., indicate the orientation or positional relationship based on the orientation or positional relationship shown in the accompanying drawings. They are only for the convenience of describing this invention and simplifying the description, and do not indicate or imply that the device or element referred to must have a specific orientation, or be constructed and operated in a specific orientation. Therefore, they should not be construed as limiting this invention. In addition, the terms "first" and "second" are used for descriptive purposes only and should not be construed as indicating or implying relative importance.

[0048] In the description of this invention, it should be noted that, unless otherwise explicitly specified and limited, the terms "installation," "connection," and "linking" should be interpreted broadly. For example, they can refer to a fixed connection, a detachable connection, or an integral connection; they can refer to a mechanical connection or an electrical connection; they can refer to a direct connection or an indirect connection through an intermediate medium; and they can refer to the internal connection of two components. Those skilled in the art can understand the specific meaning of the above terms in this invention based on the specific circumstances. This invention relates to circuits, electronic components, and modules, all of which are prior art and can be fully implemented by those skilled in the art.

[0049] Unless otherwise specified, the experimental methods used in the following examples are conventional methods.

[0050] Unless otherwise specified, all materials and reagents used in the following examples are commercially available.

[0051] Example 1

[0052] This invention provides a crude dimethyl sulfoxide dephosphate system. The technical solution of this invention will be further described below with reference to the accompanying drawings:

[0053] See Figure 1 As shown, the crude dimethyl sulfoxide dephosphaterization system provided by the present invention includes an adsorption unit, a feeding system, and a discharging system;

[0054] The adsorption unit includes: T-01A adsorption tank 1, T-01B adsorption tank 2 and T-01C adsorption tank 3. All three adsorption tanks are filled with anion exchange resin (which can be a strong base anion exchange resin) for adsorbing phosphate ions.

[0055] The feeding system includes a first feed pipe 11, a second feed pipe 21, and a third feed pipe 31. A first feed pipe switching valve 14, a second feed pipe switching valve 24, and a third feed pipe switching valve 34 are respectively installed on the first feed pipe 11, the second feed pipe 21, and the third feed pipe 31. The first feed pipe 11 is connected to the bottom of the T-01A adsorption tank 1, the second feed pipe 21 is connected to the bottom of the T-01B adsorption tank 2, and the third feed pipe 31 is connected to the bottom of the T-01C adsorption tank 3. All three feed pipes are connected to the main feed pipe 4.

[0056] The discharge system includes a first discharge pipe 12, a second discharge pipe 22, and a third discharge pipe 32. The first discharge pipe 12, the second discharge pipe 22, and the third discharge pipe 32 are respectively equipped with a first discharge pipe switch valve 15, a second discharge pipe switch valve 25, and a third discharge pipe switch valve 35. The first discharge pipe 12 is connected to the top of the T-01A adsorption tank 1, the second discharge pipe 22 is connected to the top of the T-01B adsorption tank 2, and the third discharge pipe 32 is connected to the top of the T-01C adsorption tank 3. The first discharge pipe 12, the second discharge pipe 22, and the third discharge pipe 32 are all connected to the main discharge pipe 5.

[0057] In the above embodiment, the T-01A adsorption tank 1 is connected to the T-01B adsorption tank 2 through the first discharge branch pipe 13. One end of the first discharge branch pipe 13 is connected to the first discharge pipe 12, and the other end is connected to the second feed pipe 21. The T-01B adsorption tank 2 is connected to the T-01C adsorption tank 3 through the second discharge branch pipe 23. One end of the second discharge branch pipe 23 is connected to the second discharge pipe 22, and the other end is connected to the third feed pipe 31. The T-01C adsorption tank 3 is connected to the T-01A adsorption tank 1 through the third discharge branch pipe 33. One end of the third discharge branch pipe 33 is connected to the third discharge pipe 32, and the other end is connected to the first feed pipe 11. The first discharge branch pipe 13, the second discharge branch pipe 23, and the third discharge branch pipe 33 are respectively equipped with a first discharge branch pipe switch valve 16, a second discharge branch pipe switch valve 26, and a third discharge branch pipe switch valve 36.

[0058] See Figure 2 As shown, the system of the present invention is further configured with a regenerant supply unit, which includes a regenerant buffer tank 6. One side of the regenerant buffer tank 6 is connected to an alkali inlet pipe 61 and a first inlet pipe 62. An alkali inlet pipe switch valve 63 is provided on the alkali inlet pipe 61, and an inlet pipe switch valve 64 is provided on the first inlet pipe 62. The other side of the regenerant buffer tank 6 is connected to a feeding pump 7 through a regenerant discharge pipe 65. The feeding pump 7 is then connected to the discharge pipe of each adsorption tank (T-01A adsorption tank 1, T-01B adsorption tank 2, and T-01C adsorption tank 3) through independent pipes, and each adsorption tank has a switch valve on its corresponding independent pipe.

[0059] In the above embodiments, the discharge pipes of adsorption tank 1 (T-01A), adsorption tank 2 (T-01B), and adsorption tank 3 (T-01C) are respectively connected to nitrogen inlet pipe 8 and second liquid inlet pipe 9, and both nitrogen inlet pipe 8 and second liquid inlet pipe 9 are equipped with switch valves.

[0060] In the above embodiments, the feed pipes of adsorption tank 1 (T-01A), adsorption tank 2 (T-01B), and adsorption tank 3 (T-01C) are all connected to a wastewater discharge pipeline and a crude dimethyl sulfoxide discharge pipeline. The wastewater discharge pipeline is connected to a waste liquid collection tank, and the crude dimethyl sulfoxide discharge pipeline is connected to a raw material tank.

[0061] Meanwhile, in the above embodiments, adsorption tanks 1 (T-01A), 2 (T-01B), and 3 (T-01C) are all equipped with pressure gauges (PIA) and level gauges (LIA) for real-time monitoring of the pressure and level inside the tanks. The system is also equipped with a corresponding integrated PLC or DCS control system to realize fully automatic switching and operation monitoring between adsorption and regeneration conditions of each adsorption tank, effectively reducing manual intervention and significantly improving the stability, safety, and repeatability of system operation.

[0062] Example 2

[0063] This embodiment describes a process for dephosphaterosis of crude dimethyl sulfoxide using the system provided in Example 1. The specific operation steps are as follows:

[0064] S1. Initial adsorption stage:

[0065] Open the first feed pipe switch valve 14, the first discharge branch pipe switch valve 16, and the second discharge pipe switch valve 25, and close the relevant valves of the other adsorption tanks, so that the T-01A adsorption tank 1 and the T-01B adsorption tank 2 form a series circuit; the crude dimethyl sulfoxide raw material pressurized to 0.4~0.6MPa flows into the first feed pipe 11 through the feed main pipe 4 and is sent into the T-01A adsorption tank 1. The material treated by the T-01A adsorption tank 1 flows into the T-01B adsorption tank 2 through the first discharge branch pipe 16; wherein T-01A is used as the first-stage adsorption tank to remove most of the phosphate ions in the material, and T-01B is used as the second-stage adsorption tank to further remove the residual phosphate ions. After adsorption treatment, the material flows into the discharge main pipe 5 through the second discharge pipe 22 for output.

[0066] S2. Operation Switching and Regeneration Startup:

[0067] After the system has been running continuously for a period of time, when the anion exchange resin in adsorption tank 1 of T-01A is close to saturation, the first feed pipe switch valve 14, the first discharge branch pipe switch valve 16, and the second discharge pipe switch valve 25 are closed; the second feed pipe switch valve 24, the second discharge branch pipe switch valve 26, and the third discharge pipe switch valve 35 are opened, and the system switches to the series operation of adsorption tank 2 of T-01B and adsorption tank 3 of T-01C, entering a new adsorption stage; at this time, T-01B acts as the first-stage adsorption tank, and T-01C acts as the second-stage adsorption tank; at the same time, adsorption tank 1 of T-01A stops feeding and enters the regeneration stage.

[0068] S3. Switching and Regeneration Cycle:

[0069] After the system continues to run for a period of time, when the anion exchange resin in adsorption tank 2 of T-01B is close to saturation, the second feed pipe switch valve 24, the second discharge branch pipe switch valve 26, and the third discharge pipe switch valve 35 are closed; the third feed pipe switch valve 34, the third discharge branch pipe switch valve 36, and the first discharge pipe switch valve 15 are opened, switching to the series operation of adsorption tanks T-01C and T-01A, with T-01C as the first-stage adsorption tank and T-01A as the second-stage adsorption tank; at the same time, adsorption tank 2 of T-01B stops feeding and enters the regeneration stage.

[0070] S4. Switching and regeneration cycle again:

[0071] After the system continues to run for a period of time, when the anion exchange resin in adsorption tank 3 of T-01C is close to saturation, the third feed pipe switch valve 34, the third discharge branch pipe switch valve 36, and the first discharge pipe switch valve 15 are closed; the first feed pipe switch valve 14, the first discharge branch pipe switch valve 16, and the second discharge pipe switch valve 25 are opened, and the system switches back to the series operation of adsorption tanks T-01A and T-01B, with T-01A as the first-stage adsorption tank and T-01B as the second-stage adsorption tank; at the same time, adsorption tank 3 of T-01C stops feeding and enters the regeneration stage.

[0072] S5. Cyclic Operation Mode:

[0073] The above switching process is repeated in sequence, forming a cyclical operation mode of three tanks rotating, two for use and one for regeneration, to ensure continuous and stable operation of the system; after each switch, two adsorption tanks are always in series adsorption state, while the other adsorption tank enters the regeneration process.

[0074] Example 3

[0075] This embodiment describes the regeneration stage of the crude dimethyl sulfoxide dephosphate removal process in Embodiment 2 above. The specific operation steps are as follows:

[0076] S11. When any adsorption tank (T-01A, T-01B or T-01C) completes adsorption operation and enters the regeneration stage, nitrogen with a purity ≥99.5% is used through nitrogen inlet pipe 8 to replace the crude dimethyl sulfoxide raw material remaining in the resin column of the adsorption tank. The material in the resin column is then pushed back to the raw material tank through the "crude dimethyl sulfoxide inlet pipeline" to realize the recycling of the material. At the same time, the organic media in the resin bed are removed to avoid the residue from interfering with the subsequent regeneration process.

[0077] S12. After the gas cap is completed, the alkaline regeneration solution (a sodium hydroxide aqueous solution with a mass concentration of 2% to 10%) prepared in the regenerator buffer tank 6 is introduced into the adsorption tank from top to bottom at a flow rate of 1 to 3 BV / h. The alkaline solution flows through the resin layer under the action of gravity or pressure, and exchanges phosphate ions (such as H2PO4) on the anion exchange resin. - HPO4 2- (etc.) undergo ion exchange reaction to achieve phosphate desorption; the waste liquid generated by the reaction carries the desorption products and is discharged to the waste liquid collection tank through the "wastewater pipeline" for centralized treatment or resource recycling.

[0078] S13. After the waste alkali solution is discharged, the resin column in the adsorption tank is rinsed with pure water or deionized water through the second inlet pipe 9 to remove residual alkali solution and soluble salts until the pH value of the effluent drops to 6.5-7.5 and the conductivity tends to stabilize, indicating that the resin has been cleaned. After regeneration, the adsorption tank is ready to be put into the next adsorption cycle.

[0079] The changes in the content of each component in crude dimethyl sulfoxide before and after treatment by the dephosphaterosis system of the present invention are shown in Table 1 below:

[0080] Table 1

[0081] Serial Number Components Before being processed by the system of this invention After being processed by the system of this invention 1 dimethyl sulfoxide 38.5％ 38.5％ 2 dimethyl sulfone 1.5％ 1.5％ 3 water 57.5％ 57.5％ 4 Methanethiol 2.5％ 2.5％ 5 phosphate 150PPM 5PPM

[0082] Table 1 shows that the contents of dimethyl sulfoxide, dimethyl sulfone, water, and methanethiol in the crude dimethyl sulfoxide remained unchanged before and after treatment, indicating that the dephosphaterosis system had no significant effect on these substances and demonstrated good selectivity, removing only phosphate ions. Furthermore, the phosphate content decreased from 150 PPM before treatment to 5 PPM after treatment, achieving a removal rate as high as 96.67%, thus demonstrating the high efficiency of the crude dimethyl sulfoxide dephosphaterosis system of this invention in removing phosphate ions.

[0083] The changes in the content of dimethyl sulfoxide and dimethyl sulfone in crude dimethyl sulfoxide before and after treatment by the crude dimethyl sulfoxide dephosphaterization system of the present invention are as follows: Figure 3 and Figure 4 As shown:

[0084] Figure 3 The figures show the GC-FID results of crude DMSO samples before treatment with the crude dimethyl sulfoxide dephosphaterization system of this invention. As can be seen from the figures, the retention time of dimethyl sulfoxide is 3.684 min, the peak area is 13115.18 pA·s, the peak area percentage is 92.167%, the peak height is 3930.91 pA, and the peak width is 0.46 min; the retention time of dimethyl sulfone is 7.919 min, the peak area is 10.47 pA·s, the peak area percentage is 0.0736%, the peak height is 2.8 pA, and the peak width is 0.29 min.

[0085] Figure 4 The figures show the GC-FID results of crude DMSO samples after treatment with the crude dimethyl sulfoxide dephosphaterization system of this invention. As can be seen from the figures, the retention time of dimethyl sulfoxide is 3.685 min, the peak area is 13177.87 pA·s, the peak area percentage is 93.676%, the peak height is 3777.92 pA, and the peak width is 0.5 min; the retention time of dimethyl sulfone is 7.919 min, the peak area is 13.420 pA·s, the peak area percentage is 0.0954%, the peak height is 3.59 pA, and the peak width is 0.28 min.

[0086] By comparing the data before and after treatment, it can be seen that the peak area and peak height of dimethyl sulfoxide (DMSO) increased slightly after treatment, but the changes were not significant; this indicates that the content of DMSO remained basically stable during the phosphate removal process, without significant changes. The peak area and peak height of dimethyl sulfone (DMS) also increased slightly after treatment, but again the changes were not significant; this indicates that the content of DMSO did not change significantly during the phosphate removal process.

[0087] This indicates that when using this system for phosphate removal, the content of dimethyl sulfoxide and dimethyl sulfone is minimally affected, remaining essentially unchanged before and after treatment. This demonstrates the system's good selectivity, primarily targeting phosphate ion removal while having minimal impact on other organic components, effectively protecting the purity and stability of the target product.

[0088] In summary, by employing a "two-use, one-regeneration" operation mode for the three adsorption tanks (T-01A, T-01B, and T-01C), not only was continuous and stable operation of the system achieved, but the phosphate content in crude dimethyl sulfoxide was also significantly reduced, achieving the expected purification effect. This process method has high practical value and promotion potential in real-world applications, and is suitable for various industrial scenarios requiring efficient phosphate removal.

[0089] The foregoing has provided a detailed description of a crude dimethyl sulfoxide dephosphaterization system and its process disclosed in this invention. Specific examples have been used to illustrate the principles and implementation methods of this invention. The descriptions of the embodiments above are merely for the purpose of helping to understand the method and core ideas of this invention. It should be noted that those skilled in the art can make various improvements and modifications to this invention without departing from its principles, and these improvements and modifications also fall within the protection scope of the claims of this invention.

Claims

1. A crude dimethyl sulfoxide dephosphaterization system, characterized in that, Includes an adsorption unit, a feeding system, and a discharging system; The adsorption unit includes a T-01A adsorption tank (1), a T-01B adsorption tank (2), and a T-01C adsorption tank (3), all three adsorption tanks being filled with anion exchange resin for adsorbing phosphate ions. The feeding system includes a first feed pipe (11), a second feed pipe (21), and a third feed pipe (31); the first feed pipe (11) is connected to the bottom of the T-01A adsorption tank (1), the second feed pipe (21) is connected to the bottom of the T-01B adsorption tank (2), and the third feed pipe (31) is connected to the bottom of the T-01C adsorption tank (3); the first feed pipe (11), the second feed pipe (21), and the third feed pipe (31) are all connected to the main feed pipe (4); The discharge system includes a first discharge pipe (12), a second discharge pipe (22), and a third discharge pipe (32); the first discharge pipe (12) is connected to the top of the T-01A adsorption tank (1), the second discharge pipe (22) is connected to the top of the T-01B adsorption tank (2), and the third discharge pipe (32) is connected to the top of the T-01C adsorption tank (3); the first discharge pipe (12), the second discharge pipe (22), and the third discharge pipe (32) are all connected to the main discharge pipe (5).

2. The crude dimethyl sulfoxide dephosphaterization system according to claim 1, characterized in that, The T-01A adsorption tank (1) is connected to the T-01B adsorption tank (2) through the first discharge branch pipe (13). One end of the first discharge branch pipe (13) is connected to the first discharge pipe (12), and the other end is connected to the second feed pipe (21). The T-01B adsorption tank (2) is connected to the T-01C adsorption tank (3) through the second discharge branch pipe (23). One end of the second discharge branch pipe (23) is connected to the second discharge pipe (22), and the other end is connected to the third feed pipe (31). The T-01C adsorption tank (3) is connected to the T-01A adsorption tank (1) through the third discharge branch pipe (33). One end of the third discharge branch pipe (33) is connected to the third discharge pipe (32), and the other end is connected to the first feed pipe (11).

3. The crude dimethyl sulfoxide dephosphaterization system according to claim 2, characterized in that, The first feed pipe (11), the second feed pipe (21) and the third feed pipe (31) are respectively equipped with a first feed pipe switch valve (14), a second feed pipe switch valve (24) and a third feed pipe switch valve (34); the first discharge pipe (12), the second discharge pipe (22) and the third discharge pipe (32) are respectively equipped with a first discharge pipe switch valve (15), a second discharge pipe switch valve (25) and a third discharge pipe switch valve (35); the first discharge branch pipe (13), the second discharge branch pipe (23) and the third discharge branch pipe (33) are respectively equipped with a first discharge branch pipe switch valve (16), a second discharge branch pipe switch valve (26) and a third discharge branch pipe switch valve (36).

4. The crude dimethyl sulfoxide dephosphaterization system according to claim 3, characterized in that, The system is also equipped with a regenerant supply unit, which includes a regenerant buffer tank (6). One side of the regenerant buffer tank (6) is connected to an alkali inlet pipe (61) and a first inlet pipe (62). An alkali inlet pipe switch valve (63) is provided on the alkali inlet pipe (61), and an inlet pipe switch valve (64) is provided on the first inlet pipe (62). The other side of the regenerant buffer tank (6) is connected to a feeding pump (7) through a regenerant discharge pipe (65). The feeding pump (7) is then connected to the discharge pipe of each adsorption tank through independent pipes, and each adsorption tank has a switch valve on its corresponding independent pipe.

5. The crude dimethyl sulfoxide dephosphaterization system according to claim 4, characterized in that, The discharge pipes of the T-01A adsorption tank (1), T-01B adsorption tank (2) and T-01C adsorption tank (3) are respectively connected to a nitrogen inlet pipe (8) and a second liquid inlet pipe (9), and both the nitrogen inlet pipe (8) and the second liquid inlet pipe (9) are equipped with switching valves.

6. The crude dimethyl sulfoxide dephosphaterization system according to claim 5, characterized in that, The feed pipes of the T-01A adsorption tank (1), T-01B adsorption tank (2) and T-01C adsorption tank (3) are all connected to a wastewater pipeline and a crude dimethyl sulfoxide inlet pipeline; the wastewater pipeline is connected to the waste liquid collection tank and the crude dimethyl sulfoxide inlet pipeline is connected to the raw material tank.

7. A process for removing acid radicals from crude dimethyl sulfoxide using the system described in any one of claims 1-6, characterized in that, Includes the following steps: S1. Initial adsorption stage: Open the first feed pipe valve, the first discharge branch pipe valve, and the second discharge pipe valve, and close the relevant valves of the other adsorption tanks to form a series circuit between adsorption tanks T-01A and T-01B. Feed crude dimethyl sulfoxide (DMSO) material pressurized to 0.4–0.6 MPa into adsorption tank T-01A via the main feed pipe and the first feed pipe. After treatment with the anion exchange resin in adsorption tank T-01A, the material flows into adsorption tank T-01B via the first discharge branch pipe. T-01A serves as the first-stage adsorption tank to remove most of the phosphate ions from the material, while T-01B serves as the second-stage adsorption tank to further remove residual phosphate ions. After adsorption treatment, the material flows into the main discharge pipe via the second discharge pipe for output. S2. Operation Switching and Regeneration Startup: After the system has been running continuously for a period of time, when the anion exchange resin in the T-01A adsorption tank is close to saturation, the first feed pipe valve, the first discharge branch pipe valve, and the second discharge pipe valve are closed; the second feed pipe valve, the second discharge branch pipe valve, and the third discharge pipe valve are opened, switching to the series operation of the T-01B and T-01C adsorption tanks, entering a new adsorption stage; at this time, T-01B acts as the first-stage adsorption tank, and T-01C acts as the second-stage adsorption tank; simultaneously, the T-01A adsorption tank stops feeding and enters the regeneration stage. S3. Switching and Regeneration Cycle: After the system continues to run for a period of time, when the anion exchange resin in the T-01B adsorption tank is close to saturation, the second feed pipe switch valve, the second discharge branch pipe switch valve, and the third discharge pipe switch valve are closed; the third feed pipe switch valve, the third discharge branch pipe switch valve, and the first discharge pipe switch valve are opened, switching to the T-01C and T-01A adsorption tanks to operate in series, with T-01C as the first-stage adsorption tank and T-01A as the second-stage adsorption tank; at the same time, the T-01B adsorption tank stops feeding and enters the regeneration stage. S4. Switching and regeneration cycle again: After the system continues to run for a period of time, when the anion exchange resin in the T-01C adsorption tank is close to saturation, the third feed pipe switch valve, the third discharge branch pipe switch valve, and the first discharge pipe switch valve are closed; the first feed pipe switch valve, the first discharge branch pipe switch valve, and the second discharge pipe switch valve are opened, and the system switches back to the series operation of the T-01A and T-01B adsorption tanks, with T-01A acting as the first-stage adsorption tank and T-01B acting as the second-stage adsorption tank; at the same time, the T-01C adsorption tank 3 stops feeding and enters the regeneration stage. S5. Cyclic Operation Mode: The above switching process is repeated in sequence, forming a cyclical operation mode of three tanks rotating, two for use and one for regeneration, to ensure continuous and stable operation of the system; after each switch, two adsorption tanks are always in series adsorption state, while the other adsorption tank enters the regeneration process.

8. The method according to claim 7, characterized in that, The regeneration stage steps are as follows: S11. When any adsorption tank (T-01A, T-01B or T-01C) completes adsorption operation and enters the regeneration stage, nitrogen is first used to replace the crude dimethyl sulfoxide raw material remaining in the resin column of the adsorption tank. The material remaining in the resin column is then pushed back to the raw material tank through the "crude dimethyl sulfoxide inlet pipeline" to realize the recycling of the material. S12. After the gas top is completed, the alkaline regeneration solution prepared in the regenerator buffer tank is introduced into the adsorption tank from top to bottom. The alkaline solution reacts with the phosphate ions on the anion exchange resin to achieve the desorption of phosphate ions. The waste liquid after the reaction is discharged to the waste liquid collection tank through the "wastewater pipeline". S13. After the waste alkaline solution is drained, the resin column is rinsed with pure water or deionized water until the pH value of the effluent drops to 6.5-7.5 and the conductivity tends to stabilize, indicating that the resin has been cleaned. After regeneration, the adsorption tank is ready to be put into the next adsorption cycle.

9. The method according to claim 8, characterized in that, The nitrogen gas purity is ≥99.5%.

10. The method according to claim 8, characterized in that, The alkaline regeneration solution is a sodium hydroxide aqueous solution with a mass concentration of 2% to 10%, and the flow rate of the alkaline solution is 1 to 3 BV / h.

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