NMP (N-Methyl Pyrrolidone) waste liquid neutralization reaction settling separation device

By integrating a neutralization reaction tank and an overflow separator, the problem of low NMP waste liquid separation efficiency in traditional methods has been solved, achieving high-efficiency NMP waste liquid separation and improving product yield and system stability.

CN223547826UActive Publication Date: 2025-11-14JIANGSU YONGMAI RECYCLING TECH CO LTD
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Patent Information

Application Number
CN202423025555.X
Authority / Receiving Office
CN · China
Patent Type
Utility models(China)
Current Assignee / Owner
Filing Date
2024-12-09
Publication Date
2025-11-14
Estimated Expiration
2034-12-09

AI Technical Summary

Technical Problem

Traditional NMP waste liquid neutralization reaction sedimentation separation method is difficult to effectively separate the aqueous phase and impurity salts, resulting in NMP decomposition, distillation system blockage, increased energy consumption, and reduced production capacity.

Method used

The separation device, which integrates a neutralization reaction tank and an overflow separator, uses an inverted conical structure and sight glass control to achieve two-stage separation of NMP waste liquid, ensuring that the salt-containing alkaline liquid is completely discharged and preventing it from entering the distillation system.

Benefits of technology

It improved the yield of NMP products, reduced the generation of secondary hazardous waste, reduced the energy consumption of the distillation system, and increased production capacity.

✦ Generated by Eureka AI based on patent content.

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Abstract

The utility model relates to an NMP (N-Methyl Pyrrolidone) waste liquid neutralization reaction settling separation device and belongs to the technical field of NMP recovery. The device comprises a neutralization reaction tank, an overflow liquid separation tank, an overflow pipeline and a first communication pipeline, a discharge hole of the neutralization reaction tank is communicated with an inlet / outlet of the overflow liquid separation tank through the first communication pipeline; tank bodies of the neutralization reaction tank and the overflow liquid separation tank are communicated through the overflow pipeline; a stirring paddle is arranged in the neutralization reaction tank. According to the NMP waste liquid neutralization reaction settling separation device, two times of liquid separation of the NMP waste liquid are carried out through the neutralization reaction tank and the overflow liquid separation tank, salt-containing alkali liquid can be thoroughly discharged out of an NMP system, and NMP decomposition caused by the fact that excessive alkali liquid cannot be discharged out of the storage tank in time is avoided, so that the product yield is improved, the salt-containing alkali liquid is prevented from entering a rectification system, and the product quality is improved. Secondary hazardous wastes are reduced, the stability of a rectification system is ensured, and the energy consumption is reduced.
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Description

Technical Field

[0001] This utility model belongs to the field of NMP recycling technology and relates to an NMP waste liquid neutralization reaction sedimentation separation device. Background Technology

[0002] Traditional methods for neutralizing and separating NMP (N-methylpyrrolidone) waste liquid mainly involve mixing, sedimentation, and periodic sludge removal (aqueous phase and impurity salts). After multiple neutralizations with alkali, the aqueous phase and insoluble impurity salts gradually accumulate and settle at the bottom of the storage tank. The traditional method of pumping the supernatant is difficult to achieve ideal separation, and the excess alkali accumulated in the storage tank can easily cause NMP decomposition if not discharged in time. In addition, pumping the supernatant can easily carry impurity salts into the next step of the distillation system, causing solid impurities to accumulate and block the reboiler, reducing heating efficiency. As a result, the circulation of the feed liquid in the distillation column is not smooth, and local overheating further aggravates the pyrolysis and polymerization of NMP, deteriorating the thermal efficiency of the reboiler. This leads to instability of the entire distillation system, increased energy consumption, and reduced production capacity. Utility Model Content

[0003] The purpose of this invention is to overcome the shortcomings of the existing technology and provide an NMP waste liquid neutralization reaction sedimentation separation device that integrates reaction and separation, is easy to operate, and has high separation efficiency.

[0004] To achieve the above objectives, this utility model employs the following technical solution:

[0005] This utility model provides an NMP waste liquid neutralization reaction sedimentation separation device, the device includes: a neutralization reaction tank, an overflow separator, an overflow pipe and a first connecting pipe;

[0006] The outlet of the neutralization reaction tank and the inlet and outlet of the overflow separator are connected through the first connecting pipe.

[0007] The neutralization reaction tank and the overflow separator are connected by the overflow pipe;

[0008] The neutralization reaction vessel is equipped with a stirring paddle.

[0009] Furthermore, the lower end caps of both the neutralization reaction tank and the overflow separator are inverted conical structures, and the outlet of the neutralization reaction tank and the inlet and outlet of the overflow separator are located at the apex of the inverted conical structure.

[0010] Furthermore, the overflow pipe is equipped with a pipe valve and a sight glass.

[0011] Furthermore, sight glasses are provided at the outlet of the neutralization reaction vessel and the inlet and outlet of the overflow separator.

[0012] Furthermore, a pipeline valve is provided between the outlet of the neutralization reaction tank and the first connecting pipe; a pipeline valve is provided between the inlet and outlet of the overflow separator and the first connecting pipe.

[0013] Furthermore, a pipe valve is installed on the first connecting pipe.

[0014] Furthermore, it also includes: the outlet of the neutralization reaction vessel is connected to the distillation system via a second connecting pipe.

[0015] Furthermore, a pipe valve is installed on the second connecting pipe.

[0016] Furthermore, it also includes: the inlet and outlet of the overflow separator are connected to the alkali collection tank via a third connecting pipe.

[0017] Furthermore, a pipe valve is installed on the third connecting pipe.

[0018] Compared with the prior art, the beneficial effects achieved by this utility model are as follows:

[0019] The NMP waste liquid neutralization reaction sedimentation separation device provided by this utility model performs two separations of NMP waste liquid through a neutralization reaction tank and an overflow separator. This can completely discharge the salt-containing alkaline solution from the NMP system, avoiding the excessive alkaline solution in the storage tank that cannot be discharged in time and cause NMP decomposition, thereby improving product yield and preventing the salt-containing alkaline solution from entering the distillation system. This helps to reduce residue in the distillation vessel, thereby reducing the generation of secondary hazardous waste, reducing the energy consumption of the distillation system, and increasing production capacity. Attached Figure Description

[0020] Figure 1 A schematic diagram of the structure of an NMP waste liquid neutralization reaction sedimentation and separation device provided in this embodiment of the present invention;

[0021] Figure 2 This is a schematic diagram of the NMP waste liquid and alkaline solution being mixed and stirred in the NMP waste liquid neutralization reaction sedimentation separation device in this embodiment of the present invention.

[0022] Figure 3 This is a schematic diagram of the NMP waste liquid neutralization reaction sedimentation separation device in this embodiment of the present invention, showing the settling and primary separation processes.

[0023] Figure 4 This is a schematic diagram of the NMP waste liquid transfer and secondary separation process performed by the NMP waste liquid neutralization reaction sedimentation separation device in this embodiment of the present invention.

[0024] Figure 5 This is a schematic diagram of the discharge of salt-containing alkaline liquid from the NMP waste liquid neutralization reaction sedimentation separation device in this embodiment of the present invention;

[0025] In the diagram, 1: Neutralization reaction vessel; 2: Overflow separator; 1-1: Agitator; 2-1: First pipeline valve; 2-2: Sixth pipeline valve; 2-3: Fourth pipeline valve; 2-4: Fifth pipeline valve; 2-5: Second pipeline valve; 2-6: Third pipeline valve; 3-1: First sight glass; 3-2: Second sight glass; 3-3: Third sight glass; 4-1: First connecting pipeline; 4-2: Overflow pipeline. Detailed Implementation

[0026] The technical solution of this utility model will be described in detail below with reference to the accompanying drawings and specific embodiments. The same reference numerals in the drawings indicate the same or similar components or parts. Those skilled in the art should understand that these drawings are not necessarily drawn to scale. The embodiments and specific features within the embodiments of this application are detailed descriptions of the technical solution of this application, and not limitations thereof. Where there is no conflict, the embodiments and technical features within the embodiments of this application can be combined with each other.

[0027] In the description of this utility model, it should be understood that the terms "center," "longitudinal," "lateral," "upper," "lower," "front," "rear," "left," "right," "vertical," "horizontal," "top," "bottom," "inner," and "outer," etc., indicating the orientation or positional relationship, are based on the orientation or positional relationship shown in the accompanying drawings. They are only for the convenience of describing this utility model 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 limitations on this utility model. Furthermore, the term "and / or" in this document is merely a description of the relationship between related objects, indicating that three relationships can exist. For example, A and / or B can represent: A existing alone, A and B existing simultaneously, and B existing alone. Additionally, the character " / " in this document generally indicates that the preceding and following related objects have an "or" relationship.

[0028] In the description of this utility model, it should be noted that, unless otherwise explicitly specified and limited, the terms "installation," "connection," and "joining" 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 utility model based on the specific circumstances.

[0029] Example 1:

[0030] like Figure 1As shown, this utility model embodiment provides an NMP waste liquid neutralization reaction sedimentation separation device, the device includes a neutralization reaction tank 1, an overflow separator 2, an overflow pipe 4-2, and a first connecting pipe 4-1; the discharge port of the neutralization reaction tank 1 and the inlet and outlet of the overflow separator 2 are connected through the first connecting pipe 4-1; the tank bodies of the neutralization reaction tank 1 and the overflow separator 2 are connected through the overflow pipe 4-2.

[0031] The top of the neutralization reaction tank 1 is equipped with an alkali inlet and an NMP waste liquid inlet, which are connected to pipelines and are equipped with pipeline valves.

[0032] The discharge port of neutralization reaction tank 1 is located at the bottom of neutralization reaction tank 1, and the inlet and outlet of overflow separator 2 are located at the bottom of overflow separator 2. The lower end caps of neutralization reaction tank 1 and overflow separator 2 are both inverted conical structures, and the discharge port of neutralization reaction tank 1 and the inlet and outlet of overflow separator 2 are located at the apex of their respective inverted conical structures.

[0033] The neutralization reaction vessel 1 is equipped with a stirring paddle 1-1, which extends from the top of the neutralization reaction vessel 1 into the vessel near the lower end cap to fully stir the liquid entering the neutralization reaction vessel 1.

[0034] The overflow pipe 4-2 is equipped with a first pipeline valve 2-1 and a first sight glass 3-1.

[0035] The first sight glass 3-1 is close to the overflow separator 2. During the secondary separation, the NMP clear liquid in the overflow separator 2 enters the neutralization reaction tank 1 through the overflow pipe 4-2. The first sight glass 3-1 can observe the liquid composition flowing into the overflow pipe 4-2 in time so as to close the first pipeline valve 2-1 in time and prevent the salt-alkali liquid from entering the neutralization reaction tank 1.

[0036] The outlet of the neutralization reaction vessel 1 is equipped with a second sight glass 3-2; a second pipeline valve 2-5 is also installed on the connecting pipeline between the outlet of the neutralization reaction vessel 1 and the first connecting pipeline 4-1.

[0037] The overflow separator 2 is equipped with a third sight glass 3-3 at its inlet and outlet; a third pipeline valve 2-6 is also provided on the connecting pipeline between the inlet and outlet of the overflow separator 2 and the first connecting pipeline 4-1.

[0038] Similar to the first sight glass 3-1, the second sight glass 3-2 is used to observe the liquid composition flowing out of the neutralization reaction tank 1 so as to close the second pipeline valve 2-5 in time. The third sight glass 3-3 is used to observe the liquid composition flowing into and out of the overflow separator 2 so as to close the third pipeline valve 2-6 in time.

[0039] By installing a first sight glass 3-1, a second sight glass 3-2, and a third sight glass 3-3 at the inlet and outlet positions of the neutralization reaction tank 1 and the overflow separator 2, the effect of precise liquid separation can be achieved.

[0040] In this embodiment, the first sight glass 3-1, the second sight glass 3-2, and the third sight glass 3-3 are all installed on the pipe, so pipe sight glasses are used.

[0041] The first connecting pipe 4-1 connects the second pipe valve 2-5 and the third pipe valve 2-6, and a fourth pipe valve 2-3 is installed on it.

[0042] The discharge port at the bottom of the neutralization reaction tank 1 of this invention is connected to the distillation system through a second connecting pipe, and the inlet and outlet at the bottom of the overflow separator 2 are connected to the alkali collection tank through a third connecting pipe.

[0043] Specifically, the second pipeline valve 2-5 is connected to the distillation system through a second connecting pipeline, and a fifth pipeline valve 2-4 is installed on the second connecting pipeline; the third pipeline valve 2-6 is connected to the alkali collection tank through a third connecting pipeline, and a sixth pipeline valve 2-2 is installed on the third connecting pipeline.

[0044] Example 2:

[0045] like Figures 2 to 5 As shown, this embodiment of the present invention provides a method for neutralization reaction sedimentation separation of NMP waste liquid. This method is based on the NMP waste liquid neutralization reaction sedimentation separation device provided in Embodiment 1. Therefore, the specific limitations of the device mentioned below can be found in the above-described limitations of the NMP waste liquid neutralization reaction sedimentation separation device, and will not be repeated here. The method specifically includes the following steps:

[0046] Initially, all pipeline valves of the NMP waste liquid neutralization reaction sedimentation separation device are closed.

[0047] like Figure 2 As shown, NMP waste liquid is added to neutralization reaction tank 1 through NMP waste liquid inlet and stirred evenly by stirring paddle 1-1. Then, the required alkali solution is added through alkali solution inlet and the NMP waste liquid and alkali solution are mixed and stirred by stirring paddle 1-1 for 1 to 2 hours.

[0048] like Figure 3 As shown, stop stirring and let stand for 2 to 3 hours to allow the NMP waste liquid and the alkaline solution to separate into two layers, with the alkaline solution containing salt at the bottom.

[0049] Open the second pipeline valve 2-5, the fourth pipeline valve 2-3 and the third pipeline valve 2-6 to allow the lower aqueous phase (containing salt and alkali solution) and the transition phase of the neutralization reaction tank 1 to enter the overflow separator 2 through the discharge port of the neutralization reaction tank 1, the first connecting pipeline 4-1 and the inlet of the overflow separator 2.

[0050] After observing through the second sight glass 3-2 to ensure that there is only NMP clear liquid in the neutralization reaction tank 1, close the fourth pipeline valve 2-3 and the third pipeline valve 2-6, open the fifth pipeline valve 2-4, and the NMP clear liquid in the upper layer of the neutralization reaction tank 1 enters the distillation system. Then close the second pipeline valve 2-5 and the fifth pipeline valve 2-4.

[0051] like Figure 4 As shown, after standing for 2 to 3 hours, the NMP clear liquid and the salt-containing alkaline liquid in the overflow separator 2 will separate into layers.

[0052] Open the first pipeline valve 2-1 to allow the organic phase (NMP clear liquid) on the upper layer of the overflow separator 2 to enter the neutralization reaction tank 1 through the overflow pipe 4-2. Observe through the first sight glass 3-1. When all the NMP clear liquid has entered the neutralization reaction tank 1, close the first pipeline valve 2-1.

[0053] Open the second pipeline valve 2-5 and the fifth pipeline valve 2-4 to introduce the NMP solution in the neutralization reaction tank 1 into the distillation system for distillation regeneration.

[0054] Finally, as Figure 5 As shown, open the third pipeline valve 2-6 and the sixth pipeline valve 2-2 to introduce the lower aqueous phase (containing salt and alkali solution) of the overflow separator 2 into the alkali solution collection tank to achieve the purpose of thorough separation.

[0055] The above description is only a preferred embodiment of the present utility model. It should be noted that for those skilled in the art, several improvements and modifications can be made without departing from the technical principles of the present utility model, and these improvements and modifications should also be considered within the scope of protection of this disclosure / application.

Claims

1. A neutralization reaction sedimentation and separation device for NMP waste liquid, characterized in that, include: Neutralization reaction vessel, overflow separator, overflow pipe and first connecting pipe; The outlet of the neutralization reaction tank and the inlet and outlet of the overflow separator are connected through the first connecting pipe. The neutralization reaction tank and the overflow separator are connected by the overflow pipe; The neutralization reaction vessel is equipped with a stirring paddle.

2. The NMP waste liquid neutralization reaction sedimentation separation device according to claim 1, characterized in that, The lower end caps of both the neutralization reaction tank and the overflow separator are inverted conical structures, and the outlet of the neutralization reaction tank and the inlet and outlet of the overflow separator are located at the apex of the inverted conical structure.

3. The NMP waste liquid neutralization reaction sedimentation separation device according to claim 1, characterized in that, The overflow pipe is equipped with a pipe valve and a sight glass.

4. The NMP waste liquid neutralization reaction sedimentation separation device according to claim 1, characterized in that, The neutralization reaction vessel's outlet and the overflow separator's inlet and outlet are both equipped with sight glasses.

5. The NMP waste liquid neutralization reaction sedimentation separation device according to claim 1, characterized in that, A pipe valve is installed between the outlet of the neutralization reaction tank and the first connecting pipe; a pipe valve is installed between the inlet and outlet of the overflow separator and the first connecting pipe.

6. The NMP waste liquid neutralization reaction sedimentation separation device according to claim 5, characterized in that, A pipe valve is installed on the first connecting pipe.

7. The NMP waste liquid neutralization reaction sedimentation separation device according to claim 1, characterized in that, Also includes: The outlet of the neutralization reaction vessel is connected to the distillation system via a second connecting pipe.

8. The NMP waste liquid neutralization reaction sedimentation separation device according to claim 7, characterized in that, A pipe valve is installed on the second connecting pipe.

9. The NMP waste liquid neutralization reaction sedimentation separation device according to claim 1, characterized in that, Also includes: The inlet and outlet of the overflow separator are connected to the alkali collection tank via a third connecting pipe.

10. The NMP waste liquid neutralization reaction sedimentation separation device according to claim 9, characterized in that, A pipe valve is installed on the third connecting pipe.