CN115228137A

CN115228137A - Modularized continuous extraction separation method

Info

Publication number: CN115228137A
Application number: CN202210985468.5A
Authority: CN
Inventors: 张圣成; 李裕超; 王培坤
Original assignee: Mingshi New Materials Co ltd
Current assignee: Mingshi New Materials Co ltd
Priority date: 2022-08-17
Filing date: 2022-08-17
Publication date: 2022-10-25
Anticipated expiration: 2042-08-17
Also published as: CN115228137B

Abstract

The invention discloses a modularized continuous extraction separation method, wherein an extraction generation module is provided with a first liquid inlet, a second liquid inlet and a first discharge port, the first liquid inlet is communicated with a pure water tank, a second liquid inlet communicated with a mixed liquid tank is provided with an annular spray head inside the extraction generation module, the first discharge port is communicated with a third liquid inlet of a solvent replacement module, a first liquid outlet is arranged between the third liquid inlet and a fourth liquid inlet, the first liquid outlet is communicated with a waste liquid tank, the fourth liquid inlet is communicated with the pure water tank, a second discharge port of a solvent extraction device is communicated with a fifth liquid inlet of a material separation device suction filtration tank, a second liquid outlet of the suction filtration tank is communicated with the waste liquid tank, and the suction filtration tank is provided with a third discharge port. The invention adopts the modularized continuous extraction separation method with the structure to perform online continuous extraction and replacement on the solvent, the number of the solvent replacement modules can be selected according to the amount of the extraction materials, and the full-automatic operation of the extraction separation process improves the product quality.

Description

Modularized continuous extraction separation method

Technical Field

The invention relates to the technical field of extraction separation, in particular to a modularized continuous extraction separation method.

Background

Polyimide is abbreviated as PI, refers to a class of polymers containing imide rings on the main chain, and is one of organic high molecular materials with the best comprehensive performance. PI is easily soluble in organic solvents such as dimethylformamide, dimethylacetamide, tetrahydrofuran, dioxygen cyclic ring and the like, and is insoluble in water. At present, the extraction process is generally adopted in PI production to realize solid-liquid separation, and because the extraction agent needs to be replaced in the extraction process, the emission standard can be reached by replacing for many times. However, the existing extraction process of PI generally adopts discontinuous operation, continuous extraction and replacement cannot be realized, the working efficiency is low, and errors generated by manual operation have obvious influence on the quality of products.

Disclosure of Invention

The invention aims to provide a modularized continuous extraction separation method, which can be used for carrying out online continuous extraction and replacement on a solvent, can select the number of solvent replacement modules according to the quantity of extracted materials, and can improve the product quality by fully-automatic operation in the extraction separation process.

In order to achieve the purpose, the invention provides a modularized continuous extraction separation method, which comprises an extraction generation module, a solvent replacement module and a material separation device which are sequentially communicated, and is characterized in that: the extraction generation module is provided with a first inlet, a second inlet and a first discharge port, the first inlet is communicated with a pure water tank, the second inlet is communicated with a mixed liquid tank, an annular spray head is arranged in the extraction generation module, the first discharge port is communicated with a third liquid inlet of the solvent replacement module, a first liquid outlet is arranged between the third liquid inlet and a fourth inlet, the first liquid outlet is communicated with a waste liquid tank, the fourth inlet is communicated with the pure water tank, a second discharge port of the solvent extraction device is communicated with a fifth liquid inlet of the material separation device, a second liquid outlet of the filtration tank is communicated with the waste liquid tank, and the filtration tank is provided with a third discharge port.

Preferably, the diameter of the extraction generation module between the first liquid inlet and the second liquid inlet is reduced and then increased, the circle center of the spray head and the circle center of the extraction generation module are located on the same axis, and the spray head is uniformly provided with a plurality of spray holes.

Preferably, the cross-section of crossing the sap cavity of solvent replacement module is circular, first liquid outlet through go out the sap cavity with cross the sap cavity intercommunication, it establishes to go out the sap cavity cover cross on the sap cavity lateral wall, go out the sap cavity inside cross the sap cavity lateral wall and evenly be equipped with a plurality of filtration pores, cross the sap cavity and be in the lateral wall cover of filtration pore department is equipped with the filter screen.

Preferably, first inlet department is equipped with first valve, second inlet department is equipped with the second valve, fourth inlet department is equipped with the third valve, first outlet department is equipped with the fourth valve, first valve the second valve the third valve with the fourth valve is the governing valve.

Preferably, first discharge gate department is equipped with first pressure transmitter, first discharge gate with be equipped with second pressure transmitter between the fourth inlet, first pressure transmitter control first valve, second pressure transmitter control the third valve.

Preferably, the pure water tank, the mixed liquid tank and the waste liquid tank are respectively provided with a third pressure transmitter.

Preferably, the solvent replacement modules are connected in series, and the pressure value of the second pressure transmitter from the extraction generation module to the material separation device is reduced in sequence.

Therefore, the modular continuous extraction and separation method adopting the structure has the beneficial effects that:

1. carrying out online continuous replacement on the extraction solvent of the PI, supplementing pure water in time according to the replacement amount of the solvent, and enabling the extraction solvent of the PI to meet the discharge requirement after continuous replacement is carried out on a plurality of solvent replacement modules;

2. the number of the solvent replacement modules can be selected according to the amount of the extraction materials by matching with the modularized design so as to meet the separation requirement, and the modules are simple to set and convenient to install and can be flexibly adjusted according to the actual requirement;

3. through reasonable setting of key parameters, full-automatic operation of the extraction and separation process can be realized, uncertain factors caused by manpower are avoided, and the product quality is more stable.

The technical solution of the present invention is further described in detail by the accompanying drawings and embodiments.

Drawings

FIG. 1 is a flow diagram of a modular continuous extraction separation process of the present invention;

FIG. 2 is a flow diagram of a solvent displacement module of a modular continuous extraction separation process of the present invention.

Reference numerals

1. An extraction generation module; 2. a solvent displacement module; 3. a suction filtration tank; 4. a spray head; 5. a pure water tank; 6. a mixed liquid tank; 7. a waste liquid tank; 8. a liquid passing cavity; 9. a liquid outlet ring cavity; 10. a filter screen; 11. a first valve; 12. a second valve; 13. a third valve; 14. a fourth valve; 15. a first pressure transmitter; 16. a second pressure transmitter.

Detailed Description

The technical scheme of the invention is further explained by the attached drawings and the embodiment.

Unless defined otherwise, technical or scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The use of "first," "second," and similar terms in the present application do not denote any order, quantity, or importance, but rather the terms are used to distinguish one element from another. The word "comprising" or "comprises", and the like, means that the element or item listed before the word covers the element or item listed after the word and its equivalents, but does not exclude other elements or items. The terms "connected" or "coupled" and the like are not restricted to physical or mechanical connections, but may include electrical connections, whether direct or indirect. "upper", "lower", "left", "right", and the like are used only to indicate relative positional relationships, and when the absolute position of the object being described is changed, the relative positional relationships may also be changed accordingly.

Fig. 1 is a flow chart of a modular continuous extraction and separation method of the present invention, fig. 2 is a flow chart of a solvent replacement module of a modular continuous extraction and separation method of the present invention, and as shown in the drawing, a modular continuous extraction and separation method includes an extraction generation module 1, a solvent replacement module 2, and a material separation module which are sequentially communicated. The extraction generation module 1 is provided with a first liquid inlet, a second liquid inlet and a first discharge hole, the first liquid inlet is communicated with a pure water tank 5, and the second liquid inlet communicated with a mixed liquid tank 6 is provided with an annular spray nozzle 4 inside the extraction generation module 1. The first discharge port is communicated with a third liquid inlet of the solvent replacement module 2, and a first liquid outlet is arranged between the third liquid inlet and the fourth liquid inlet. The first liquid outlet is communicated with the waste liquid tank 7, the fourth liquid inlet is communicated with the pure water tank 5, and the second discharge hole of the solvent extraction device is communicated with the fifth liquid inlet of the material separation module suction filtration tank 3. The second liquid outlet of the pumping filtration tank 3 is communicated with the waste liquid tank 7, and the pumping filtration tank 3 is provided with a third discharge hole.

The extraction generation module 1 is used for mixing the PI organic solution with pure water, and PI forms suspended matters in emulsion of water and organic solvent in the mixing process. The PI enters the solvent replacement module 2 along with the emulsion, and the organic solvent in the emulsion is gradually replaced by water in the process of moving from the solvent replacement module 2 to the material separation module. Because the PI is insoluble in water, the suspension of the PI and the water is subjected to solid-liquid separation in the suction filtration tank 3 finally, the obtained solid is a finished product, and the liquid enters the waste liquid tank 7.

The diameter of the extraction generation module 1 between the first liquid inlet and the second liquid inlet is reduced and then increased, the circle center of the spray nozzle 4 and the circle center of the extraction generation module 1 are positioned on the same axis, and the spray nozzle 4 is uniformly provided with a plurality of spray holes. The diameter of the first liquid inlet and the second liquid inlet is set, so that the flow speed of pure water is increased after the diameter is reduced, the pure water is matched with the spray head 4, and the uniform mixing of the uniformly sprayed PI organic solution and the high-speed flowing pure water is ensured.

The cross section of the liquid passing cavity 8 of the solvent replacement module 2 is circular, and the first liquid outlet is communicated with the liquid passing cavity 8 through the liquid outlet ring cavity 9. The liquid outlet ring cavity 9 is sleeved on the outer side wall of the liquid passing cavity 8, a plurality of filter holes are uniformly formed in the side wall of the liquid passing cavity 8 in the liquid outlet cavity, and a filter screen 10 is sleeved on the outer side wall of the liquid passing cavity 8 at the filter holes. When the PI flows along with the emulsion in the liquid passing cavity 8, part of the emulsion enters the liquid outlet annular cavity 9 through the filter holes due to the pressure of the emulsion and the pressure difference between the liquid outlet annular cavity 9. Meanwhile, the pressure in the liquid passing cavity 8 is reduced, and pure water needs to be supplemented to the interior of the liquid passing cavity 8, so that the solvent can be replaced. The aperture of the filter screen 10 can be set according to the size of PI particles, so that PI is prevented from entering the liquid outlet ring cavity 9.

The first liquid inlet is provided with a first valve 11, the second liquid inlet is provided with a second valve 12, the fourth liquid inlet is provided with a third valve 13, and the first liquid outlet is provided with a fourth valve 14. The first valve 11, the second valve 12, the third valve 13 and the fourth valve 14 are all adjusting valves, and the first valve 11, the second valve 12 and the third valve 13 can perform water supplementing adjustment according to pressure changes.

A first pressure transmitter 15 is arranged at the first outlet, and a second pressure transmitter 16 is arranged between the first outlet and the fourth inlet. A first pressure transmitter 15 controls the first valve 11 and a second pressure transmitter 16 controls the third valve 13. The first pressure transmitter 15 and the second pressure transmitter 16 respectively monitor the pressure inside the extraction generation module 1 and the liquid passing cavity 8, and when the pressure drops, the first valve 11 and the second valve 12 supplement pure water in time.

The pure water tank 5, the mixed liquid tank 6 and the waste liquid tank 7 are all provided with a third pressure transmitter.

The solvent replacement modules 2 are arranged in series, and the pressure values of the second pressure transmitters 16 from the extraction generation module 1 to the material separation module are sequentially reduced. The number of the solvent replacement modules 2 can be set according to actual conditions, and the replacement effect of the solvent is ensured.

The working process is as follows:

pure water in the pure water tank 5 enters the extraction generation module 1 through the first liquid inlet, and PI organic solution in the mixed liquid tank 6 enters the extraction generation module 1 through the second liquid inlet and the spray head 4. After pure water and PI organic solution are mixed in the extraction generation module 1, PI and emulsion enter the solvent replacement module 2.

The PI and the emulsion sequentially pass through the liquid passing cavities 8 of the plurality of solvent replacement modules 2, part of the emulsion enters the liquid outlet annular cavity 9 through the filter holes, and the emulsion in the liquid outlet annular cavity 9 enters the waste liquid tank 7 through the fourth valve 14. The pressure drops due to the reduction of the emulsion, pure water enters the liquid passing cavity 8 through the third valve 13, and the suspension of PI and pure water flows out of the last solvent replacement module 2.

The suspension enters a suction filtration tank 3 for solid-liquid separation, and the waste liquid enters a waste liquid tank 7 for PI solid collection.

Therefore, the invention adopts the modularized continuous extraction separation method with the structure to perform online continuous extraction and replacement on the solvent, can select the number of the solvent replacement modules according to the amount of the extraction materials, and fully automatically operates to improve the product quality.

Finally, it should be noted that: the above embodiments are only for illustrating the technical solutions of the present invention and not for limiting the same, and although the present invention is described in detail with reference to the preferred embodiments, those of ordinary skill in the art should understand that: modifications and equivalents may be made to the disclosed embodiments without departing from the spirit and scope of the present invention.

Claims

1. A modularization continuous extraction separation method comprises an extraction generation module, a solvent replacement module and a material separation device which are sequentially communicated, and is characterized in that: the extraction generation module is provided with a first inlet, a second inlet and a first discharge port, the first inlet is communicated with a pure water tank, the second inlet is communicated with a mixed liquid tank, an annular spray head is arranged inside the extraction generation module, the first discharge port is communicated with a third liquid inlet of the solvent replacement module, a first liquid outlet is arranged between the third liquid inlet and a fourth inlet, the first liquid outlet is communicated with a waste liquid tank, the fourth inlet is communicated with the pure water tank, a second discharge port of the solvent extraction device is communicated with a fifth inlet of the material separation device suction filtration tank, a second liquid outlet of the suction filtration tank is communicated with the waste liquid tank, and the suction filtration tank is provided with a third discharge port.

2. A modular continuous extractive separation process according to claim 1, wherein: the diameter of the extraction generation module between the first liquid inlet and the second liquid inlet is reduced and then increased, the circle center of the spray head and the circle center of the extraction generation module are located on the same axis, and the spray head is uniformly provided with a plurality of spray holes.

3. A modular continuous extractive separation process according to claim 1, wherein: the cross-section of the liquid passing cavity of the solvent replacement module is circular, the first liquid outlet is communicated with the liquid passing cavity through a liquid outlet ring cavity, the liquid outlet ring cavity is sleeved on the outer side wall of the liquid passing cavity, the liquid passing cavity is internally provided with a plurality of filter holes, and the outer side wall of each filter hole is sleeved with a filter screen.

4. A modular continuous extractive separation process according to claim 1, wherein: first inlet port department is equipped with first valve, second inlet port department is equipped with the second valve, fourth inlet port department is equipped with the third valve, first outlet port department is equipped with the fourth valve, first valve the second valve the third valve with the fourth valve is the governing valve.

5. A modular continuous extractive separation process according to claim 1, wherein: first discharge gate department is equipped with first pressure transmitter, first liquid outlet with be equipped with second pressure transmitter between the fourth inlet, first pressure transmitter control first valve, second pressure transmitter control the third valve.

6. A modular continuous extractive separation process according to claim 1, wherein: and the pure water tank, the mixed liquid tank and the waste liquid tank are respectively provided with a third pressure transmitter.

7. A modular continuous extractive separation process according to claim 1, wherein: and the solvent replacement modules are connected in series, and the pressure values of the second pressure transmitters in the direction of the material separation device are sequentially reduced from the extraction generation module.