Novel two-section type extraction and purification equipment of MMA device

Abstract

The utility model relates to the technical field of chemical equipment, in particular to novel two-section type extraction and purification equipment of an MMA (Methyl Methacrylate) device. Comprising an efficient mixing extraction tank, a jet mixer, a coarse MMA feeding line, an extraction water nozzle, an MMA extraction liquid upper overflow pipe, an extraction water lower overflow pipe, a purification extraction tower, a desalted water inlet pipe and a packed tray, the jet mixer is arranged at the upper part of the interior of the efficient mixing and extracting tank, and a certain distance is kept between the jet mixer and the inner side wall of the efficient mixing and extracting tank; the jet mixer comprises an expansion part arranged on the upper portion and a mixing part arranged on the lower portion, the expansion part and the mixing part are both of a horn-shaped structure, the small opening end of the expansion part and the small opening end of the mixing part are communicated to form an integrated structure, and the diameter of the large opening end of the expansion part is larger than that of the large opening end of the mixing part; according to the utility model, the high-efficiency extraction process is ensured, so that the overall extraction efficiency is improved, and the purity and the quality of a final product are also ensured.

Description

Technical Field

[0001] The utility model relates to the technical field of chemical equipment, in particular to a novel two-stage extraction and purification equipment for an MMA device. Background Art

[0002] In the acetone cyanohydrin process for producing MMA (methyl methacrylate), acetone cyanohydrin (ACH) first reacts with 100% sulfuric acid in an amidation reactor to produce methacrylamide sulfate. This step is a key starting reaction in the entire production process, providing essential intermediates for subsequent steps.

[0003] The methacrylamide sulfate is then fed into the first esterification reactor, where it undergoes an exothermic hydrolysis reaction. During this process, the methacrylamide sulfate decomposes into methacrylic acid and ammonium bisulfate. Methacrylic acid, as an important organic acid, is the direct raw material for the subsequent esterification reaction.

[0004] Next, methacrylic acid undergoes an esterification reaction with methanol under the catalysis of sulfuric acid. This reaction is the core step in the production of methyl methacrylate (MMA), and the esterification reaction produces MMA and water.

[0005] The crude MMA (approximately 65-70% concentration) obtained from the esterification reactor is then fed into an extraction column for extraction. Desalted water is used as the extractant in this column. Since methanol is miscible with water, while methyl methacrylate (MMA) has a low solubility in water, extraction effectively separates MMA from water. Furthermore, since methyl methacrylate has a lower specific gravity than the aqueous phase, after separation, MMA is in the upper layer, while the aqueous phase is in the lower layer, achieving the desired separation.

[0006] After extraction, the crude organic phase, containing 87-93% (operationally, a concentration of ≥90%) MMA, is sent to the refining process for further purification. The aqueous phase is recycled back to the esterification reactor to recover methanol and provide preliminary purification and separation of methyl methacrylate.

[0007] In order to achieve better extraction results, the extraction equipment needs to meet the following two conditions: first, the extractant and the extraction material need to be mixed vigorously and evenly; second, the static slow separation time of the extraction mixture needs to be prolonged as much as possible to achieve better separation effects. However, since the extraction process is continuous, the above two requirements form a contradictory relationship for the existing technology. It is difficult to solve the problem of intense and uniform mixing and static separation without interfering with each other in the same equipment. In addition, the existing crude MMA extraction generally adopts overflow tank extraction or extraction tower, which occupies a relatively large space, the extraction mixing is not sufficient, the extraction operation flexibility is small, and it is very easy to have incomplete separation, resulting in the phenomenon of MMA carrying water after extraction; and water and MMA are very easy to form azeotropic phenomena, which will seriously affect the normal operation of the subsequent distillation tower. Utility Model Content

[0008] The utility model provides a novel two-stage extraction and purification equipment for an MMA device, which aims to achieve intense and uniform mixing of an extractant and a feed liquid through a first-stage jet mixing co-current flow extraction and a second-stage countercurrent extraction, utilizes a jet mixing chamber to achieve intense and uniform mixing of an extractant and a feed liquid, and extends the residence time and separation time of the MMA in water through a trumpet-shaped inverted expansion chamber as a clarification chamber and the co-directional downward movement of the MMA and the extraction water, thereby solving the problem of mutual interference between intense and uniform mixing and static separation in the prior art, and further solving the problem of incomplete extraction and separation and a large amount of water in the MMA after extraction.

[0009] In order to achieve the above purpose, the technical solution of the utility model is:

[0010] The utility model provides a novel two-stage extraction and purification equipment for an MMA device, comprising a high-efficiency mixed extraction tank, a jet mixer, a crude MMA feed line, an extraction water nozzle, an MMA extract upper overflow pipe, an extraction water underwater overflow pipe, a purification extraction tower, a desalted water inlet pipe and a packing tray;

[0011] The jet mixer is arranged above the interior of the high-efficiency mixing and extraction tank and maintains a certain distance from the inner side wall of the high-efficiency mixing and extraction tank; the jet mixer includes an expansion portion arranged above and a mixing portion arranged below, the expansion portion and the mixing portion are both trumpet-shaped structures, the small end of the expansion portion is connected to the small end of the mixing portion to form an integrated structure, and the large end of the expansion portion has a larger diameter than the large end of the mixing portion;

[0012] The outlet end of the crude MMA feed line is arranged near the small mouth end of the mixing section; the extraction water nozzle is arranged along the axis of the mixing section, and the outlet end of the extraction water nozzle is arranged near the middle of the mixing section and below the outlet end of the crude MMA feed line;

[0013] The highest point of the purification and extraction tower is connected to an MMA extract overflow pipe, the packing tray is arranged in the upper inner half of the purification and extraction tower, and the outlet end of the desalted water inlet pipe is arranged inside the purification and extraction tower and above the packing tray;

[0014] One end of the MMA extract upper overflow pipe is connected to the high-efficiency mixed extraction tank, and the other end is connected to the purification extraction tower; the axis of the MMA extract upper overflow pipe is located below the jet mixer and the packed tower tray; one end of the extraction underwater overflow pipe is connected to the high-efficiency mixed extraction tank, and the other end is connected to the purification extraction tower; the extraction underwater overflow pipe is arranged below the MMA extract upper overflow pipe;

[0015] The lowest point of the purification extraction tower is connected to an extraction water circulation pipe, the other end of the extraction water circulation pipe is connected to an extraction water circulation pump, and the outlet end of the extraction water circulation pump is connected to the inlet end of the extraction water nozzle.

[0016] Furthermore, the lowest point of the high-efficiency mixed extraction tank is connected to an extraction water discharge pipe.

[0017] Furthermore, the ratio of the area of ​​the large end of the expansion portion to the area of ​​the horizontal cross section at the same height of the high-efficiency mixed extraction tank is

[0018] Furthermore, the ratio of the horizontal cross-sectional area of ​​the mixing portion at the height of the extraction water nozzle outlet end to the horizontal cross-sectional area of ​​the high-efficiency mixing extraction tank at the same height is

[0019] Furthermore, a level meter is provided on the purification and extraction tower.

[0020] The beneficial effects achieved by the utility model are:

[0021] The utility model includes a high-efficiency mixed extraction tank, a jet mixer, a mixing chamber, a clarification chamber, and a purification extraction tower. Through this innovative MMA device, the extractant (specifically, a mixture of water and methanol solution) and the MMA liquid are fully mixed through a jetting process, ensuring the efficient extraction process and thus improving the overall extraction efficiency. After the extraction water and the MMA liquid are mixed, they flow in the same direction under laminar conditions for static separation. This design extends the mass transfer time and further improves the separation effect. This optimization not only facilitates subsequent distillation operations but also ensures the purity and quality of the final product.

[0022] The separated solutes are then further processed and separated by reverse extraction using an extractant, thereby obtaining MMA with higher purity. This design not only optimizes the extraction and purification process, but also brings significant improvements in results:

[0023] In addition, compared with traditional extraction equipment, the equipment design of this patent is more compact and the volume can be reduced by about 20-30%, which not only saves space but also reduces equipment costs and maintenance difficulty. BRIEF DESCRIPTION OF THE DRAWINGS

[0024] In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the following briefly introduces the drawings required for use in the embodiments or the description of the prior art. Obviously, the drawings described below are only some embodiments of the present invention. For ordinary technicians in this field, other drawings can be obtained based on the structures shown in these drawings without paying any creative work.

[0025] Figure 1 It is a schematic diagram of the overall structure of the utility model.

[0026] Figure 2 This is a simplified diagram of the liquid flow of the jet mixer of the present invention.

[0027] Figure 3 This is a partial enlarged view of the high-efficiency mixed extraction tank of the utility model.

[0028] Figure 4 yes Figure 3 Middle AA cross-section.

[0029] Figure 5 yes Figure 3 Middle BB cross-section.

[0030] In the figure, 1. High-efficiency mixing extraction tank; 11. Jet mixer; 111. Crude MMA feed line; 112. Extraction water nozzle; 12. Mixing chamber; 13. Clarification chamber; 14. Extraction water discharge pipe; 15. MMA extract upper overflow pipe; 16. Extraction water underwater overflow pipe; 17. Extraction water circulation pump; 2. Purification extraction tower; 21. MMA extract overflow pipe; 22. Level meter; 23. Desalted water inlet pipe; 24. Packing tray; 25. Extraction water circulation pipe. DETAILED DESCRIPTION

[0031] The following will be combined with the drawings in the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the embodiments described are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making creative efforts are within the scope of protection of the present invention.

[0032] It should be noted that if the embodiments of the present invention involve directional indications (such as up, down, left, right, front, back, etc.), the directional indications are only used to explain the relative position relationship, movement status, etc. between the various components under a certain specific posture (as shown in the accompanying drawings). If the specific posture changes, the directional indications will also change accordingly.

[0033] In addition, if there are descriptions involving "first", "second", etc. in the embodiments of the present invention, the descriptions of "first", "second", etc. are only for descriptive purposes and cannot be understood as indicating or implying their relative importance or implicitly indicating the number of the indicated technical features. Therefore, the features defined as "first" and "second" may explicitly or implicitly include at least one of such features. In addition, if the meaning of "and / or" appearing in the full text is to include three parallel schemes, taking "A and / or B" as an example, it includes scheme A, or scheme B, or a scheme in which A and B are satisfied at the same time. In addition, the technical solutions between the various embodiments can be combined with each other, but it must be based on the ability of ordinary technicians in this field to implement. When the combination of technical solutions is mutually contradictory or cannot be implemented, it should be deemed that such a combination of technical solutions does not exist and is not within the scope of protection required by the present invention.

[0034] The utility model provides a novel two-stage extraction and purification device for an MMA device, which utilizes a first-stage jet mixing co-current flow mass transfer extraction and a second-stage countercurrent extraction. A jet mixing structure forms a turbulent mixed liquid flow to achieve uniform mixing. The mixed liquid enters a gradually expanding bell-shaped mixing chamber 12 for thorough mixing. Under laminar flow conditions, the MMA and extraction water are further separated by mass transfer in a co-current, stable descent in the clarification chamber 13. This process effectively prolongs the residence time and separation time of the MMA in the water, achieving rapid and uniform mixing and low-speed separation. The extraction effect is then enhanced through a second stage of extraction. The rational combination of the mixer and the clarification chamber 13 achieves a compact, simple, and efficient structure.

[0035] like Figures 1 to 5 As shown, the two-stage extraction and purification equipment includes a high-efficiency mixed extraction tank 1, a jet mixer 11, a crude MMA feed line 111, an extraction water nozzle 112, an MMA extract upper overflow pipe 15, an extraction water underwater overflow pipe 16, a purification extraction tower 2, a desalted water inlet pipe 23 and a packing tray 24.

[0036] The jet mixer 11 is arranged above the interior of the high-efficiency mixing and extraction tank 1 and maintains a certain distance from the inner wall of the high-efficiency mixing and extraction tank 1; the jet mixer 11 includes an expansion portion arranged above and a mixing portion arranged below, and the expansion portion and the mixing portion are both trumpet-shaped structures. The small mouth end of the expansion portion is connected to the small mouth end of the mixing portion to form an integrated structure, and the diameter of the large mouth end of the expansion portion is larger than the diameter of the large mouth end of the mixing portion.

[0037] The inlet end of the crude MMA feed line 111 is connected to the previous process for obtaining crude MMA, and the outlet end of the crude MMA feed line 111 is arranged near the small mouth end of the mixing section; the extraction water nozzle 112 is arranged along the axis of the mixing section, and the outlet end of the extraction water nozzle 112 is arranged near the middle of the mixing section and below the outlet end of the crude MMA feed line 111.

[0038] The lowest point of the high-efficiency mixed extraction tank 1 is connected to an extraction water discharge pipe 14 , and the other end of the extraction water discharge pipe 14 is connected to a recovery system.

[0039] The highest point of the purification and extraction tower 2 is connected to an MMA extract overflow pipe 21, and the other end of the MMA extract overflow pipe 21 is connected to the next MMA processing system; the packed tower tray 24 is arranged in the upper inner half of the purification and extraction tower 2; the inlet end of the desalted water inlet pipe 23 is connected to a water source, and the outlet end is arranged inside the purification and extraction tower 2 and above the packed tower tray 24.

[0040] One end of the MMA extract upper overflow pipe 15 is connected to the high-efficiency mixed extraction tank 1, and the other end is connected to the purification extraction tower 2; the axis of the MMA extract upper overflow pipe 15 is located below the jet mixer 11 and the packing tray 24; one end of the extraction underwater overflow pipe 16 is connected to the high-efficiency mixed extraction tank 1, and the other end is connected to the purification extraction tower 2; the extraction underwater overflow pipe 16 is arranged below the MMA extract upper overflow pipe 15.

[0041] The lowest point of the purification extraction tower 2 is connected to an extraction water circulation pipe 25 , the other end of the extraction water circulation pipe 25 is connected to an extraction water circulation pump 17 , and the outlet end of the extraction water circulation pump 17 is connected to the inlet end of the extraction water nozzle 112 .

[0042] The diameters of the large opening ends of the expansion portion and the mixing portion are both larger than the diameters of their respective small opening ends.

[0043] Among them, the packing tray 24 belongs to the existing technology, and its function is to improve the mass transfer efficiency of the material tower by supporting the packing and separating the fluid. Therefore, the specific principles and technical details are not repeated here.

[0044] The area enclosed by the expanded portion is the mixing chamber 12 , and the area between the inner wall of the high-efficiency mixing extraction tank 1 and the outer wall of the jet mixer 11 is the clarification chamber 13 .

[0045] Further, if Figure 4As shown in the AA section, the ratio of the area of ​​the large end of the expanded portion to the area of ​​the horizontal cross section at the same height of the high-efficiency mixed extraction tank 1 is like Figure 5 As shown in the BB section, the ratio of the horizontal cross-sectional area of ​​the mixing portion at the height of the outlet end of the extraction water nozzle 112 to the horizontal cross-sectional area of ​​the high-efficiency mixing extraction tank 1 at the same height is It is worth noting that the specific values ​​need to be further optimized and adjusted according to differences in working conditions.

[0046] Furthermore, the purification and extraction tower 2 is provided with an interface meter 22, which is arranged above the packing tray 24. The interface meter 22 is a prior art instrument for measuring the liquid level of a known medium, and is particularly suitable for measuring the stratification position of two immiscible liquids.

[0047] Specifically, the workflow of this utility model is:

[0048] The crude MMA to be extracted and separated passes through the crude MMA feed line 111 and the extraction water nozzle 112 in the jet mixer 11. The upward circulating flow of the extraction water sprayed by the extraction water nozzle 112 creates a turbulent flow, so that the crude MMA and the extraction water are fully stirred and mixed in the jet mixer 11.

[0049] Under the force of the jet, the extract mixture flows upward, overcoming gravity. Mixed within mixing chamber 12, the mixture then turns at a low speed and descends into a slowly descending separation phase within the narrow-at-top, wide-at-bottom clarification chamber 13 formed between the high-efficiency mixing and extraction tank 1 and the jet mixer 11. The crude MMA and extract water simultaneously descend slowly, with the water droplets rapidly descending due to gravity and increasing in volume as they absorb more water molecules. Simultaneously, the water and methanol molecules contained in the crude MMA further demulsify and separate from the extract water phase. After separation in clarification chamber 13 between the high-efficiency mixing and extraction tank 1 and the jet mixer 11, the majority of the crude MMA extract phase flows through the MMA extract overflow pipe 15 and enters the purification extraction tower 2. The extract water flows through the extract water bottom overflow pipe 16 and enters the purification extraction tower 2. The remaining extract water and methanol phase exits the system through the extract water discharge pipe 14.

[0050] After the crude MMA and the extraction water are separated in the clarification chamber 13 between the high-efficiency mixing extraction tank 1 and the jet mixer 11 , the crude MMA enters the purification extraction tower 2 through the MMA extract overflow pipe 15 .

[0051] After entering purification extraction column 2, the crude MMA extract continues to rise due to buoyancy, coming into contact with fresh desalted water entering purification extraction column 2 through desalted water inlet pipe 23 on packing trays 24, achieving extraction and purification. The purified MMA then enters the next MMA processing system through MMA extract overflow pipe 21.

[0052] The extraction water from the purification extraction tower 2 enters the jet mixer 11 through the extraction water circulation pipe 25, the extraction water circulation pump 17 and the extraction water nozzle 112 to form an upward turbulent liquid flow.

[0053] Table 1 is a comparison of the composition and consumption of the extraction materials between the prior art and the application of this patent.

[0054]

[0055]

[0056] Table 1

[0057] Among them, for the purpose of this patent, the crude MMA in Table 1 refers to the material at the crude MMA feed line 11, the crude MMA organic phase refers to the material at the MMA extract overflow pipe 21, and the extraction water phase group refers to the material at the extraction water discharge pipe 14.

[0058] As can be seen in Table 1, after applying this patent, while the composition of the crude MMA material obtained from the esterification reactor remains similar, the proportions of water and methanol in the crude MMA organic phase and the proportion of MMA in the extracted aqueous phase both decrease significantly. This demonstrates that this patent enhances the extraction and separation effect, achieving a more thorough crude separation of MMA from water and methanol. The significantly thinner thickness of the interlayer at the interface between MMA and the aqueous phase in purification extraction column 2 further confirms the improved extraction effect.

[0059] The above description is merely an optional embodiment of the present invention and does not limit the patent scope of the present invention. All equivalent structural transformations made by utilizing the contents of the present invention specification and drawings under the inventive concept of the present invention, or direct / indirect application in other related technical fields are included in the patent protection scope of the present invention.

Claims

1. A novel two-stage extraction and purification equipment for an MMA device, characterized by: The invention comprises a high-efficiency mixed extraction tank (1), a jet mixer (11), a crude MMA feed line (111), an extraction water nozzle (112), an MMA extract upper overflow pipe (15), an extraction water lower overflow pipe (16), a purification extraction tower (2), a desalted water inlet pipe (23) and a packing tower tray (24); The jet mixer (11) is arranged above the interior of the high-efficiency mixing and extraction tank (1) and maintains a certain distance from the inner wall of the high-efficiency mixing and extraction tank (1); the jet mixer (11) comprises an expansion portion arranged above and a mixing portion arranged below, the expansion portion and the mixing portion both being trumpet-shaped structures, the small end of the expansion portion being connected to the small end of the mixing portion to form an integrated structure, and the large end of the expansion portion having a diameter greater than the large end of the mixing portion; The outlet end of the crude MMA feed line (111) is arranged near the small mouth end of the mixing section; the extraction water nozzle (112) is arranged along the axis of the mixing section, and the outlet end of the extraction water nozzle (112) is arranged near the middle of the mixing section and below the outlet end of the crude MMA feed line (111); The highest point of the purification and extraction tower (2) is connected to an MMA extract overflow pipe (21), the packed tray (24) is arranged in the upper inner half of the purification and extraction tower (2), and the outlet end of the desalted water inlet pipe (23) is arranged inside the purification and extraction tower (2) and above the packed tray (24); One end of the MMA extract upper overflow pipe (15) is connected to the high-efficiency mixed extraction tank (1), and the other end is connected to the purification extraction tower (2); the axis of the MMA extract upper overflow pipe (15) is located below the jet mixer (11) and the packing tray (24); one end of the extraction water underwater overflow pipe (16) is connected to the high-efficiency mixed extraction tank (1), and the other end is connected to the purification extraction tower (2); the extraction water underwater overflow pipe (16) is arranged below the MMA extract upper overflow pipe (15); The lowest point of the purification extraction tower (2) is connected to an extraction water circulation pipe (25), the other end of the extraction water circulation pipe (25) is connected to an extraction water circulation pump (17), and the outlet end of the extraction water circulation pump (17) is connected to the inlet end of the extraction water nozzle (112).

2. The novel two-stage extraction and purification equipment for an MMA device according to claim 1, characterized in that: The lowest point of the high-efficiency mixed extraction tank (1) is connected to an extraction water discharge pipe (14).

3. The novel two-stage extraction and purification equipment for an MMA device according to claim 1, characterized in that: The ratio of the area of ​​the large opening end of the expansion portion to the area of ​​the horizontal cross section at the same height of the high-efficiency mixed extraction tank (1) is 4. The novel two-stage extraction and purification equipment for an MMA device according to claim 1, characterized in that: The ratio of the horizontal cross-sectional area of ​​the mixing portion at the height of the outlet end of the extraction water nozzle (112) to the horizontal cross-sectional area of ​​the high-efficiency mixing extraction tank (1) at the same height is 5. The novel two-stage extraction and purification equipment for an MMA device according to claim 1, characterized in that: The purification extraction tower (2) is provided with a level meter (22).

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