A preparation device and preparation process of 3-methyl-3-penten-2-one

Abstract

The invention discloses a preparation device and a preparation process of 3-methyl-3-pentene-2-ketone, and relates to the technical field of 3-methyl-3-pentene-2-ketone preparation; the invention comprises a distillation device, the distillation device also comprises a tower body, a liquid collecting component is arranged in the tower body, used for guiding the flow of liquid, a tray component is arranged in the tower body, the liquid collecting component penetrates the tray component, used for increasing the contact time of gas phase and liquid phase, a condensation component is arranged outside the tower body, the condensation component is connected with the liquid collecting component, used for condensing and liquefying the gas phase; the invention can improve the efficiency of gas-liquid separation, and further improve the efficiency and purity of distillation and purification of 3-methyl-3-pentene-2-ketone.

Description

Technical Field

[0001] The invention relates to the technical field of 3-methyl-3-pentene-2-one preparation, and in particular to a preparation device and a preparation process of 3-methyl-3-pentene-2-one. Background Art

[0002] ‌3-Methyl-3-penten-2-one is an organic compound, belonging to pharmaceutical intermediates and other synthetic material intermediates. The synthesis of 3-methyl-3-penten-2-one is a process of aldol condensation reaction between butanone and acetaldehyde in the presence of a concentrated acid catalyst. With acetaldehyde and butanone as raw materials, a condensation reaction is first carried out in a reactor to generate a product, and then butanone and water are separated in a vacuum distillation tower, and then the by-products and 3-methyl-3-penten-2-one are separated by distillation according to different boiling points.

[0003] In the step of separating by-products and 3-methyl-3-pentene-2-one by distillation, the evaporated gas phase, in the process of rising, in the process of contacting with the refluxing liquid phase, generally gradually contacts with the gas phase from top to bottom for heat and mass transfer. Although the contact time of the gas phase and the liquid phase can be increased to a certain extent in this process, the efficiency of separation of the gas phase and the liquid phase is low. At the same time, the liquid phase is easily carried up to the condenser during the rising process of the gas phase, and the condensed refluxed liquid phase is not conducive to improving the heat and mass transfer between the gas phase and the liquid phase, resulting in low efficiency of distillation separation of by-products and 3-methyl-3-pentene-2-one, resulting in low purity of 3-methyl-3-pentene-2-one.

[0004] Therefore, a preparation device and a preparation process of 3-methyl-3-pentene-2-one are invented to solve the above problems. Summary of the invention

[0005] The main purpose of the present invention is to provide a preparation device and a preparation process of 3-methyl-3-pentene-2-one, which can effectively solve the technical problems in the background technology.

[0006] To achieve the above-mentioned purpose, the technical solution adopted by the present invention is: a preparation device for 3-methyl-3-pentene-2-one, including a distillation device, the distillation device also including a tower body, a liquid collecting component is arranged in the tower body, which is used to guide the flow of liquid, a tower plate component is arranged in the tower body, the liquid collecting component runs through the tower plate component, which is used to increase the contact time between the gas phase and the liquid phase, a condensation component is arranged on the outside of the tower body, the condensation component is connected to the liquid collecting component, and is used to condense and liquefy the gas phase; the liquid collecting component includes a liquid collecting plate located inside the tower body and fixedly connected to the tower body, the lower end of the liquid collecting plate is fixedly connected to a vertically extending guide pipe, and the lower end of the guide pipe is fixedly connected to at least two branch pipes connected to the interior thereof.

[0007] Preferably, the liquid collecting plate is in a conical shape, and the diameter of the liquid collecting plate at one end close to the guide tube is smaller than the diameter of the liquid collecting plate at one end away from the guide tube.

[0008] Preferably, a plurality of first air outlet holes which are circumferentially spaced and connected to each other are formed on a side of the liquid collecting plate away from the guide tube.

[0009] Preferably, the tower plate assembly comprises a plurality of support plates fixedly connected to the tower body and distributed vertically, the guide pipe passes through the plurality of support plates in sequence, and each of the support plates is semicircular.

[0010] Preferably, each of the support plates is provided with a through second air outlet hole, and each of the support plates is fixedly connected with a plurality of bubble caps corresponding to and communicating with the second air outlet holes.

[0011] Preferably, two adjacent support plates are symmetrically distributed, and an overflow plate is provided at one end of each support plate that is not in contact with the inner wall of the tower body. Both ends of each overflow plate are in close contact with the inner wall of the tower body, and the upper end of each overflow plate is higher than the upper end of the corresponding support plate.

[0012] Preferably, the condensation assembly includes a condenser located above the tower body, wherein one end of the condenser close to the tower body is connected to the upper end of the tower body through an air inlet pipe, and the side of the condenser away from the tower body is connected to the upper side of the guide pipe through a reflux pipe.

[0013] Preferably, a spiral heating pipe located below the tower plate assembly is provided at the inner bottom of the tower body, a temperature gauge is provided on the outer side of the tower body, and a liquid level measuring device is connected to the outer side of the tower body.

[0014] Preferably, the upper end of the tower body is fixedly connected with a liquid inlet pipe communicating with the interior thereof, and the lower end of the tower body is fixedly connected with a liquid discharge pipe communicating with the interior thereof.

[0015] A preparation process of 3-methyl-3-pentene-2-one comprises the following steps:

[0016] S1. Aldol condensation reaction: butanone, process water and concentrated sulfuric acid are heated in a reaction kettle, and then acetaldehyde is added to carry out an aldol condensation reaction;

[0017] S2. Neutralization and washing: The material after the aldol condensation reaction is collected by washing kettle, followed by neutralization and washing with NaOH solution, and then standing and stratifying to remove wastewater and waste acid;

[0018] S3. Recovery of butanone: using a distillation tower to carry out vacuum distillation of the neutralized and washed material to recover butanone;

[0019] S4. Pre-distillation storage: the material after vacuum distillation is pre-distilled and stored in a supporting storage tank;

[0020] S5. Distillation separation: Inject the material in S4 into the distillation device for distillation separation to obtain the product, then store the material after distillation in the matching storage tank, and discharge the distillation residue at the same time.

[0021] Technical effects and advantages of the present invention:

[0022] 1. The present invention arranges a plurality of support plates at intervals, and under the action of the overflow plate and the bubble cap, it can ensure that there is a certain liquid phase on the support plate, so that during the rising process of the gas phase, it can better contact with the liquid phase on the support plate for heat and mass transfer, and better separate the gas phase and the liquid phase, thereby improving the efficiency of distillation separation and purification.

[0023] 2. In the process of the refluxed liquid phase flowing into the tower body through the guide pipe in the present invention, the liquid phase transfers its temperature to the guide pipe, and the temperature on the guide pipe can be transferred to the rising gas phase, so that the heavy components in the gas phase are liquefied and fall on the support plate, and the support plate is ensured to have a liquid phase, which is convenient for the gas phase and the liquid phase to fully contact and separate. When the gas phase rises to the position of the liquid collecting plate and rises along the first air outlet at the edge thereof, not only can the liquid phase carried by the gas phase fall on the support plate under the action of its own gravity, but also can make the liquid phase fall by itself under the action of the liquid collecting plate, and at the same time avoid the gas phase driving the liquid phase to rise into the condenser. Under the synergistic action of the tower plate assembly, the liquid collecting plate and the guide pipe, not only can the gas phase and the liquid phase be fully contacted for mass transfer and heat transfer, but also the efficiency of mass transfer and heat transfer between the gas phase and the liquid phase can be improved, and at the same time, a large amount of liquid phase can be avoided from being carried up by the gas phase, thereby improving the efficiency of gas-liquid separation, and further improving the efficiency and purity of the distillation and purification of 3-methyl-3-penten-2-one. BRIEF DESCRIPTION OF THE DRAWINGS

[0024] Figure 1 It is a three-dimensional schematic diagram of the distillation device in the present invention;

[0025] Figure 2 It is a schematic diagram of the cutaway structure of the distillation device in the present invention;

[0026] Figure 3 It is a schematic diagram of the structure of the tray assembly and the liquid collecting assembly in the present invention;

[0027] Figure 4 It is a schematic diagram of the structure of the liquid collecting component in the present invention;

[0028] Figure 5 It is a structural schematic diagram of the tower plate assembly in the present invention;

[0029] Figure 6 It is a structural schematic diagram of the support plate in the present invention;

[0030] Figure 7 It is a process flow chart of the present invention.

[0031] In the figure: 1. reactor; 2. washing kettle; 3. distillation tower; 4. supporting storage tank; 5. distillation device; 51. tower body; 52. liquid collecting assembly; 521. liquid collecting plate; 522. guide pipe; 523. branch pipe; 524. first air outlet; 53. tower plate assembly; 531. support plate; 532. second air outlet; 533. bubble cap; 534. overflow plate; 54. condensation assembly; 541. condenser; 542. air inlet pipe; 543. reflux pipe; 55. heating pipe; 56. thermometer; 57. liquid level measuring device; 58. liquid inlet pipe; 59. liquid discharge pipe. DETAILED DESCRIPTION

[0032] 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 described embodiments 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 creative work are within the scope of protection of the present invention.

[0033] When the crude 3-methyl-3-pentene-2-one is distilled and purified, the crude 3-methyl-3-pentene-2-one needs to be heated to gasify it, and then the gas phase is condensed into a liquid phase. In this process, the gas phase and the liquid phase are in contact with each other for sufficient distillation. However, the contact time between the gas phase and the liquid phase is currently short, resulting in low heat and mass transfer efficiency between the gas phase and the liquid phase. This embodiment is specially invented to solve the above problem.

[0034] like Figure 1-Figure 3 As shown, a preparation device of 3-methyl-3-pentene-2-one according to an embodiment of the present invention comprises a distillation device 5, the distillation device 5 further comprises a tower body 51, a tower plate assembly 53 is arranged in the tower body 51, a liquid collecting assembly 52 penetrates the tower plate assembly 53, and is used to increase the contact time of the gas phase and the liquid phase, the tower plate assembly 53 comprises a plurality of support plates 531 fixedly connected to the tower body 51 and vertically distributed, a guide pipe 522 sequentially penetrates the plurality of support plates 531, each support plate 531 is semicircular, and each The support plates 531 are each provided with a through second air outlet hole 532, and each support plate 531 is fixedly connected with a plurality of blisters 533 corresponding to and connected to the second air outlet holes 532, and two adjacent support plates 531 are symmetrically distributed, and an overflow plate 534 is provided at one end of each support plate 531 that is not in contact with the tower body 51, and both ends of each overflow plate 534 are in close contact with the inner wall of the tower body 51, and the upper end of each overflow plate 534 is higher than the upper end of the corresponding support plate 531.

[0035] A spiral heating tube 55 is provided at the bottom of the tower body 51 and is located below the tower plate assembly 53. A thermometer 56 is provided on the outside of the tower body 51. A liquid level measuring device 57 is connected to the outside of the tower body 51. A liquid inlet pipe 58 connected to the interior of the tower body 51 is fixedly connected to the upper end of the tower body 51. A liquid discharge pipe 59 connected to the interior of the tower body 51 is fixedly connected to the lower end of the tower body 51.

[0036] During use, the crude 3-methyl-3-pentene-2-one gradually flows from the top of the tower body 51 to the bottom of the tower body 51 through the liquid inlet pipe 58 and the tower plate assembly 53, and a part of the liquid phase remains between the support plate 531 and the overflow plate 534. Under the action of the heating tube 55 at the bottom of the tower body 51, the heating tube 55 heats the crude 3-methyl-3-pentene-2-one to convert it into a gas phase. At this time, the gas phase moves upward along the tower body 51. When the gas phase contacts the lower end surface of the support plate 531 and under the action of the continuously rising gas phase, very little liquid phase remains from the bubble cap 533 and the second gas outlet 532. The gas phase continues to rise from the second gas outlet 532, and under the action of the bubble cap 533, The gas phase cannot rise from the second gas outlet 532 to the adjacent support plate 531, so that the gas phase can flow out from the side of the bubble cap 533. At this time, the gas phase can fully contact with the liquid phase for heat and mass transfer, so that the heavy components in the gas phase are liquefied into liquid phase, and the light components in the liquid phase are vaporized and continue to rise with the gas phase. In addition, under the setting of the multi-layer support plate 531, the gas phase and the liquid phase can be fully in contact with each other for a long time, which can improve the efficiency and purity of distillation separation and purification. It should be noted that a liquid level meter 57 and a thermometer 56 are provided on the tower body 51, which can accurately control the water level and temperature of the liquid phase in the tower body 51, so as to facilitate better distillation and separation work.

[0037] Among them, multiple support plates 531 are arranged at intervals, and under the action of the overflow plate 534 and the bubble cap 533, it is possible to ensure that there is a certain liquid phase on the support plate 531, so that during the rising process of the gas phase, it can better contact with the liquid phase on the support plate 531 for heat and mass transfer, and better separate the gas phase and liquid phase, thereby improving the efficiency of distillation separation and purification.

[0038] In the process of fully contacting and separating the gas phase and the liquid phase through the tower plate assembly 53, the gas phase easily drives the liquid phase to rise, resulting in insufficient contact between the liquid phase and the gas phase. At the same time, the liquefaction efficiency of the heavy components in the gas phase is not high. Therefore, further improvements are made based on the above-mentioned embodiments.

[0039] like Figure 2-Figure 6As shown, a liquid collecting assembly 52 is provided in the tower body 51 for guiding the flow of liquid. The liquid collecting assembly 52 includes a liquid collecting plate 521 located inside the tower body 51 and fixedly connected to the tower body 51. A vertically extending guide tube 522 is fixedly connected to the lower end of the liquid collecting plate 521. At least two branch tubes 523 connected to the interior of the guide tube 522 are fixedly connected to the lower end of the guide tube 522. The liquid collecting plate 521 is conical in shape. The diameter of the end of the liquid collecting plate 521 close to the guide tube 522 is smaller than the diameter of the end away from the guide tube 522. A plurality of circumferentially spaced and through-going first air outlet holes 524 are provided on the side of the liquid collecting plate 521 away from the guide tube 522.

[0040] A condensation assembly 54 is provided on the outside of the tower body 51, and the condensation assembly 54 is connected to the liquid collecting assembly 52 for condensing and cooling the gas phase. The condensation assembly 54 includes a condenser 541 located above the tower body 51, and one end of the condenser 541 close to the tower body 51 is connected to the upper end of the tower body 51 through an air inlet pipe 542, and the side of the condenser 541 away from the tower body 51 is connected to the upper side of the guide pipe 522 through a reflux pipe 543.

[0041] When the gas phase flows into the condenser 541 through the air inlet pipe 542, the gas phase is liquefied into a liquid phase again under the action of the condenser 541. At this time, the liquid phase in the condenser 541 flows into the guide pipe 522 through the reflux pipe 543. At this time, the liquid phase transfers the temperature to the guide pipe 522, so that the continuously rising gas phase contacts the tube wall of the guide pipe 522 for mass transfer and heat transfer, so that the heavy components in the gas phase are liquefied and fall on the support plate 531, ensuring the presence of the liquid phase on the support plate 531, and also increasing the contact time between the gas phase and the liquid phase, which is convenient for distillation separation, and the refluxed liquid phase is injected into the tower body 51 again through the guide pipe 522 and the branch pipe 523. It should be noted that the branch pipe 523 is inclined and arranged obliquely downward, and the lower end of the guide pipe 522 is in a sealed state, which can effectively prevent the gas phase from rising directly along the guide pipe 522. The liquid phase in the guide pipe 522 cannot flow normally into the tower body 51 under the action of the gas phase.

[0042] When the gas phase rises to contact the lower end of the liquid collecting plate 521, since the liquid collecting plate 521 is a cone with a larger top and a smaller bottom, the gas phase close to the axis of the guide tube 522 first contacts the side wall of the liquid collecting plate 521, causing the gas phase to rise obliquely along the side wall of the liquid collecting plate 521, and at the same time, the liquid phase carried by the gas phase moves downward along the side wall of the liquid collecting plate 521. Since the distance between the gas phase far away from the axis of the guide tube 522 and the liquid collecting plate 521 is slightly larger, after contacting the side wall of the liquid collecting plate 521, the liquid phase carried by the gas phase will fall under the action of its own gravity, and then The gas phase rises to the top of the liquid collecting plate 521 through the first gas outlet hole 524, and the first gas outlet holes 524 are all located at the edge of the liquid collecting plate 521. At the same time, the liquid phase injected from the liquid inlet pipe 58 can flow better from the liquid collecting plate 521 into the guide pipe 522, which also avoids the gas phase carrying a large amount of liquid phase during the rising process. Repeating the above movement can effectively improve the efficiency of distillation, separation and purification. When the distillation is completed, the waste liquid in the tower body 51 is discharged to the outside for treatment through the drain pipe 59.

[0043] In the process of the refluxed liquid phase flowing into the tower body 51 through the guide pipe 522, the liquid phase transfers the temperature to the guide pipe 522, and the temperature on the guide pipe 522 can be transferred to the rising gas phase, so that the heavy components in the gas phase are liquefied and fall on the support plate 531, and the support plate 531 is ensured to have a liquid phase, which is convenient for the gas phase and the liquid phase to fully contact and separate. When the gas phase rises to the position of the liquid collecting plate 521, the liquid phase carried by the gas phase falls on the support plate 531 under the action of its own gravity, avoiding the gas phase driving the liquid phase to rise into the condenser 541. Under the synergistic effect of the tower plate assembly 53, the liquid collecting plate 521 and the guide pipe 522, not only can the gas phase and the liquid phase be fully contacted and transferred, but also the efficiency of the gas phase and the liquid phase can be improved. At the same time, it is also avoided that a large amount of liquid phase is carried up by the gas phase, thereby improving the efficiency of gas-liquid separation, and further improving the efficiency and purity of the distillation and purification of 3-methyl-3-penten-2-one.

[0044] On the basis of the above embodiments, this embodiment also provides a preparation process of 3-methyl-3-pentene-2-one, such as Figure 7 As shown, the following steps are included:

[0045] S1. Aldol condensation reaction: using reactor 1 to heat butanone, process water and 90% sulfuric acid, and then adding acetaldehyde to carry out aldol condensation reaction, mainly heating butanone, process water and 90% sulfuric acid to 50 degrees, and then adding acetaldehyde to carry out aldol condensation reaction to prepare a crude product of 3-methyl-3-penten-2-one;

[0046] S2. Neutralization and washing: The material after the aldol condensation reaction is collected by washing tank 2, and then a NaOH solution is added for neutralization and washing, and then the waste water and waste acid are removed by standing and stratifying, mainly by adding a 30% NaOH solution to the crude product of 3-methyl-3-pentene-2-one for neutralization and washing, and then standing and stratifying to remove the waste water and waste acid;

[0047] S3. Recovery of butanone: Using a distillation column 3 to carry out vacuum distillation of the neutralized and washed material to recover butanone, mainly by distilling the crude 3-methyl-3-pentene-2-one under vacuum distillation, and finally separating butanone for recovery;

[0048] S4. Pre-distillation storage: The material after vacuum distillation is stored in the supporting storage tank 4;

[0049] S5. Distillation separation: The material in S4 is injected into the distillation device 5 for distillation separation to obtain the product, and then the material after distillation is stored in the supporting storage tank 4, and the distillation residue is discharged.

[0050] The above shows and describes the basic principles and main features of the present invention and the advantages of the present invention. It should be understood by those skilled in the art that the present invention is not limited to the above embodiments. The above embodiments and descriptions are only for explaining the principles of the present invention. Without departing from the spirit and scope of the present invention, the present invention may have various changes and improvements, which fall within the scope of the present invention to be protected. The scope of protection of the present invention is defined by the attached claims and their equivalents.

Claims

1. A preparation device for 3-methyl-3-penten-2-one, comprising a distillation device (5), characterized in that: The distillation device (5) further comprises a tower body (51), wherein a liquid collecting component (52) is arranged in the tower body (51) for guiding the flow of liquid, wherein a tray component (53) is arranged in the tower body (51), wherein the liquid collecting component (52) penetrates the tray component (53) for increasing the contact time between the gas phase and the liquid phase, and wherein a condensing component (54) is arranged outside the tower body (51), wherein the condensing component (54) is connected to the liquid collecting component (52) for condensing and liquefying the gas phase; The liquid collecting assembly (52) comprises a liquid collecting plate (521) located inside the tower body (51) and fixedly connected to the tower body (51); a vertically extending guide tube (522) is fixedly connected to the lower end of the liquid collecting plate (521); at least two branch tubes (523) communicating with the interior of the liquid collecting plate (522) are fixedly connected to the lower end of the guide tube (522); the liquid collecting plate (521) is in a conical shape; the diameter of the end of the liquid collecting plate (521) close to the guide tube (522) is smaller than the diameter of the end of the liquid collecting plate (521) away from the guide tube (522); the branch tubes (523) are inclined and arranged obliquely downward, and the lower end of the guide tube (522) is in a sealed state; A plurality of first air outlet holes (524) which are distributed at intervals in the circumferential direction and are connected to each other are formed on a side of the liquid collecting plate (521) away from the guide tube (522); The tower plate assembly (53) comprises a plurality of support plates (531) fixedly connected to the tower body (51) and distributed vertically, the guide pipe (522) sequentially passes through the plurality of support plates (531), and each of the support plates (531) is semicircular; Each of the support plates (531) is provided with a through second air outlet hole (532), and each of the support plates (531) is fixedly connected with a plurality of bubble caps (533) corresponding to and in communication with the second air outlet holes (532); Two adjacent support plates (531) are symmetrically distributed, and an overflow plate (534) is provided at one end of each support plate (531) that is not in contact with the inner wall of the tower body (51), and both ends of each overflow plate (534) are in close contact with the inner wall of the tower body (51), and the upper end of each overflow plate (534) is higher than the upper end of the corresponding support plate (531); The condensation assembly (54) comprises a condenser (541) located above the tower body (51); an end of the condenser (541) close to the tower body (51) is connected to the upper end of the tower body (51) via an air inlet pipe (542); and a side of the condenser (541) away from the tower body (51) is connected to the upper side of the guide pipe (522) via a reflux pipe (543); When the refluxed liquid phase flows into the tower body (51) through the guide pipe (522), the liquid phase transfers its temperature to the guide pipe (522), and the temperature on the guide pipe (522) can be transferred to the rising gas phase, so that the heavy components in the gas phase are liquefied and fall onto the support plate (531).

2. The preparation equipment of 3-methyl-3-penten-2-one according to claim 1, characterized in that: A spiral heating pipe (55) is provided at the bottom of the tower body (51) and is located below the tower plate assembly (53). A temperature gauge (56) is provided on the outside of the tower body (51). A liquid level measuring device (57) is connected to the outside of the tower body (51).

3. The preparation equipment of 3-methyl-3-penten-2-one according to claim 2, characterized in that: The upper end of the tower body (51) is fixedly connected to a liquid inlet pipe (58) communicating with the interior thereof, and the lower end of the tower body (51) is fixedly connected to a liquid discharge pipe (59) communicating with the interior thereof.

4. A process for preparing 3-methyl-3-penten-2-one, using the preparation equipment for 3-methyl-3-penten-2-one according to claim 3, characterized in that: The following steps are involved: S1. Aldol condensation reaction: using a reaction vessel (1) to heat butanone, process water and concentrated sulfuric acid, and then adding acetaldehyde to carry out an aldol condensation reaction; S2. Neutralization and washing: The material after the aldol condensation reaction is collected by a washing kettle (2), followed by neutralization and washing with NaOH solution, and then allowed to stand for stratification to remove waste water and waste acid; S3. Recovery of butanone: using a distillation tower (3) to carry out vacuum distillation of the neutralized and washed material to recover butanone; S4. Pre-distillation storage: the material after vacuum distillation is stored in a supporting storage tank (4); S5. Distillation separation: The material in S4 is injected into the distillation device (5) for distillation separation to obtain a product, and then the distilled material is stored in a matching storage tank (4), and the distillation residue is discharged.

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