A hexenone purification device
By combining multi-stage distillation units and precision filters with vacuum pump negative pressure dehydration, the problem of existing equipment being unable to effectively remove impurities has been solved, achieving efficient purification of hexenone with a purity of 99.5%.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- LANZHOU FUERSHENG TECH DEV CO LTD
- Filing Date
- 2025-07-17
- Publication Date
- 2026-07-31
AI Technical Summary
Existing hexenone purification equipment is inadequate in terms of separation efficiency, making it difficult to effectively remove impurities with boiling points close to that of hexenone, resulting in a purity of only about 95%, and requiring secondary operations.
The system employs multi-stage distillation units for initial distillation, refining, and stripping, combined with precision filters and 3A molecular sieve packing. It utilizes a vacuum pump for negative pressure dehydration and a sealed structure to improve connection tightness, thereby achieving highly efficient purification.
This method achieves highly efficient purification of hexenone, with a purity of over 99.5%, meeting pharmaceutical-grade requirements. It also simplifies the operation process and improves separation efficiency.
Smart Images
Figure CN224573244U_ABST
Abstract
Description
Technical Field
[0001] This utility model relates to the field of organic chemical product purification technology, and in particular to a hexenone purification device. Background Technology
[0002] Hexenone is an important organic synthesis intermediate widely used in pharmaceuticals, pesticides, and fragrances. However, the preparation of hexenone is accompanied by impurities such as acetic acid, ketene, water, and high-boiling-point polymers, the presence of which can seriously affect the quality of downstream products.
[0003] Existing hexenone purification equipment has many problems. In terms of separation efficiency, traditional distillation columns only use a single distillation section for separation, which makes it difficult to effectively remove impurities with boiling points close to that of hexenone. The removal effect is poor, resulting in a hexenone purity that can usually only reach about 95%. Secondary operations are required, which is time-consuming and labor-intensive. Therefore, an improved and upgraded hexenone purification equipment is proposed. Utility Model Content
[0004] The purpose of this section is to outline some aspects of embodiments of the present invention and to briefly describe some preferred embodiments. Simplifications or omissions may be made in this section, as well as in the abstract and title of the present invention, to avoid obscuring the purpose of these documents, and such simplifications or omissions should not be construed as limiting the scope of the present invention.
[0005] Therefore, the purpose of this invention is to provide a hexenone purification device that can solve the technical problem that existing traditional distillation columns, which rely solely on a single distillation section for separation, are unable to effectively remove impurities with boiling points close to that of hexenone.
[0006] To solve the above-mentioned technical problems, this utility model provides a hexenone purification device, which adopts the following technical solution: It includes a support frame, a raw material storage tank is fixedly installed on the upper end of the support frame, a connecting pipe is fixedly installed at the bottom of the raw material storage tank and one end of the connecting pipe is fixedly installed inside a dehydration tower, a filter is fixedly installed on the outer wall of the connecting pipe, a connecting pipe is fixedly installed on the outer wall of the dehydration tower, a sealing structure is provided at one end of the connecting pipe and a primary distillation tower is provided on one side of the sealing structure, a liquid outlet pipe is fixedly installed at the bottom of the primary distillation tower and one end of the liquid outlet pipe is fixedly connected to the connecting pipe, a refining tower is provided on one side of the primary distillation tower, a stripping tower is provided on one side of the refining tower, a condensation recovery tank is provided on one side of the stripping tower, and a residual liquid pyrolysis vessel is provided on one side of the condensation recovery tank.
[0007] Optionally, a solenoid valve is fixedly installed on the outer wall of the connecting pipe, and a filter element is fixedly installed inside the filter, and the filter adopts a snap-fit structure.
[0008] Optionally, a vacuum pump is fixedly installed at the upper end of the dehydration tower and connected to a connecting pipe, and a liquid level sensor is fixedly installed at the bottom of the dehydration tower.
[0009] Optionally, the sealing structure includes installation conduits, and the number of installation conduits is set to three, with the three installation conduits respectively fixedly installed in the primary distillation column, the refining column, and the stripping column. A sealing disc is fixedly installed at one end of each installation conduit, and a sealing cover is fixedly installed at one end of each connecting pipe.
[0010] Optionally, the sealing disc has a sealing groove inside, a rubber sealing gasket is provided inside the sealing groove, a sealing ring is fitted to the outer wall of the rubber sealing gasket, and the sealing cover is snapped into the sealing groove inside the sealing disc.
[0011] Optionally, positioning holes are provided on both sides of the inner side of the sealing cover, and anti-slip knobs are symmetrically arranged on the outer side of the sealing disc. Sealing screws are fixedly connected to the outer wall of the anti-slip knobs, and the outer walls of the two sealing screws are threadedly connected to the inside of the sealing disc, with their extended ends inserted into the positioning holes.
[0012] In summary, this utility model has at least one of the following beneficial effects: 1. A dehydration tower is connected to the bottom of the raw material storage tank through a connecting pipe. The connecting pipe is equipped with a precision filter with a filter element pore size of 5μm, which is used to remove solid impurities in the raw material. The dehydration tower is filled with 3A molecular sieve packing and has primary distillation, refining and stripping in a multi-stage distillation unit, which achieves efficient purification of hexenone, so that the purity of hexenone can reach more than 99.5%, which meets the requirements of pharmaceutical grade raw materials.
[0013] By connecting the various connecting pipes to the installation conduits on the primary distillation, refining, and stripping columns, and aligning the sealing cover plate on the connecting pipe with the sealing disc, one end of the sealing cover plate squeezes the rubber sealing gasket and sealing ring, thereby achieving a relative seal between the connecting pipe and the installation conduit. Finally, by rotating two anti-slip knobs, the sealing screw is rotated to fix the sealing cover plate inside the sealing disc, facilitating the sealed transport of liquid from the primary distillation column and the dehydration column, preventing leakage, and improving the connection sealing performance. Attached Figure Description
[0014] To more clearly illustrate the technical solutions of the embodiments of this utility model, the accompanying drawings used in the description of the embodiments will be briefly introduced below. Obviously, the drawings described below are only some embodiments of this utility model. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.
[0015] Figure 1 This is a schematic diagram of the overall structure of a hexenone purification device according to the present invention; Figure 2This is a schematic diagram of the rear structure of a hexenone purification device according to the present invention; Figure 3 for Figure 1 A magnified schematic diagram of the local structure; Figure 4 for Figure 2 A magnified diagram of the partially disassembled structure.
[0016] The components represented by each number in the attached diagram are listed below: 1. Support frame; 2. Raw material storage tank; 21. Connecting pipe; 22. Solenoid valve; 3. Dehydration tower; 31. Vacuum pump; 4. Filter; 5. Connecting pipe; 6. Sealing structure; 61. Installation conduit; 62. Sealing disc; 63. Sealing cover plate; 64. Sealing groove; 65. Rubber sealing gasket; 66. Sealing ring; 67. Anti-slip knob; 68. Sealing screw; 69. Positioning hole; 7. Pre-distillation tower; 8. Refining tower; 9. Stripping tower; 10. Condensation recovery tank; 11. Liquid outlet pipe; 12. Residual liquid pyrolysis vessel. Detailed Implementation
[0017] The technical solutions of the present utility model will be clearly and completely described below with reference to the accompanying drawings of the embodiments. Obviously, the described embodiments are only some embodiments of the present utility model, and not all embodiments. Based on the embodiments of the present utility model, all other embodiments obtained by those of ordinary skill in the art without creative effort are within the protection scope of the present utility model.
[0018] The following is in conjunction with the appendix Figure 1 —4. This utility model will be described in further detail.
[0019] Reference Figure 1-4 In this embodiment, in order to solve the problem that existing traditional distillation columns can only separate impurities with a single distillation section and it is difficult to effectively remove impurities with a boiling point close to that of hexenone, this utility model discloses a hexenone purification device. The system includes a support frame 1, a raw material storage tank 2 fixedly installed on the upper end of the support frame 1, a connecting pipe 21 fixedly installed at the bottom of the raw material storage tank 2, one end of the connecting pipe 21 fixedly installed inside the dehydration tower 3, a filter 4 fixedly installed on the outer wall of the connecting pipe 21, a connecting pipe 5 fixedly installed on the outer wall of the dehydration tower 3, a sealing structure 6 installed at one end of the connecting pipe 5, a primary distillation tower 7 installed on one side of the sealing structure 6, a liquid outlet pipe 11 fixedly installed at the bottom of the primary distillation tower 7, a connecting pipe 5 fixedly connected at one end of the liquid outlet pipe 11, a refining tower 8 installed on one side of the primary distillation tower 7, a stripping tower 9 installed on one side of the refining tower 8, a condensation recovery tank 10 installed on one side of the stripping tower 9, and a residual liquid cracking vessel 12 installed on one side of the condensation recovery tank 10. Specifically, a solenoid valve 22 is fixedly installed on the outer wall of the connecting pipe 21, and a filter element is fixedly installed inside the filter 4, and the filter 4 adopts a snap-fit structure.
[0020] The raw material is preheated by a jacketed preheating layer on the outer wall of the raw material storage tank 2, and hot water at 80-100℃ is introduced. The bottom of the raw material storage tank 2 is connected to the dehydration tower 3 through a connecting pipe 21. A precision filter 4 with a filter element pore size of 5μm is installed on the connecting pipe 21 to remove solid impurities in the raw material. The dehydration tower 3 is filled with 3A molecular sieve packing. Specifically, a vacuum pump 31 is fixedly installed at the upper end of the dehydration tower 3, and the vacuum pump 31 is connected to the connecting pipe 21. A liquid level sensor is fixedly installed at the bottom of the dehydration tower 3.
[0021] A vacuum pump 31 is connected to the top of the tower, with a vacuum degree of 0.08MPa. The moisture content of the raw material is reduced to below 0.1% by negative pressure dehydration. A first liquid level sensor is installed at the bottom of the dehydration tower 3. The first liquid level sensor is linked with the feed valve of the raw material storage tank 2 to realize automatic feeding. The primary distillation tower 7, the refining tower 8 and the stripping tower 9 are connected in sequence and connected by a connecting pipe 5 and a liquid outlet pipe 11. A control valve is installed on the outer wall of the connecting pipe 5. Specifically, the sealing structure 6 includes an installation conduit 61, and there are three installation conduits 61. The three installation conduits 61 are respectively fixedly installed in the primary distillation column 7, the refining column 8, and the stripping column 9. A sealing plate 62 is fixedly installed at one end of the installation conduit 61, and a sealing cover plate 63 is fixedly installed at one end of the connecting pipe 5.
[0022] By precisely aligning and fixing the sealing cover plate 63 on the connecting pipe 5 with the sealing disc 62 on the installation conduit 61, the installation of the connecting pipe 5 and the installation conduit 61 becomes relatively stable. Specifically, the sealing disc 62 has a sealing groove 64 inside, a rubber sealing gasket 65 is provided inside the sealing groove 64, a sealing ring 66 is attached to the outer wall of the rubber sealing gasket 65, and a sealing cover plate 63 is snapped into the sealing groove 64 inside the sealing disc 62.
[0023] The sealing cover plate 63 presses the rubber sealing gasket 66 and sealing ring 65 inside the sealing disc 62, thereby promoting a relative seal during connection and splicing to prevent material leakage from affecting use.
[0024] Specifically, the sealing cover plate 63 has positioning holes 69 on both sides inside, and anti-slip knobs 67 are symmetrically arranged on the outer side of the sealing disc 62. The outer wall of the anti-slip knobs 67 is fixedly connected to sealing screws 68. The outer walls of the two sealing screws 68 are threaded to the inside of the sealing disc 62 and the extended ends are inserted into the positioning holes 69.
[0025] The sealing cover plate 63 is fixed inside the sealing disc 62 by two sealing screws 68, which makes it easier for the two to be spliced together more securely and sealed, and improves the stability of the connection.
[0026] The specific working principle is as follows: Crude hexenone is fed into the raw material storage tank 2. The jacketed preheating layer of the raw material storage tank 2 preheats the raw material. The raw material is then transported through the connecting pipe 21 and passes through the filter element in the precision filter 4 to remove solid impurities before entering the dehydration tower 3. The dehydration tower 3 is filled with 3A molecular sieve packing. The vacuum pump 31 connected to the top of the tower controls the vacuum degree at 0.08MPa, performing negative pressure dehydration on the raw material. After dehydration, the moisture content of the raw material is reduced, and then it is transported into the primary distillation tower 7 through the connecting pipe 5. The connecting pipe 5 is connected to the installation conduit 61 on the primary distillation tower 7. During the connection... The sealing cover plate 63 on the connecting pipe 5 is aligned and inserted with the sealing disc 62, so that one end of the sealing cover plate 63 squeezes the rubber sealing gasket 66 and the sealing ring 65, thereby sealing the connection between the connecting pipe 5 and the installation conduit 61. Finally, by rotating the two anti-slip knobs 67, the sealing screw 68 is rotated to fix the sealing cover plate 63 inside the sealing disc 62, which facilitates the sealed transport of liquid from the primary distillation column 7 to the dehydration column 3 and prevents leakage. The dehydrated raw material first enters the primary distillation column 7. The heating temperature of the heat transfer oil heating jacket in the column bottom is controlled at 140℃. The top condenser adopts - A 5℃ ethylene glycol solution is used as the condensing medium to separate low-boiling-point impurities such as ketene. The distillate is sent to the tail gas treatment unit. The material after initial distillation enters the refining tower 8, which uses a 30-layer stepped tray. The top temperature of the tower is controlled at 127℃, and the reflux ratio controller adjusts the reflux ratio to 3:1 to obtain crude hexenone. The crude hexenone enters the stripping tower 9, where the bottom temperature is controlled at 150℃ to remove high-boiling-point polymer impurities. The stripped hexenone vapor enters the condensation recovery tank 10, where it is cooled by an internal primary condenser and a secondary cryocooler. The cooled hexenone enters the finished product storage tank, and the discharge valve is automatically opened. The residual liquid produced by the stripping tower 9 enters the residual liquid cracking vessel 12, which is electrically heated to 200-220℃ to crack the high-boiling-point polymers into small-molecule organic compounds. The cracked material enters the neutralization process.
[0027] It should be noted that, in this document, relational terms such as "first" and "second" are used only to distinguish one entity or operation from another, and do not necessarily require or imply any such actual relationship or order between these entities or operations. Furthermore, the terms "comprising," "including," or any other variations thereof are intended to cover non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements includes not only those elements but also other elements not expressly listed, or elements inherent to such process, method, article, or apparatus.
[0028] Although embodiments of the present invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made to these embodiments without departing from the principles and spirit of the present invention, the scope of which is defined by the appended claims and their equivalents.
Claims
1. A hexenone purification device, comprising a support frame (1), characterized in that: A raw material storage tank (2) is fixedly installed on the upper end of the support frame (1). A connecting pipe (21) is fixedly installed at the bottom of the raw material storage tank (2), and one end of the connecting pipe (21) is fixedly installed inside the dehydration tower (3). A filter (4) is fixedly installed on the outer wall of the connecting pipe (21). A connecting pipe (5) is fixedly installed on the outer wall of the dehydration tower (3). A sealing structure (6) is provided at one end of the connecting pipe (5), and a primary distillation tower (7) is provided on one side of the sealing structure (6). An outlet pipe (11) is fixedly installed at the bottom of the primary distillation tower (7), and one end of the outlet pipe (11) is fixedly connected to the connecting pipe (5). A refining tower (8) is provided on one side of the primary distillation tower (7), a stripping tower (9) is provided on one side of the refining tower (8), a condensation recovery tank (10) is provided on one side of the stripping tower (9), and a residual liquid cracking vessel (12) is provided on one side of the condensation recovery tank (10).
2. The hexenone purification equipment according to claim 1, characterized in that: A solenoid valve (22) is fixedly installed on the outer wall of the connecting pipe (21), and a filter element is fixedly installed inside the filter (4), and the filter (4) adopts a snap-fit structure.
3. The hexenone purification equipment according to claim 2, characterized in that: A vacuum pump (31) is fixedly installed at the upper end of the dehydration tower (3), and the vacuum pump (31) is connected to the connecting pipe (21). A liquid level sensor is fixedly installed at the bottom of the dehydration tower (3).
4. The hexenone purification equipment according to claim 1, characterized in that: The sealing structure (6) includes an installation conduit (61), and there are three installation conduits (61). The three installation conduits (61) are respectively fixedly installed in the primary distillation column (7), the refining column (8) and the stripping column (9). A sealing plate (62) is fixedly installed at one end of the installation conduit (61), and a sealing cover plate (63) is fixedly installed at one end of the connecting pipe (5).
5. The hexenone purification equipment according to claim 4, characterized in that: The sealing disc (62) has a sealing groove (64) inside, and a rubber sealing gasket (65) is provided inside the sealing groove (64). A sealing ring (66) is attached to the outer wall of the rubber sealing gasket (65), and the sealing cover plate (63) is snapped into the sealing groove (64) inside the sealing disc (62).
6. The hexenone purification equipment according to claim 5, characterized in that: The sealing cover (63) has positioning holes (69) on both sides inside. The sealing disc (62) has anti-slip knobs (67) symmetrically arranged on the outside. The outer wall of the anti-slip knob (67) is fixedly connected to a sealing screw (68). The outer walls of the two sealing screws (68) are threaded to the inside of the sealing disc (62) and the extended ends are inserted into the positioning holes (69).