A high-purity terpineol dehydration device

Abstract

The utility model relates to the technical field of terpineol production equipment, especially to a high purity terpineol dehydration device, its technical scheme includes: reaction subassembly and distillation subassembly, is provided with intelligent reflux ratio controller on the reflux pipe, is provided with the phase separation subassembly on the stable base, the phase separation subassembly includes the phase separator, is provided with coalescence filler in the phase separator, is provided with the condensation assembly on the stable base and the side above phase separator, the condensation assembly includes the condenser, the utility model discloses through the setting of reaction subassembly and distillation subassembly coordinated operation has improved the efficiency, selectivity and stability of reaction process significantly, has improved the controllability, stability and separation efficiency of separation process significantly, through the setting of phase separation subassembly and condensation assembly can realize the efficient condensation of gas phase component, guarantees the material balance of distillation subassembly, can control distillation operation pressure simultaneously, guarantees the process stability and security, promotes the efficient operation of subsequent separation process.

Description

Technical Field

[0001] This utility model relates to the technical field of terpineol production equipment, and in particular to a high-purity terpineol dehydration device. Background Technology

[0002] Terpineol, an important fine chemical raw material, is widely used in the fields of fragrance, pharmaceuticals, cosmetics, and surfactants. Its purity directly determines the quality of the end product; for example, high-end fragrances require terpineol purity ≥95%. Industrially, terpineol is mainly prepared through the dehydration reaction of hydrated terpene diols. The core of this process lies in efficient catalytic dehydration and precise separation and purification. The synergistic control of these two aspects is key to improving product purity and reducing energy consumption. Existing terpineol dehydration devices mostly use concentrated sulfuric acid liquid acid as a catalyst or use solid acid catalysts. Although liquid acid can promote the dehydration reaction, it is highly corrosive, while solid acid is prone to insufficient contact with the reaction liquid and rapid activity decay due to agglomeration, resulting in relatively low catalytic system efficiency. At the same time, the mixed vapor generated by the dehydration reaction needs to be separated by a distillation column, but existing devices mostly use bulk packing, which leads to uneven gas-liquid mass transfer, low separation efficiency, and insufficient distillation separation precision. Therefore, we propose a high-purity terpineol dehydration device. Utility Model Content

[0003] The purpose of this invention is to address the problems existing in the background technology by proposing a high-purity terpineol dehydration device.

[0004] The technical solution of this utility model is as follows: A high-purity terpineol dehydration device, comprising a reaction component and a distillation component. The reaction component includes a reaction vessel containing a solid-liquid mixed acid catalyst module. The distillation component includes a distillation column containing a structured metal wire mesh packing. A connecting pipe is provided between the reaction component and the distillation component, and a liquid flow meter is installed on the connecting pipe. A reflux pipe is provided between the top of the distillation column and the top of the reaction vessel, and an intelligent reflux ratio controller is installed on the reflux pipe. A stable base is provided on the side of the distillation column away from the reaction vessel, and a phase separation component is provided on the stable base. The phase separation component includes a phase separator containing coalescing packing. A condensation component is provided on the stable base above the phase separator, and the condensation component includes a condenser. An outlet pipe is provided at one end of the condenser, and a pressure sensor is installed in the outlet pipe.

[0005] Preferably, the mounting end of the solid-liquid mixed acid catalyst module is installed corresponding to the inner wall of the reactor. The solid-liquid mixed acid catalyst module includes a supported polymer solid acid carrier and a dilute sulfuric acid mixed layer. A guide plate is provided in the inner ring of the solid-liquid mixed acid catalyst module.

[0006] Preferably, the installation end of the wire mesh structured packing is installed corresponding to the inner wall of the distillation column, and multiple sets of temperature sensors are uniformly arranged along the height direction of the wire mesh structured packing inside the distillation column. The temperature sensors are electrically connected to the intelligent reflux ratio controller.

[0007] Preferably, the two ends of the connecting pipe are respectively installed on the side of the reactor and the distillation column that are close to each other, the installation end of the liquid flow meter is installed corresponding to the connecting pipe, the two ends of the reflux pipe are respectively installed corresponding to the top end of the reactor and the distillation column, the installation end of the intelligent reflux ratio controller is installed corresponding to the reflux pipe, and the liquid flow meter is electrically connected to the intelligent reflux ratio controller.

[0008] Preferably, the phase separator is a horizontal tank structure, the mounting end of the phase separator is installed correspondingly to the middle position on the stable base, a condenser pipe is provided between the phase separator and the condenser, a discharge oil pipe is provided on the phase separator at the oil phase outlet, and the coalescing packing is made of L stainless steel corrugated plate.

[0009] Preferably, the intelligent reflux ratio controller has a built-in PLC controller, and both the reflux pipe and the discharge oil pipe are equipped with electric regulating valves, and the intelligent reflux ratio controller is electrically connected to the electric regulating valves.

[0010] Preferably, the mounting end of the condenser is installed corresponding to the upper side of the stable base, a connecting pipe is provided between one end of the condenser and the distillation column, one end of the outlet pipe is installed corresponding to one end of the condenser, the mounting end of the pressure sensor is installed corresponding to the inner wall of the outlet pipe, the pressure sensor is electrically connected to the intelligent reflux ratio controller, a branch pipe is provided on one side of the outer ring of the condenser, and a pressure relief valve is provided in the branch pipe.

[0011] Compared with the prior art, the present invention has the following beneficial technical effects:

[0012] This invention features a simple and compact overall structure. By combining reaction and distillation components, it solves the problems of uneven catalyst dispersion, low mass transfer efficiency, and numerous side reactions in traditional reactors. This significantly improves the efficiency, selectivity, and stability of the reaction process, while also significantly enhancing the controllability, stability, and separation efficiency of the separation process. The combination of phase separation and condensation components enables efficient condensation of gaseous components, ensures material balance in the distillation component, and allows for control of distillation pressure, ensuring process stability and safety and promoting efficient operation of subsequent separation processes. Attached Figure Description

[0013] Figure 1 This is a schematic diagram of the overall structure of this utility model;

[0014] Figure 2 This is a schematic diagram of the structure of this utility model from another perspective;

[0015] Figure 3 This is a partial cross-sectional view of the present invention.

[0016] Reference numerals: 1. Reaction assembly; 11. Reactor; 12. Solid-liquid mixed acid catalyst module; 13. Baffle plate; 2. Distillation assembly; 21. Distillation column; 22. Structured metal mesh packing; 23. Temperature sensor; 3. Connecting pipe; 4. Liquid flow meter; 5. Reflux pipe; 6. Intelligent reflux ratio controller; 7. Stable base; 8. Phase separation assembly; 81. Phase separator; 82. Coalescing packing; 83. Discharge oil pipe; 9. Condensation assembly; 91. Condenser; 92. Outlet pipe; 93. Pressure sensor; 94. Branch pipe; 95. Pressure relief valve; 10. Connecting pipe; 15. Condenser pipe. Detailed Implementation

[0017] The technical solution of this utility model will be further described below with reference to the accompanying drawings and specific embodiments.

[0018] Example

[0019] like Figure 1-3 As shown, this utility model proposes a high-purity terpineol dehydration device, including a reaction component 1 and a distillation component 2. The reaction component 1 includes a reaction vessel 11, inside which a solid-liquid mixed acid catalyst module 12 is installed. The mounting end of the solid-liquid mixed acid catalyst module 12 is installed corresponding to the inner wall of the reaction vessel 11. The mounting end of the solid-liquid mixed acid catalyst module 12 is fixed to the inner wall of the reaction vessel 11 by bolts. The bolt fixing setting facilitates the operator to replace the solid-liquid mixed acid catalyst module 12 in the future. The solid-liquid mixed acid catalyst module 12 includes a mixed layer of a supported polymer solid acid carrier and dilute sulfuric acid. The synergistic system of the supported polymer solid acid and dilute sulfuric acid is reusable. The solid-liquid mixed acid catalyst module 12 is designed independently for easy and rapid replacement and regeneration, reducing catalyst consumption costs. The inner ring of the solid-liquid mixed acid catalyst module 12 is provided with a flow guide plate 13, and the mounting end of the flow guide plate 13 is fixedly connected to the solid-liquid mixed acid catalyst module 12. The flow guide plate 13 can enhance the liquid-solid contact efficiency, thereby enabling better catalytic dehydration of terpineol. The overall design of the reaction component 1 has a synergistic mechanism of flow field guidance, efficient catalyst contact, and homogenization of the reaction environment, which solves the problems of uneven dispersion of solid-liquid mixed catalyst, low mass transfer efficiency, and many side reactions in traditional reactors, significantly improving the efficiency, selectivity, and stability of the reaction process.

[0020] The distillation assembly 2 includes a distillation column 21, inside which a wire mesh structured packing 22 is installed. The mounting end of the wire mesh structured packing 22 is installed corresponding to the inner wall of the distillation column 21 and is fixedly connected to the inner wall of the distillation column 21. The installation of the wire mesh structured packing 22 can significantly improve the mass transfer efficiency and separation rate. Multiple sets of temperature sensors 23 are uniformly arranged along the height direction of the wire mesh structured packing 22 inside the distillation column 21. The mounting end of the temperature sensor 23 is fixedly connected to the inner ring of the wire mesh structured packing 22. The temperature sensor 23 can capture the temperature gradient in real time, accurately control the mass transfer balance, and at the same time avoid local overheating or low temperature, ensuring product purity and stability. The overall setup of the distillation assembly 2 has a linkage mechanism of accurate monitoring, efficient mass transfer and dynamic control, which significantly improves the controllability, stability and separation efficiency of the separation process.

[0021] A connecting pipe 3 is provided between the reaction assembly 1 and the distillation assembly 2. Both ends of the connecting pipe 3 are respectively installed on the sides of the reactor 11 and the distillation column 21, respectively, and are fixedly connected to the reactor 11 and the distillation column 21. A liquid flow meter 4 is installed on the connecting pipe 3, with its mounting end corresponding to the connecting pipe 3 and fixedly connected to it. The liquid flow meter 4 allows for precise control of the reaction discharge rate, ensuring stable operation of the distillation column and preventing safety hazards caused by excessive material. A reflux pipe 5 is provided between the top of the distillation column 21 and the top of the reactor 11, with both ends of the reflux pipe 5 connected to the top of the reactor 11 and the distillation column 21, respectively. Correspondingly, the two ends of the reflux pipe 5 are fixedly connected to the reactor 11 and the distillation column 21, respectively. An intelligent reflux ratio controller 6 is installed on the reflux pipe 5. The mounting end of the intelligent reflux ratio controller 6 is installed correspondingly to the reflux pipe 5 and fixedly connected to the reflux pipe 5. The intelligent reflux ratio controller 6 has a built-in PLC controller. The temperature sensor 23 is electrically connected to the intelligent reflux ratio controller 6, and the liquid flow meter 4 is electrically connected to the intelligent reflux ratio controller 6. The cooperative setup of the reflux pipe 5 and the intelligent reflux ratio controller 6 can accurately control the reflux ratio, improve separation efficiency and product quality, and at the same time build a synergistic closed loop of reaction and separation, optimize the overall process energy efficiency, support full-process automation, and promote the upgrading of intelligent manufacturing.

[0022] A stable base 7 is installed on the side of the distillation column 21 away from the reactor 11. A phase separation assembly 8 is installed on the stable base 7, including a phase separator 81. The phase separator 81 has a horizontal tank structure, and its mounting end corresponds to the middle position on the stable base 7. The mounting end of the phase separator 81 is fixedly connected to the stable base 7. A discharge oil pipe 83 is installed on the phase separator 81 at the oil phase outlet, and its mounting end is fixedly connected to the oil phase outlet. The discharge oil pipe 83 facilitates discharge. Both the reflux pipe 5 and the discharge oil pipe 83 are equipped with electric regulating valves. An intelligent reflux ratio controller 6 and... The electric regulating valve is electrically connected to the intelligent reflux ratio controller 6, which allows the operator to control the opening and closing of the electric regulating valve through the intelligent reflux ratio controller 6. This enables the operator to control the material flow rate between the reflux pipe 5 and the discharge oil pipe 83. The phase separator 81 is equipped with coalescing packing 82, which is made of 316L stainless steel corrugated plate. The installation end of the coalescing packing 82 is fixedly connected to the inner wall of the phase separator 81. The coalescing packing 82 has a dual function of wetting coalescing and collision coalescing. The setting of the coalescing packing 82 significantly improves the separation efficiency and breaks through the traditional gravity settling limit.

[0023] A condensing assembly 9 is installed on the stable base 7, above the phase separator 81. The condensing assembly 9 includes a condenser 91, with its mounting end corresponding to the upper side of the stable base 7 and fixedly connected to it. A condensing pipe 15 is installed between the phase separator 81 and the condenser 91, with both ends fixedly connected to the phase separator 81 and the condenser 91 respectively, thus connecting the phase separator 81 and the condenser 91. A connecting pipe 10 is installed between one end of the condenser 91 and the distillation column 21, with both ends fixedly connected to the condenser 91 and the distillation column 21 respectively, thus connecting the distillation column 21 and the condenser 91. The connection pipe 10 and the condensing pipe 15 allow the condenser 91 to connect the distillation column 21 and the phase separator 81. An outlet pipe 92 is installed at one end of the condenser 91, with one end corresponding to one end of the condenser 91. The mounting end is fixedly connected to the condenser 91. A pressure sensor 93 is installed inside the outlet pipe 92. The mounting end of the pressure sensor 93 is installed corresponding to the inner wall of the outlet pipe 92. The mounting end of the pressure sensor 93 is fixedly connected to the outlet pipe 92. The pressure sensor 93 is electrically connected to the intelligent reflux ratio controller 6. The intelligent reflux ratio controller 6 can automatically control the pressure sensor 93. A branch pipe 94 is provided on one side of the outer ring of the condenser 91. The mounting end of the branch pipe 94 is fixedly connected to the condenser 91. A pressure relief valve 95 is provided inside the branch pipe 94. The mounting end of the pressure relief valve 95 is fixedly connected to the inner wall of the branch pipe 94. When the pressure in the outlet pipe 92 exceeds a predetermined threshold, the branch pipe 94 is automatically opened to relieve pressure. The condenser assembly 9 can work in conjunction with the reaction assembly 1 and the distillation assembly 2 to achieve efficient condensation of gaseous components, ensure the material balance of the distillation assembly 2, control the distillation operation pressure, ensure process stability and safety, and promote the efficient operation of subsequent separation processes.

[0024] In this embodiment, the operator adds high-purity hydrated terpene diol crystals and an appropriate amount of water to the reaction vessel 11 at a mass ratio of 1:1. Then, the operator powers on the reaction vessel 11, causing the sulfonic acid resin in the solid-liquid mixed acid catalyst module 12 to synergistically catalyze the dehydration of the hydrated terpene diol to produce terpineol. The resulting vapor containing terpineol and water is then introduced into the distillation column 21 through the connecting pipe 3. At this time, the rising vapor and falling liquid in the distillation column 21 undergo mass transfer on the surface of the wire mesh structured packing 22. The water vapor moves to the top of the column, while the heavy component terpineol flows back to the bottom. Temperature sensor 23 monitors the temperature of each section in the distillation column 21 in real time and then transmits the data to the intelligent reflux ratio controller 6. If the temperature of a certain section deviates from the set value, the heating power is adjusted. The water vapor is cooled by condenser 91 to form an oil-water mixture, which enters condenser 91. The oil phase and water phase are accelerated to separate by coalescing packing 82. The oil phase is discharged from the discharge oil pipe 83, and the water phase is discharged from the bottom, thus completing the dehydration of high-purity terpineol.

[0025] When the pressure in the outlet pipe 92 exceeds the set threshold, the pressure sensor 93 triggers the pressure relief valve 95 to open, releasing the overpressure vapor.

[0026] The above-described specific embodiments are merely preferred embodiments of the present invention. Based on the technical solution of the present invention and the relevant teachings of the above embodiments, those skilled in the art can make various alternative improvements and combinations to the above-described specific embodiments.

Claims

1. A high-purity terpineol dehydration device, comprising a reaction assembly (1) and a distillation assembly (2), characterized in that: The reaction assembly (1) includes a reaction vessel (11), which is equipped with a solid-liquid mixed acid catalyst module (12). The distillation assembly (2) includes a distillation column (21), which is equipped with a metal wire mesh structured packing (22). A connecting pipe (3) is provided between the reaction assembly (1) and the distillation assembly (2). A liquid flow meter (4) is provided on the connecting pipe (3). A reflux pipe (5) is provided between the top of the distillation column (21) and the top of the reaction vessel (11). An intelligent reflux ratio controller is provided on the reflux pipe (5). (6) A stable base (7) is provided on the side of the distillation column (21) away from the reactor (11). A phase separation component (8) is provided on the stable base (7). The phase separation component (8) includes a phase separator (81). A coalescing packing (82) is provided inside the phase separator (81). A condensation component (9) is provided on the side of the stable base (7) above the phase separator (81). The condensation component (9) includes a condenser (91). An outlet pipe (92) is provided at one end of the condenser (91). A pressure sensor (93) is provided inside the outlet pipe (92).

2. The high-purity terpineol dehydration device according to claim 1, characterized in that, The mounting end of the solid-liquid mixed acid catalyst module (12) is installed corresponding to the inner wall of the reactor (11). The solid-liquid mixed acid catalyst module (12) includes a supported polymer solid acid carrier and a dilute sulfuric acid mixed layer. A guide plate (13) is provided in the inner ring of the solid-liquid mixed acid catalyst module (12).

3. The high-purity terpineol dehydration device according to claim 1, characterized in that, The installation end of the metal wire mesh structured packing (22) is installed corresponding to the inner wall of the distillation column (21). Multiple sets of temperature sensors (23) are uniformly arranged in the distillation column (21) along the height direction of the metal wire mesh structured packing (22). The temperature sensors (23) are electrically connected to the intelligent reflux ratio controller (6).

4. The high-purity terpineol dehydration device according to claim 1, characterized in that, The two ends of the connecting pipe (3) are respectively installed on the side close to the reactor (11) and the distillation column (21). The installation end of the liquid flow meter (4) is installed in relation to the connecting pipe (3). The two ends of the reflux pipe (5) are respectively installed in relation to the top of the reactor (11) and the distillation column (21). The installation end of the intelligent reflux ratio controller (6) is installed in relation to the reflux pipe (5). The liquid flow meter (4) is electrically connected to the intelligent reflux ratio controller (6).

5. The high-purity terpineol dehydration device according to claim 1, characterized in that, The phase separator (81) is a horizontal tank structure. The installation end of the phase separator (81) is installed in the middle position on the stable base (7). A condenser pipe (15) is provided between the phase separator (81) and the condenser (91). A discharge oil pipe (83) is provided on the phase separator (81) at the oil phase outlet. The coalescing packing (82) is made of 316L stainless steel corrugated plate.

6. The high-purity terpineol dehydration device according to claim 5, characterized in that, The intelligent reflux ratio controller (6) has a built-in PLC controller. Both the reflux pipe (5) and the discharge oil pipe (83) are equipped with electric regulating valves. The intelligent reflux ratio controller (6) is electrically connected to the electric regulating valves.

7. The high-purity terpineol dehydration device according to claim 1, characterized in that, The mounting end of the condenser (91) is installed corresponding to the upper side of the stable base (7). A connecting pipe (10) is provided between one end of the condenser (91) and the distillation column (21). One end of the outlet pipe (92) is installed corresponding to one end of the condenser (91). The mounting end of the pressure sensor (93) is installed corresponding to the inner wall of the outlet pipe (92). The pressure sensor (93) is electrically connected to the intelligent reflux ratio controller (6). A branch pipe (94) is provided on one side of the outer ring of the condenser (91). A pressure relief valve (95) is provided inside the branch pipe (94).

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