Glycerin triacetate efficient esterification reaction system
By designing an efficient connection system between the esterification tower and the esterification tank during the production process of glycerol triacetate, the problems of temperature gradient and energy consumption in the esterification reaction are solved, and the effects of efficient esterification and energy saving and consumption reduction are achieved.
Patent Information
- Application Number
- CN202421153745.7
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- Filing Date
- 2024-05-24
- Publication Date
- 2025-01-10
- Estimated Expiration
- 2034-05-24
AI Technical Summary
During the existing industrial production process of glycerol triacetate, the material is coking due to the temperature gradient during the esterification reaction, and the heating device increases energy consumption and cost. At the same time, the process of removing low-boiling solvents is complicated, which affects the esterification efficiency.
A high-efficiency esterification reaction system including an esterification tower and an esterification tank is designed. A heater is installed in the esterification tank, and the feed port and evaporation port are respectively provided at the bottom and the top, which are connected to the esterification tower through a pipeline to realize The preheating of the material, removing moisture and low boiling solvents are involved in the esterification reaction to avoid cooling and reheating processes.
It improves the esterification efficiency, reduces heating energy consumption, simplifies the system structure, reduces production costs, and avoids the problems of materials adhesion on the tower wall and maintenance of the mixing mechanism.
Smart Images
Figure CN222325140U_ABST
Abstract
Description
Technical Field
[0001] The utility model belongs to the technical field of chemical equipment, and in particular relates to a triacetin efficient esterification reaction system with high esterification efficiency, sufficient reaction, energy saving and consumption reduction. Background Art
[0002] Glyceryl triacetate is a colorless oily liquid with a faint fruity, meaty and sweet taste. It is an organic compound with a bitter taste at low concentrations. It is widely used in the formulation of daily chemical flavors and is mainly used as a fixative. The key process in the industrial production of glyceryl triacetate is the esterification reaction, and its esterification is achieved by bringing the water-carrying agent into a slightly boiling or sub-boiling state with the water generated by the reaction. The steam is condensed and separated by a condenser. The upper layer of the water-carrying agent is refluxed to continue to participate in the reaction or be extracted. The lower water layer is continuously removed until the speed of water generation is slow or there is no water phase. A certain amount of acetic anhydride is added to the kettle, and the reaction is continued for a period of time. After cooling and analysis, the catalyst is filtered out, and the filtrate is distilled to recover excess acetic acid and toluene to obtain glyceryl triacetate.
[0003] Since the materials in the esterification tower kettle need to be continuously heated during the esterification reaction to keep the esterification reaction in a slightly boiling or sub-boiling state, the materials are generally preheated by setting a mixing preheating kettle in front of the esterification tower kettle, and then a heating device is set at the lower part of the esterification tower. However, setting a heating device at the lower part of the esterification tower easily causes a large temperature gradient between the center and the edge of the tower, and in order to ensure that the esterification materials are in a slightly boiling or sub-boiling state as a whole to improve the esterification efficiency, the tower wall often needs to maintain a high temperature, which easily causes the esterification materials to adhere to the tower wall, such as coking; and in order to avoid adhesion to the tower wall, the temperature of the tower wall can only be reduced, which makes it difficult for the materials in the center of the tower to reach a slightly boiling or sub-boiling state, seriously affecting the esterification efficiency. For this reason, in the prior art, a stirring mechanism or a catalyst lifting mechanism is set in the esterification tower to reduce the temperature difference of the materials in the tower, but the stirring mechanism and the catalyst lifting mechanism need to cooperate with a tight sealing structure, which not only complicates the structure of the esterification tower, but also increases the maintenance cost of the sealing structure. In addition, in the prior art, after the esterification reaction is completed, it is often necessary to pass the esterification reactants into a low-temperature evaporator in advance, remove residual water and low-boiling point solvents by reheating, and then pass them into a refining esterification tower kettle for further refining, so as to obtain high-purity triacetin; this results in the esterification reactants needing to be first cooled and filtered in the esterification tower, and then heated and distilled, which not only increases the energy consumption of the esterification reaction, but also causes the removed low-boiling point solvent to be only used for the next batch of esterification reactions, resulting in a large amount of low-boiling point solvent required for one esterification reaction and a high heating energy consumption, which pushes up the esterification cost. Utility Model Content
[0004] According to the deficiencies of the prior art, the utility model develops a triacetin efficient esterification reaction system which has high esterification efficiency, sufficient reaction, energy saving and consumption reduction.
[0005] The utility model is implemented as follows: it comprises an esterification tower and an esterification tank, wherein a heater is arranged in the middle or lower part of the esterification tank, a feed port II is arranged at the bottom of the esterification tank and an evaporation port II is arranged at the top, a discharge port is arranged at the bottom of the esterification tower and an evaporation port I is arranged at the top, the discharge port is communicated with the feed port II through a pipeline I, a feed port I is arranged at the lower or middle part of the esterification tower, the feed port I is communicated with the evaporation port II through a pipeline II, a feed pipe is arranged at one side or the bottom of the esterification tank, the feed pipe is communicated with a batching device or an ester separator at the upper part of the esterification tower, and the discharge port is higher than the feed port II.
[0006] Furthermore, the esterification tank is transversely arranged on one side of the esterification tower, and a liquid equalizing pipe is arranged inside the esterification tank below the heater. The liquid equalizing pipe has a plurality of through holes I spaced apart along the length direction, and the liquid equalizing pipe is connected to the feed port II.
[0007] Furthermore, the heater is arranged along the axial direction of the esterification tank and its two ends are respectively connected to the steam inlet pipe and the steam outlet pipe on the outer wall of the esterification tank and steam is introduced into the heater. The liquid equalizing pipe extends along the axial direction of the esterification tank and its two ends are closed. The liquid equalizing pipe is provided with a plurality of through holes I at intervals below the heater.
[0008] Furthermore, the feed pipe is arranged at one end of the esterification tank and the opening on the inner wall is lower than the lower bottom surface of the heater.
[0009] Furthermore, a material equalizing pipe is provided inside the esterification tank below the heater. The material equalizing pipe extends axially along the esterification tank and is connected to the feed pipe at one end and closed at the other end. The material equalizing pipe is provided with a plurality of through holes II at intervals below the heater.
[0010] Furthermore, a discharge pipe is provided at the bottom or one side of the esterification tank, and a valve I is provided on the discharge pipe and is connected to a subsequent esterification device.
[0011] Furthermore, the esterification tank is also provided with a thermocouple whose measuring end extends to the middle or lower part of the esterification tank, and the thermocouple and the heater are electrically connected to the control device respectively.
[0012] Furthermore, a valve II is provided on the pipeline I, and a valve III is provided on the feed pipe.
[0013] Furthermore, a plurality of circular or square fins are arranged at intervals on the pipeline of the heater.
[0014] Compared with the prior art, the beneficial effects of the utility model are:
[0015] 1. The utility model arranges an esterification tank on one side of the esterification tower. The heatable esterification tank can not only preheat the esterification materials to play the role of a mixed preheating kettle, but also continue to heat the esterification reactants after the esterification of the esterification tower to further remove residual moisture and low-boiling point solvents, thereby playing the role of a low-temperature evaporator, that is, achieving the effect of dual use of one thing and effectively simplifying the esterification system.
[0016] 2. The esterification tank of the utility model is arranged on one side of the esterification tower, and the discharge port at the bottom of the esterification tower is connected with the feed port II at the bottom of the esterification tank through a pipeline I, so that the hot esterification reactants are directly introduced into the esterification tank at the end of esterification or in the late stage of the esterification reaction, and then continue to be heated to remove residual moisture and low-boiling point solvents, which can avoid the process of cooling and reheating the esterification reactants, not only improving the removal speed to improve the esterification efficiency, but also significantly reducing the energy consumption of heating, and the evaporation port II arranged on the top of the esterification tank is connected with the feed port I at the lower or middle part of the esterification tower through the pipeline II, and the low-boiling point solvent can be refluxed to the esterification tower to continue to participate in the esterification reaction, reducing the amount of low-boiling point solvent required for one esterification reaction and reducing the esterification cost.
[0017] 3. The utility model uses the evaporation port II arranged on the top of the esterification tank to communicate with the feed port I at the lower or middle part of the esterification tower through the pipeline II, so that the reactants at the bottom of the esterification tower are heated by the esterification tank to form steam that flows back into the esterification tower, so that the materials in the esterification tower reach a slightly boiling or sub-boiling state, which can not only ensure the esterification efficiency, but also avoid the adhesion of the tower wall of the esterification tower, and will not cause the problem of difficult maintenance of the stirring mechanism or the catalyst lifting mechanism.
[0018] 4. The discharge port at the bottom of the esterification tower of the utility model is connected with the feed port II at the bottom of the esterification tank through a pipeline I, so that the material at the bottom of the esterification tower passes into the lower part of the heater of the esterification tank, and the material is heated by the heater to form an upward convection, so that the material can fully react in the esterification tank, and finally be heated and evaporated to enter the esterification tower again to participate in the esterification, thereby avoiding the problem that the material is vaporized from the top of the esterification tank and is difficult to fully react, thereby improving the efficiency of the esterification reaction.
[0019] In summary, the utility model has the characteristics of high esterification efficiency, sufficient reaction, energy saving and consumption reduction. BRIEF DESCRIPTION OF THE DRAWINGS
[0020] Figure 1 It is a schematic diagram of the structure of the utility model;
[0021] Figure 2 for Figure 1 Left view of
[0022] Figure 3 for Figure 2 Right view of the esterification tank;
[0023] In the figure: 1-esterification tower, 11-discharge port, 12-feed port I, 2-esterification tank, 21-heater, 22-feed port II, 23-evaporation port II, 24-feed pipe, 25-liquid equalizing pipe, 26-steam inlet pipe, 27-steam outlet pipe, 28-equalizing pipe, 29-discharge pipe, 2A-fin, 3-pipeline I, 4-pipeline II, 5-valve II, 6-valve I, 7-thermocouple, 8-valve III. DETAILED DESCRIPTION
[0024] The present invention is further described below in conjunction with the accompanying drawings and embodiments, but the present invention is not limited in any way. Any changes or improvements made based on the teachings of the present invention belong to the protection scope of the present invention.
[0025] like Figure 1 , 2 As shown in Figures 1 and 3, the utility model includes an esterification tower 1 and an esterification tank 2. A heater 21 is provided in the middle or lower part of the esterification tank 2. A feed port II 22 is provided at the bottom of the esterification tank 2 and an evaporation port II 23 is provided at the top. A discharge port 11 is provided at the bottom of the esterification tower 1 and an evaporation port I is provided at the top. The discharge port 11 is connected with the feed port II 22 through a pipeline I3. A feed port I 12 is provided at the lower or middle part of the esterification tower 1. The feed port I 12 is connected with the evaporation port II 23 through a pipeline II 4. A feed pipe 24 is provided at one side or the bottom of the esterification tank 2. The feed pipe 24 is connected with a batching device or an ester separator at the top of the esterification tower 1. The discharge port 11 is higher than the feed port II 22.
[0026] The esterification tank 2 is transversely arranged on one side of the esterification tower 1 . A liquid averaging pipe 25 is arranged below the heater 21 inside the esterification tank 2 . The liquid averaging pipe 25 has a plurality of through holes Ⅰ spaced apart along the length direction. The liquid averaging pipe 25 is connected to the feed port Ⅱ22 .
[0027] The heater 21 is arranged along the axial direction of the esterification tank 2 and its two ends are respectively connected to the steam inlet pipe 26 and the steam outlet pipe 27 on the outer wall of the esterification tank 2 and steam is introduced. The liquid equalizing pipe 25 extends along the axial direction of the esterification tank 2 and is closed at both ends. The liquid equalizing pipe 25 is provided with a plurality of through holes I at intervals below the heater 21.
[0028] The feed pipe 24 is disposed at one end of the esterification tank 2 and the opening on the inner wall is lower than the bottom surface of the heater 21 .
[0029] A material equalizing pipe 28 is further provided inside the esterification tank 2 below the heater 21 . The material equalizing pipe 28 extends axially along the esterification tank 2 and is connected to the feed pipe 24 at one end and closed at the other end. The material equalizing pipe 28 is provided with a plurality of through holes II at intervals below the heater 21 .
[0030] A discharge pipe 29 is also provided at the bottom or one side of the esterification tank 2. A valve I6 is provided on the discharge pipe 29 and the discharge pipe 29 is connected to the subsequent esterification device.
[0031] The esterification tank 2 is also provided with a thermocouple 7 whose measuring end extends to the middle or lower part of the esterification tank 2. The thermocouple 7 and the heater 21 are electrically connected to the control device, respectively. The control device is any commercially available thermal control device.
[0032] The pipeline I3 is provided with a valve II5 , and the feed pipe 24 is provided with a valve III8 .
[0033] A plurality of circular or square fins 2A are arranged at intervals on the pipeline of the heater 21 .
[0034] The working principle and working process of this utility model:
[0035] like Figure 1 , 2 As shown in Figure 3, first open the valve connected to the feed pipe 24, add glycerol, acetic acid and water-carrying agent into the esterification tank 2, and add the catalyst into the esterification tower 1, then close the valve Ⅰ6, open the steam inlet pipe 26 and the steam outlet pipe 27 to allow flowing steam to pass, heat and evaporate the materials in the esterification tank 2 through the heater 21, and pass them into the esterification tower 1 through the evaporation port Ⅱ23 at the top through the pipeline Ⅱ4 and the feed port Ⅰ12 for esterification reaction. The pressure in the esterification tower 1 can be adjusted by a pressure regulator. During the esterification reaction, the water-carrying agent and water in the upper part of the esterification tower 1 are separated from the condensing device and the separation device at the top, and the material at the bottom of the esterification tower 1 flows out from the discharge port 11, passes through the pipeline Ⅰ3 and the valve Ⅱ5 through the feed port Ⅱ22 to enter the bottom of the esterification tank 2, rises under the heating of the heater 21 for convection and reaction, and finally passes through the evaporation port Ⅱ23 and the pipeline Ⅱ4 through the feed port 12 to enter the esterification tower 1, heat the material in the esterification tower 1 and participate in the esterification reaction; after the reaction is completed, continue to open the steam inlet pipe 26 and the steam outlet Flowing steam is introduced into pipe 27, and residual water and low boiling point solvent in the material in esterification tank 2 are removed through heater 21. The material after water and low boiling point solvent are removed passes through discharge pipe 29 at the bottom of esterification tank 2, and is further refined into refining kettle through valve I6 and pump to obtain triacetin finished product; water vapor and low boiling point solvent enter esterification tower 1 again and are separated by condensation device and separation device at the top, water is discharged, and low boiling point solvent remains in esterification tower 1 or returns to esterification tank 2 to participate in the next batch of esterification reaction.
[0036] The above is only a preferred specific implementation of the utility model, but the protection scope of the utility model is not limited thereto. Any changes or substitutions that can be easily thought of by any technician familiar with the technical field within the technical scope disclosed by the utility model should be included in the protection scope of the utility model. Therefore, the protection scope of the utility model should be based on the protection scope of the claims.
Claims
1. A triacetin efficient esterification reaction system, characterized in that: The invention comprises an esterification tower (1) and an esterification tank (2), wherein a heater (21) is arranged in the middle or lower part of the esterification tank (2), a feed port II (22) is arranged at the bottom of the esterification tank (2) and an evaporation port II (23) is arranged at the top, a discharge port (11) is arranged at the bottom of the esterification tower (1) and an evaporation port I is arranged at the top, the discharge port (11) is connected to the feed port II (22) through a pipeline I (3), a feed port I (12) is arranged at the lower or middle part of the esterification tower (1), the feed port I (12) is connected to the evaporation port II (23) through a pipeline II (4), a feed pipe (24) is arranged on one side or at the bottom of the esterification tank (2), the feed pipe (24) is connected to a batching device or an ester separator at the top of the esterification tower (1), and the discharge port (11) is higher than the feed port II (22).
2. The triacetin efficient esterification reaction system according to claim 1, characterized in that: The esterification tank (2) is arranged transversely on one side of the esterification tower (1). A liquid averaging pipe (25) is arranged inside the esterification tank (2) below the heater (21). The liquid averaging pipe (25) is provided with a plurality of through holes I at intervals along the length direction. The liquid averaging pipe (25) is connected to the feed port II (22).
3. The efficient esterification reaction system of triacetin according to claim 2, characterized in that: The heater (21) is arranged along the axial direction of the esterification tank (2) and its two ends are respectively connected to the steam inlet pipe (26) and the steam outlet pipe (27) on the outer wall of the esterification tank (2) and allow steam to flow into the heater (21). The liquid balancing pipe (25) extends along the axial direction of the esterification tank (2) and its two ends are closed. The liquid balancing pipe (25) is provided with a plurality of through holes I at intervals below the heater (21).
4. The efficient esterification reaction system of triacetin according to claim 2, characterized in that: The feed pipe (24) is arranged at one end of the esterification tank (2), and the opening on the inner wall is lower than the bottom surface of the heater (21).
5. The efficient esterification reaction system of triacetin according to claim 4, characterized in that: A material equalizing pipe (28) is further provided inside the esterification tank (2) below the heater (21). The material equalizing pipe (28) extends along the axial direction of the esterification tank (2) and is connected to the feed pipe (24) at one end and is closed at the other end. The material equalizing pipe (28) is provided with a plurality of through holes II at intervals below the heater (21).
6. The efficient esterification reaction system of triacetin according to any one of claims 1 to 5, characterized in that: A discharge pipe (29) is also provided at the bottom or one side of the esterification tank (2). A valve I (6) is provided on the discharge pipe (29) and the discharge pipe (29) is connected to a subsequent esterification device.
7. The efficient esterification reaction system of triacetin according to claim 6, characterized in that: The esterification tank (2) is also provided with a thermocouple (7) whose measuring end extends to the middle or lower part of the esterification tank (2). The thermocouple (7) and the heater (21) are electrically connected to the control device respectively.
8. The triacetin efficient esterification reaction system according to claim 6, characterized in that: The pipeline I (3) is provided with a valve II (5), and the feed pipe (24) is provided with a valve III (8).
9. The triacetin efficient esterification reaction system according to claim 6, characterized in that: A plurality of circular or square fins (2A) are arranged at intervals on the pipeline of the heater (21).