DOTP continuous production device

Abstract

The utility model belongs to the technical field of polyester production, and particularly relates to a DOTP continuous production device. Comprising a slurry preparation tank, the slurry preparation tank is connected with a slurry delivery pump through a slurry intermediate tank, the slurry delivery pump is connected with an esterification process tower through an esterification reaction kettle, the esterification process tower is respectively connected with an esterification condenser and an esterification condensate collecting tank, and the esterification condenser is also connected with the esterification condensate collecting tank; the primary esterification reaction kettle is also connected with a secondary esterification process tower through a secondary esterification reaction kettle, the secondary esterification process tower is respectively connected with a secondary esterification condensate collecting tank and a secondary esterification condenser, and the secondary esterification condensate collecting tank is also connected with the secondary esterification condenser. The device is convenient and efficient in production and low in energy consumption, and the production process is easy to control.

Description

Technical Field

[0001] The utility model belongs to the technical field of polyester production, and specifically relates to a DOTP continuous production device. Background Art

[0002] DOTP continuous production is an important development direction for DOTP synthesis. During the production process, the solid raw materials and liquid raw materials need to be fully mixed first and then enter the reactor for multi-step reactions.

[0003] However, all current DOTP production devices use cumbersome intermittent pulping and esterification intermittent reaction process steps, which will cause some problems: high production energy consumption, cumbersome steps, long time consumption, and poor stability of product quality indicators. Utility Model Content

[0004] The utility model aims to provide a DOTP continuous production device, which has convenient and efficient production, low energy consumption and easy control of the production process.

[0005] In order to achieve the above purpose and other related purposes, the utility model provides the following technical solutions:

[0006] A DOTP continuous production device comprises a slurry preparation tank, wherein the slurry preparation tank is connected to a slurry delivery pump via a slurry intermediate tank, the slurry delivery pump is connected to an esterification process tower via an esterification reactor, the esterification process tower is respectively connected to an esterification condenser and an esterification condensate collection tank, and the esterification condenser and the esterification condensate collection tank are also connected; the esterification reactor is also connected to a diesterification process tower via a diesterification reactor, the diesterification process tower is respectively connected to a diesterification condensate collection tank and a diesterification condenser, and the diesterification condensate collection tank and the diesterification condenser are also connected.

[0007] In one embodiment of the utility model, the slurry preparation tank is provided with a first agitator, the slurry intermediate tank is provided with a second agitator, the slurry intermediate tank is heated by steam, and the slurry delivery pump is controlled by frequency conversion.

[0008] In one embodiment of the utility model, the esterification reaction kettle has multiple reaction chambers, each reaction chamber has an agitator three, the esterification reaction kettle has a heating control system, the esterification reaction kettle is also connected to an esterification kettle liquid level gauge, and the esterification kettle liquid level gauge is also connected to the slurry delivery pump.

[0009] By adopting the above technical solution, the esterification reactor is provided with multiple reaction chambers to allow the materials to fully react and achieve the effect of first-in-first-out and last-in-last-out. Different from the general conventional production process which requires cumbersome intermittent operation, the esterification reactor of the present application can produce continuously with stable quality; in addition, the production process of the device is not limited to the synthesis of DOTP.

[0010] In one embodiment of the utility model, the esterification reaction kettle is connected to a catalyst addition pipeline, and the catalyst addition pipeline is provided with a catalyst addition regulating valve and a catalyst addition flow meter, and the catalyst addition regulating valve and the catalyst addition flow meter are also connected.

[0011] In one embodiment of the utility model, the esterification reaction kettle is connected to an octanol adding pipeline, and the octanol adding pipeline is provided with an octanol adding regulating valve and an octanol flowmeter, and the octanol adding regulating valve and the octanol flowmeter are also connected.

[0012] In one embodiment of the utility model, the esterification condenser is also connected to a tail gas venting pipe, the tail gas venting pipe is connected to an esterification pressure transmitter through a tail gas regulating valve, the esterification pressure transmitter is connected to a gas phase pipeline one, and the gas phase pipeline one is arranged between the esterification reaction kettle and the esterification process tower.

[0013] In one embodiment of the utility model, the esterified condensate collecting tank is also connected to an esterified condensate collecting tank level gauge, the esterified condensate collecting tank level gauge is connected to regulating valve 1, and the regulating valve 1 is connected to the esterified condensate collecting tank.

[0014] In one embodiment of the present invention, the first esterification reactor is connected to the diesterification reactor through an esterification to diesterification material delivery pipeline, the diesterification reactor is also connected to the diesterification reactor level gauge, the diesterification reactor level gauge is connected to the material regulating valve, and the material regulating valve is in turn connected to the first esterification to diesterification material delivery pipeline.

[0015] In one embodiment of the utility model, a stirrer four is provided in the diesterification reaction kettle, and the diesterification reaction kettle is also connected to an external finished product storage system or a tank truck or a finished product tank through a finished product delivery pipeline. A regulating valve two and a flow meter one are provided on the finished product delivery pipeline, and the regulating valve two and the flow meter one are also connected.

[0016] In one embodiment of the utility model, the diesterification condensate collecting tank is connected to a diesterification condensate collecting tank level gauge, the diesterification condensate collecting tank level gauge is connected to a regulating valve three, and the regulating valve three is connected to the diesterification condensate collecting tank.

[0017] The beneficial effects of the utility model are:

[0018] First, the present application includes a slurry preparation tank, a slurry intermediate tank, an esterification reactor, a diesterification reactor, etc., wherein the esterification reactor is provided with four chambers, each chamber is provided with three agitators, so that the materials are subjected to staged reactions. The present application can realize continuous production, shorten the reaction time, and realize stable and controllable quality of the finished product. In the prior art, the conventional intermittent reaction time is 6-10 hours for one batch.

[0019] Second, the present application includes an esterification process tower, an esterification condenser, an esterification condensate collection tank, a diesterification process tower, a diesterification condenser, a diesterification condensate collection tank, etc., so that the water generated by the reaction can be separated and discharged from octanol in time, and a liquid level meter is used for monitoring, which can intuitively display the speed of the reactor, which makes the product quality of the present application higher and the process easier to control.

[0020] Third, the present application is provided with a plurality of regulating valves, flow meters, and pipelines, which can be combined to accurately control the liquid raw materials entering the reactor, which makes the present application device have high reaction efficiency, convenient production, and easy process control.

[0021] In summary, the device of the present application makes polyester production convenient and efficient, with low energy consumption and easy control of the production process. BRIEF DESCRIPTION OF THE DRAWINGS

[0022] The accompanying drawings are used to provide a further understanding of the present invention and constitute a part of the specification. Together with the embodiments of the present invention, they are used to explain the present invention and do not constitute a limitation of the present invention. In the accompanying drawings:

[0023] Figure 1 It is a schematic diagram of the overall structure of the utility model;

[0024] Figure 2 The utility model Figure 1 Schematic diagram of the structure of the middle A part;

[0025] Figure 3 The utility model Figure 1 Schematic diagram of the structure of the middle B part;

[0026] The following are marked in the figure: 1. slurry preparation tank; 2. pipeline 1; 3. slurry intermediate tank; 4. slurry delivery pump; 5. slurry delivery pipeline; 6. an esterification reactor; 7. an esterification reactor level gauge; 8. a gas phase pipeline 1; 9. an esterification process tower; 10. an octanol reflux pipeline 1; 11. an esterification condensate collection tank; 12. an esterification water pipeline 1; 13. a gas phase pipeline 2; 14. an esterification condenser; 15. an exhaust gas venting pipeline; 16. an exhaust gas regulating valve; 17. an esterification condensate collection tank level gauge; 18. a regulating valve; 19. an esterification pressure transmitter; 20. a catalyst addition pipeline; 21. a catalyst addition regulating valve; 22. Catalyst addition flow meter; 23. Octanol addition pipeline; 24. Octanol flow meter; 25. Octanol addition regulating valve; 26. Material conveying pipeline from esterification to diesterification; 27. Diesterification reactor level meter; 28. Material regulating valve; 29. ​​Diesterification reactor; 30. Diesterification gas phase pipeline one; 31. Diesterification process tower; 32. Diesterification gas phase pipeline two; 33. Diesterification condenser; 34. Diesterification condensate collection tank; 35. Diesterification condensate collection tank level meter; 36. Regulating valve three; 37. Esterification water pipeline two; 38. Octanol reflux pipeline two; 39. Finished product conveying pipeline; 40. Regulating valve two; 41. Flow meter one. DETAILED DESCRIPTION

[0027] The technical solutions in the embodiments of the utility model are described clearly and completely below. Obviously, the described embodiments are only part of the embodiments of the utility model, not all of them. Based on the embodiments of the utility model, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the utility model.

[0028] Unless otherwise specified, the equipment and materials used in the examples can be easily obtained from commercial companies.

[0029] Among them, the slurry conveying pipeline 5, the gas phase pipeline 18, the octanol reflux pipeline 10, the esterification water pipeline 12, the gas phase pipeline 2 13, the tail gas venting pipeline 15, the catalyst adding pipeline 20, the octanol adding pipeline 23, the first esterification to diesterification material conveying pipeline 26, the diesterification gas phase pipeline 1 30, the diesterification gas phase pipeline 2 32, the esterification water pipeline 2 37, the octanol reflux pipeline 2 38, and the finished product conveying pipeline 39 are all pipelines. The first esterification kettle level gauge 7, the first esterification condensate collecting tank level gauge 17, the diesterification reactor level gauge 27, and the diesterification condensate collecting tank level gauge 35 are all level gauges. The first esterification process tower 9 and the diesterification process tower 31 are all esterification process towers. The tail gas regulating valve 16, the regulating valve 18, the catalyst adding regulating valve 21, the octanol adding regulating valve 25, the material regulating valve 28, the regulating valve 3 36, and the regulating valve 2 40 are all regulating valves. The first esterification condenser 14 and the second esterification condenser 33 are condensers. The catalyst addition flow meter 22, the octanol flow meter 24, and the flow meter 41 are flow meters. The first esterification reaction kettle 6 and the second esterification reaction kettle 29 are esterification reaction kettles. The agitator 1 to the agitator 4 are agitators.

[0030] The working principles of the aforementioned contents are well known and will not be elaborated here.

[0031] Example 1

[0032] like Figures 1 to 3 As shown, a DOTP continuous production device includes a slurry preparation tank 1.

[0033] Reference Figure 1~2 There is a stirrer 1 in the slurry preparation tank 1, and the stirrer 1 is used to evenly mix the solid raw materials. A liquid level meter can also be provided for the slurry preparation tank 1.

[0034] The bottom outlet of the slurry preparation tank 1 is connected to the slurry intermediate tank 3 through a pipe 2. The slurry intermediate tank 3 is provided with an agitator to prevent the prepared slurry from settling. A liquid level gauge can also be provided for the slurry intermediate tank 3. The slurry intermediate tank 3 is heated by steam.

[0035] The bottom of the slurry intermediate tank 3 is connected to a slurry delivery pump 4 by a pipeline. The slurry delivery pump 4 is a screw pump, and its working principle is well known and will not be described in detail. The slurry delivery pump 4 is connected to an esterification reactor 6 through a slurry delivery pipeline 5. The slurry delivery pump 4 adopts frequency conversion control, which can accurately control the amount of slurry delivered to the esterification reactor 6.

[0036] The first esterification reaction kettle 6 is provided with four chambers, each of which is provided with a stirrer 2, which allows the material to react fully and enables the material to flow from chamber to chamber. The first esterification reaction kettle 6 is provided with a heating control system.

[0037] An esterification reaction kettle 6 is connected to a catalyst adding pipeline 20, and the catalyst adding pipeline 20 is used for adding a catalyst. The catalyst adding pipeline 20 is provided with a catalyst adding regulating valve 21 and a catalyst adding flow meter 22, and the catalyst adding regulating valve 21 and the catalyst adding flow meter 22 are also connected. An esterification reaction kettle 6 is also connected to an octanol adding pipeline 23, and the octanol adding pipeline 23 is used for adding octanol. The octanol adding pipeline 23 is provided with an octanol adding regulating valve 25 and an octanol flow meter 24, and the octanol adding regulating valve 25 and the octanol flow meter 24 are also connected. The catalyst adding regulating valve 21 and the catalyst adding flow meter 22 as well as the octanol adding regulating valve 25 and the octanol flow meter 24 are used to control the flow and accurately control the reaction process.

[0038] The esterification reaction kettle 6 is also connected to an esterification kettle liquid level meter 7 via a pipeline, and the esterification kettle liquid level meter 7 is connected to the slurry delivery pump 4 via a pipeline.

[0039] Reference Figure 1 and Figure 3 The top of an esterification reaction kettle 6 is connected to an esterification process tower 9 through a gas phase pipeline 18, and an esterification process tower 9 is connected to an esterification condenser 14 through a gas phase pipeline 2 13. The esterification condenser 14 is used for cooling, and cooling can obtain condensate. The top of an esterification condenser 14 is connected to a tail gas venting pipeline 15, and the tail gas venting pipeline 15 is connected to a tail gas regulating valve 16. The tail gas regulating valve 16 is also connected to an esterification pressure transmitter 19 in a pipeline manner. The esterification pressure transmitter 19 is a pressure transmitter, and its working principle is well known and will not be described in detail. An esterification pressure transmitter 19 is connected to a gas phase pipeline 8. According to actual conditions, the device can be automatically adjusted and regulated by an esterification pressure transmitter 19 in cooperation with the tail gas regulating valve 16.

[0040] Reference Figure 1 and Figure 3 The bottom of an esterification condenser 14 is connected to an esterification condensate collecting tank 11 by pipeline. The esterification condensate collecting tank 11 is connected to an esterification condensate collecting tank level meter 17 by pipeline. The esterification condensate collecting tank level meter 17 has the function of an interface level meter and can be used to detect the interface position of octanol and water.

[0041] An esterification condensate collecting tank level gauge 17 is pipeline-connected to a regulating valve 18, and the regulating valve 18 is connected to an esterification condensate collecting tank 11 through an esterification water pipeline 12.

[0042] An esterification condensate collection tank 11 is also connected to an esterification process tower 9 through an octanol reflux pipeline 10.

[0043] Octanol in the upper part of an esterification condensate collection tank 11 can flow back to an esterification process tower 9 through an octanol reflux pipe 10, and liquid level parameters can be set for a regulating valve 18. When the liquid level in an esterification condensate collection tank 11 is too high, the regulating valve 18 cooperates with an esterification condensate collection tank liquid level gauge 17 and an esterification water pipe 12 to automatically adjust with reference to the liquid level parameters.

[0044] Reference Figure 1~2 The bottom of an esterification reaction kettle 6 is connected to a diesterification reaction kettle 29 through an esterification to diesterification material delivery pipeline 26, the diesterification reaction kettle 29 is pipeline-connected to a diesterification reaction kettle level gauge 27, the diesterification reaction kettle level gauge 27 is pipeline-connected to a material regulating valve 28, and the material regulating valve 28 is connected to an esterification to diesterification material delivery pipeline 26. The diesterification reaction kettle level gauge 27 cooperates with the material regulating valve 28 to automatically control the liquid level of the diesterification reaction kettle 29.

[0045] A stirrer 4 is provided in the diesterification reactor 29, and the stirrer 4 is used to stir the materials, accelerate the reaction, and prevent precipitation. The bottom of the diesterification reactor 29 is also connected to an external finished product storage system or a tank truck or a finished product tank through a finished product delivery pipeline 39, and a regulating valve 2 40 and a flow meter 1 41 are provided on the finished product delivery pipeline 39, and the regulating valve 2 40 and the flow meter 1 41 are also connected to each other, so that the product flow can be accurately controlled.

[0046] The top of the diesterification reaction kettle 29 is connected to the diesterification process tower 31 through the diesterification gas phase pipeline 1 30, and the diesterification process tower 31 is connected to the diesterification condenser 33 through the diesterification gas phase pipeline 2 32. The diesterification condenser 33 is used for cooling, and cooling can obtain condensate. The bottom of the diesterification condenser 33 is connected to the diesterification condensate collecting tank 34 by pipeline. The diesterification condensate collecting tank 34 is a pipeline diesterification condensate collecting tank level gauge 35. The diesterification condensate collecting tank level gauge 35 has an interface level gauge function and is used to detect the interface position of octanol and water. The diesterification condensate collecting tank level gauge 35 is pipeline-connected to the regulating valve 3 36, and the regulating valve 3 36 is connected to the diesterification condensate collecting tank 34 through the esterification water pipeline 2 37.

[0047] The diesterification condensate collection tank 34 is also connected to the diesterification process tower 31 via an octanol reflux pipeline 38 .

[0048] The octanol in the upper part of the diesterification condensate collection tank 34 can be refluxed to the diesterification process tower 31 through the octanol reflux pipe 2 38, and the liquid level parameters can also be set for the regulating valve 3 36. When the liquid level in the diesterification condensate collection tank 34 is too high, the regulating valve 3 36 cooperates with the diesterification condensate collection tank level gauge 35 and the esterification water pipe 2 37 to automatically adjust with reference to the liquid level parameters.

[0049] Reference Figure 1~Figure 3 The DOTP continuous production device proposed in this application has the following working process:

[0050] The raw materials (such as PTA and octanol) are added to the slurry preparation tank 1 and stirred fully. After stirring, the raw materials are moved to the slurry intermediate tank 3 through the pipeline 2. The slurry delivery pump 4 is started to deliver the materials to the esterification reactor 6 for reaction. The water and excess octanol generated by the reaction pass through the esterification process tower 9 and enter the esterification condenser 14 for cooling. The condensate is cooled and enters the esterification condensate collection tank 11. The upper part of the esterification condensate collection tank 11 is octanol. The octanol is completely refluxed to the esterification process tower 9 through the octanol reflux pipeline 10. Excess water is discharged through the regulating valve 18.

[0051] An esterification reaction kettle 6 is added with catalyst and octanol during the reaction process. The catalyst and octanol flow from chamber 1 to chamber 2, chamber 2 to chamber 3, and chamber 3 to chamber 4. After the reaction is completed, the reactants are accurately controlled to enter the diesterification reaction kettle 29 through an esterification to diesterification material delivery pipeline 26 and a material regulating valve 28, and are stirred and continue to react in the diesterification reaction kettle 29. The octanol and water vapor generated in the reaction enter the diesterification process tower 31 through a diesterification gas phase pipeline 1 30, and then enter the diesterification condenser 33 through a diesterification gas phase pipeline 2 32 for cooling, and the cooling obtains condensate, which enters the diesterification condensate collecting tank 34. The upper part of the diesterification condensate collecting tank 34 is octanol, and octanol is refluxed to the diesterification process tower 31 through an octanol reflux pipeline 2 38, and the water at the bottom of the diesterification condensate collecting tank 34 is discharged through an esterification water pipeline 2 37. After the reaction of the materials in the diesterification reactor 29 is completed, they are accurately measured through the finished product delivery pipeline 39, the regulating valve 2 40 and the flow meter 1 41 and then discharged into an external storage device (such as a finished product storage system or a tank truck or a finished product tank).

[0052] The device of the present application is not only applicable to the production of DOTP, but can also be used in the production of other polyesters, by changing the raw materials according to the actual situation. The production process of the device of the present application is not limited to the synthesis of DOTP.

[0053] The above description is only a preferred embodiment of the utility model and is not intended to limit the utility model. Although the utility model is described in detail with reference to the above embodiments, those skilled in the art can still modify the technical solutions recorded in the above embodiments or replace some of the technical features therein by equivalents. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the utility model shall be included in the protection scope of the utility model.

Claims

1. A DOTP continuous production device, characterized in that: The invention comprises a slurry preparation tank (1), wherein the slurry preparation tank (1) is connected to a slurry delivery pump (4) via a slurry intermediate tank (3), wherein the slurry delivery pump (4) is connected to an esterification process tower (9) via an esterification reaction kettle (6), wherein the esterification process tower (9) is respectively connected to an esterification condenser (14) and an esterification condensate collection tank (11), and wherein the esterification condenser (14) and the esterification condensate collection tank (11) are also connected to each other; the esterification reaction kettle (6) is also connected to a diesterification process tower (31) via a diesterification reaction kettle (29), wherein the diesterification process tower (31) is respectively connected to a diesterification condensate collection tank (34) and a diesterification condenser (33), and wherein the diesterification condensate collection tank (34) and the diesterification condenser (33) are also connected to each other.

2. The DOTP continuous production device according to claim 1, characterized in that: The slurry preparation tank (1) is provided with a stirrer 1, the slurry intermediate tank (3) is provided with a stirrer 2, the slurry intermediate tank (3) is heated by steam, and the slurry delivery pump (4) is controlled by frequency conversion.

3. The DOTP continuous production device according to claim 1, characterized in that: The esterification reaction kettle (6) has a plurality of reaction chambers, each of which has a stirrer (3). The esterification reaction kettle (6) has a heating control system. The esterification reaction kettle (6) is also connected to an esterification kettle liquid level meter (7), and the esterification kettle liquid level meter (7) is also connected to the slurry delivery pump (4).

4. The DOTP continuous production device according to claim 1, characterized in that: The first esterification reaction kettle (6) is connected to a catalyst addition pipeline (20), and the catalyst addition pipeline (20) is provided with a catalyst addition regulating valve (21) and a catalyst addition flow meter (22), and the catalyst addition regulating valve (21) and the catalyst addition flow meter (22) are also connected.

5. The DOTP continuous production device according to claim 1, characterized in that: The first esterification reaction kettle (6) is connected to an octanol adding pipeline (23), and an octanol adding regulating valve (25) and an octanol flow meter (24) are provided on the octanol adding pipeline (23). The octanol adding regulating valve (25) and the octanol flow meter (24) are also connected.

6. The DOTP continuous production device according to claim 1, characterized in that: The first esterification condenser (14) is also connected to a tail gas venting pipeline (15), and the tail gas venting pipeline (15) is connected to an esterification pressure transmitter (19) through a tail gas regulating valve (16). The first esterification pressure transmitter (19) is further connected to a gas phase pipeline (8), and the gas phase pipeline (8) is arranged between the first esterification reaction kettle (6) and the first esterification process tower (9).

7. The DOTP continuous production device according to claim 1, characterized in that: The esterified condensate collecting tank (11) is also connected to an esterified condensate collecting tank level gauge (17), the esterified condensate collecting tank level gauge (17) is connected to a regulating valve (18), and the regulating valve (18) is in turn connected to the esterified condensate collecting tank (11).

8. The DOTP continuous production device according to claim 1, characterized in that: The first esterification reaction kettle (6) is connected to the diesterification reaction kettle (29) via an esterification to diesterification material conveying pipeline (26); the diesterification reaction kettle (29) is also connected to a diesterification reaction kettle liquid level meter (27); the diesterification reaction kettle liquid level meter (27) is connected to a material regulating valve (28); and the material regulating valve (28) is in turn connected to the first esterification to diesterification material conveying pipeline (26).

9. The DOTP continuous production device according to claim 1, characterized in that: The diesterification reaction kettle (29) is provided with a stirrer four, and the diesterification reaction kettle (29) is also connected to an external finished product storage system or a tank truck or a finished product tank through a finished product delivery pipeline (39). The finished product delivery pipeline (39) is provided with a regulating valve two (40) and a flow meter one (41), and the regulating valve two (40) and the flow meter one (41) are also connected.

10. The DOTP continuous production device according to claim 1, characterized in that: The diesterification condensate collecting tank (34) is connected to a diesterification condensate collecting tank level gauge (35), the diesterification condensate collecting tank level gauge (35) is connected to a regulating valve three (36), and the regulating valve three (36) is in turn connected to the diesterification condensate collecting tank (34).

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