A continuous tubular reactor for the synthesis of phosphate ester wetting dispersants

Abstract

The utility model relates to continuous flow chemical reaction engineering and fine chemical equipment, concretely to a kind of continuous tubular reaction device for phosphate ester wetting dispersant synthesis, the problem proposed in background art is solved, it includes base, static mixing pipe, first tubular reactor, second tubular reactor, vacuum tank, discharge pump, control module, online detection unit, bypass tank, mechanical seal system and so on and so on.The utility model realizes the quick premixing of raw material by static mixing pipe, avoids the non-productive waiting time such as feeding, temperature rising, heat preservation of batch kettle, and production efficiency can be improved;Online viscosity detection unit can according to viscosity feedback data, timely fine-tune process parameter;Vacuum tank can exclude moisture generated by reaction in time, ensure product purity;Mechanical seal system reduces the risk of shaft seal leakage;Combined with control module, operation is more systematized, automated.

Description

Technical Field

[0001] This utility model relates to continuous flow chemical reaction engineering and fine chemical equipment, specifically a continuous tubular reaction device for the synthesis of phosphate ester wetting and dispersing agents. Background Technology

[0002] In the field of fine chemicals, the production of phosphate ester wetting and dispersing agents typically involves the esterification or polymerization of high-viscosity materials. Traditional synthesis processes generally employ batch reactors, which have certain limitations. First, the materials undergo a drastic change in viscosity from low to high within the reactor, requiring high levels of stirring and heat and mass transfer, which can easily lead to uneven mixing, long reaction cycles, and batch-to-batch product quality fluctuations. Second, if the moisture generated during the reaction is not removed in time, it will inhibit the forward reaction and affect the final conversion rate. Furthermore, batch production has limited automation, making it difficult to monitor and control the reaction process in real time and accurately, which is not conducive to achieving efficient, stable, and continuous industrial production. In recent years, although continuous flow technology has been developed in the chemical industry, its application to such high-viscosity reaction systems with the removal of byproducts still faces a series of engineering and technical challenges, including material conveying, uniform reaction, online detection, and integrated control of the entire process. To address these issues, a continuous tubular reactor for the synthesis of phosphate ester wetting and dispersing agents is proposed. Utility Model Content

[0003] To solve the above problems, this utility model provides the following technical solution:

[0004] A continuous tubular reaction apparatus for the synthesis of phosphate ester wetting and dispersing agents includes a base; a static mixing tube is fixedly mounted on the base, the static mixing tube including a tube body, a static mixer being disposed inside the tube body, and at least three feed inlets being disposed on the side wall of the tube body; a first tubular reactor and a second tubular reactor are fixedly mounted on the base, the inlet of the first tubular reactor being connected to the outlet of the static mixing tube, and the inlet of the second tubular reactor being connected to the outlet of the first tubular reactor via a first connecting pipe; a vacuum tank is fixedly mounted on the base. The vacuum tank inlet is connected to the outlet of the second tubular reactor via a second connecting pipe, and an interface is provided on the top of the vacuum tank; a discharge pump is fixedly installed on the base, the discharge pump includes a pump body and a pump drive motor, the drive shaft of the pump body is connected to the output shaft of the pump drive motor, the inlet of the discharge pump is connected to the bottom outlet of the vacuum tank, and the outlet of the discharge pump is connected to a discharge pipe; a control module is fixedly installed on the base, and is provided with an operation panel and a power interface; the control module is electrically connected to the discharge pump, the first tubular reactor, and the second tubular reactor.

[0005] Further, the first tubular reactor comprises a second pipe body, a first temperature control jacket is arranged outside the second pipe body, a first stirring shaft is arranged inside the second pipe body, a first motor is fixed at the end of the second pipe body, one end of the first stirring shaft is fixedly connected to the output shaft of the first motor through a coupling, and a plurality of groups of first stirring blades are arranged on the first stirring shaft;

[0006] Further, the second tubular reactor comprises a third pipe body, a second temperature control jacket, a second stirring shaft, a second motor and a plurality of groups of second stirring blades.

[0007] Further, the control module is provided with an operation panel and a power interface, and is electrically connected with the first motor, the second motor, the first temperature control jacket, the second temperature control jacket, the discharge pump and the pump drive motor thereof; the operation panel is integrated with a temperature control unit for adjusting the reaction temperature and a rotation speed control unit for adjusting the stirring speed.

[0008] Further, the system also comprises an on-line detection unit and a matching bypass tank thereof; the on-line detection unit comprises a first on-line viscometer arranged on the first connecting pipeline and a second on-line viscometer arranged on the discharge pipeline; the control module is in signal connection with the first on-line viscometer and the second on-line viscometer through signal cables.

[0009] Further, the first on-line viscometer and the second on-line viscometer are on-line rotational viscometers, the sensors of which respectively extend into a stirred bypass tank, and a stirrer is arranged in the bypass tank.

[0010] Further, the inlet ends of the at least three feed ports are respectively connected with the outlets of three metering pumps.

[0011] Further, the first connecting pipeline is an inverted U-shaped pipe, and the highest point thereof is provided with a vent valve; both the outlet of the first tubular reactor and the inlet of the second tubular reactor are connected with the first connecting pipeline through reducing pipe joints.

[0012] Further, a back pressure valve is installed on the end pipeline of the discharge pipeline.

[0013] Further, the system also comprises a mechanical seal system, which comprises a first double mechanical seal sleeved on the first stirring shaft, a second double mechanical seal sleeved on the second stirring shaft, a third double mechanical seal sleeved on the transmission shaft of the discharge pump, and a seal liquid circulation station connected with the above mechanical seals.

[0014] Further, the first stirring blades and the second stirring blades are frame-type blades, and the outer edge contour of the frame-type blades is parallel to the inner wall contour of the pipe body of the reactor where they are located.

[0015] Compared with the prior art, the beneficial effects of the present utility model are as follows:

[0016] The raw materials are rapidly premixed through a static mixing tube, and then sequentially fed into a two-stage tubular reactor for deep reaction. This avoids the non-production waiting time of batch reactors, such as feeding, heating, and heat preservation, thus improving production efficiency. The second tubular reactor has a relatively fast stirring speed to accommodate the increased viscosity of the materials in the later stages of the reaction, promoting a more uniform and thorough reaction. An online viscosity detection unit can monitor the viscosity changes of the products at each stage in real time, and can fine-tune process parameters in a timely manner based on viscosity feedback data, enabling more precise control of the reaction process. A vacuum tank can promptly remove moisture and other substances generated during the reaction, ensuring product purity. Frame-type impellers help scrape the inner wall of the reactor, reducing material adhesion, while a bypass tank provides a stable measurement environment for the viscometer, improving the accuracy of online detection and long-term operational reliability. A mechanical seal system reduces the risk of shaft seal leakage. Combined with the control module, the operation becomes more systematic and automated. Attached Figure Description

[0017] The accompanying drawings are provided to further illustrate the present invention and form part of the specification. They are used together with the embodiments of the present invention to explain the present invention, but do not constitute a limitation thereof. In the drawings:

[0018] Figure 1 This is a frontal axonometric structural schematic diagram of the present invention;

[0019] Figure 2 This is a schematic diagram of the rear-view axonometric structure of this utility model;

[0020] Figure 3 This is a top view schematic diagram of part of the structure of this utility model;

[0021] Figure 4 This is a top sectional view of part of the structure of this utility model;

[0022] Figure 5 This is a frontal cross-sectional view of the static mixer of this utility model.

[0023] In the diagram, dashed lines represent electrical connections, dotted lines represent signal connections, and double-dotted lines represent pipe connections.

[0024] In the diagram: 1. Base; 2. Static mixing tube; 21. Tube body one; 22. Static mixer; 23. Feed inlet; 3. First tubular reactor; 31. Tube body two; 32. Temperature control jacket one; 33. Stirring shaft one; 34. Motor one; 35. Stirring blade one; 4. Second tubular reactor; 41. Tube body three; 42. Temperature control jacket two; 43. Stirring shaft two; 44. Motor two; 45. Stirring blade two; 5. First connecting pipe; 51. Exhaust valve; 52. Reducer; 6. Vacuum tank; 7. 8. Second connecting pipe; 8. Discharge pump; 81. Pump body; 82. Pump drive motor; 9. Discharge pipe; 10. Online detection unit; 101. First online viscometer; 102. Second online viscometer; 11. Control module; 111. Operation panel; 112. Power interface; 12. Bypass tank; 13. Back pressure valve; 14. Mechanical seal system; 141. First double-end mechanical seal; 142. Second double-end mechanical seal; 143. Third double-end mechanical seal; 144. Sealing fluid circulation station. Detailed Implementation

[0025] The technical solutions of the present utility model will be clearly and completely described below with reference to the accompanying drawings of the embodiments of the present utility model. Obviously, the described embodiments are only some embodiments of the present utility model, and not all embodiments. All other embodiments obtained by those skilled in the art based on the embodiments of the present utility model without creative effort are within the protection scope of the present utility model.

[0026] Example 1

[0027] like Figure 1-5 As shown, this embodiment provides a continuous tubular reaction apparatus for the synthesis of phosphate ester wetting and dispersing agents, including a base 1; a static mixing tube 2 is fixedly arranged on the base 1 to allow the raw materials to be initially mixed. The static mixing tube 2 includes a tube body 21, a static mixer 22 is arranged inside the tube body 21, and at least three feed ports 23 are arranged on the side wall of the tube body 21.

[0028] A first tubular reactor 3 and a second tubular reactor 4 are also fixedly installed on the base 1; the inlet of the first tubular reactor 3 is connected to the outlet of the static mixing pipe 2, and the inlet of the second tubular reactor 4 is connected to the outlet of the first tubular reactor 3 through the first connecting pipe 5.

[0029] A vacuum tank 6 is fixedly installed on the base 1 to remove volatile products and ensure the purity of the products. The inlet of the vacuum tank 6 is connected to the outlet of the second tubular reactor 4 through the second connecting pipe 7. An interface is provided on the top of the vacuum tank 6.

[0030] A discharge pump 8 is fixedly installed on the base 1; the discharge pump 8 is a screw pump, which makes it easier to transport high-viscosity products, including a pump body 81 and a pump drive motor 82; the drive shaft of the pump body 81 is connected to the output shaft of the pump drive motor 82; the inlet of the discharge pump 8 is connected to the bottom outlet of the vacuum tank 6, and the outlet of the discharge pump 8 is connected to a discharge pipe 9.

[0031] A control module 11 is fixedly installed on the base 1. The control module 11 is equipped with an operation panel 111 and a power interface 112. The control module 11 is electrically connected to the discharge pump 8, the first tubular reactor 3 and the second tubular reactor 4.

[0032] In this embodiment, the specific structure of the first tubular reactor 3 includes a tube body 31, a temperature control jacket 32 ​​is provided on the outside of the tube body 31, and a stirring shaft 33 is provided inside; a motor 34 is fixed at the end of the tube body 31, and one end of the stirring shaft 33 is fixedly connected to the output shaft of the motor 34 through a coupling; and multiple sets of stirring blades 35 are provided on the stirring shaft 33.

[0033] The structure of the second tubular reactor 4 is the same as that of the first tubular reactor 3. Accordingly, it includes a tube body 41, a temperature control jacket 42, a stirring shaft 43, a motor 44, and multiple sets of stirring blades 45, which ensures the stability of the reaction conditions.

[0034] The control module 11 has an integrated temperature control unit for adjusting the reaction temperature and a speed control unit for adjusting the stirring speed on its operation panel 111. These control units are used to control the temperatures of temperature control jacket 1 32 and temperature control jacket 2 42, as well as the speeds of motor 1 34 and motor 2 44, respectively.

[0035] Preferably, the device further includes an online detection unit 10 and a bypass tank 12 therewith, providing information on the stage and final product; the online detection unit 10 includes a first online viscometer 101 disposed on the first connecting pipe 5 and a second online viscometer 102 disposed on the discharge pipe 9; the control module 11 is connected to the first online viscometer 101 and the second online viscometer 102 via a signal cable; more preferably, the first online viscometer 101 and the second online viscometer 102 are online rotary viscometers, and their sensors extend into the bypass tank 12, which is equipped with a stirrer.

[0036] Furthermore, the inlet ends of at least three feed ports 23 are respectively connected to the outlets of three metering pumps to ensure that a variety of raw materials can be continuously fed in a precise and constant ratio.

[0037] Furthermore, the first connecting pipe 5 is an inverted U-shaped pipe with an exhaust valve 51 at its highest point; the outlet of the first tubular reactor 3 and the inlet of the second tubular reactor 4 are both connected to the first connecting pipe 5 through a reducing pipe joint 52 to remove gas from the pipe and reduce obstruction to the flow of materials.

[0038] Furthermore, a back pressure valve 13 is installed on the end pipe of the discharge pipe 9 to stabilize the flow and reduce pulsation.

[0039] Furthermore, the device also includes a mechanical seal system 14; the mechanical seal system 14 includes a first double-end mechanical seal 141 mounted on the stirring shaft 33, a second double-end mechanical seal 142 mounted on the stirring shaft 43, a third double-end mechanical seal 143 mounted on the drive shaft of the discharge pump 8, and a sealing liquid circulation station 144 connected to the above mechanical seals, making the equipment safer and more environmentally friendly.

[0040] Furthermore, the first stirring blade 35 and the second stirring blade 45 are frame-type blades, and the outer edge contour of the frame-type blades is parallel to the inner wall contour of the tube in the reactor.

[0041] After precise metering and premixing, various raw materials are sequentially fed into a two-stage tubular reactor connected in series. The synthesis reaction is completed under independently controllable temperature and stirring conditions. An online viscometer monitors the reaction process and the quality of the final product in real time and feeds the data back to the control module 11 to achieve closed-loop control and stable production.

[0042] 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.

[0043] 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 continuous tubular reaction apparatus for the synthesis of phosphate ester wetting and dispersing agents, characterized in that, Includes a base (1); a static mixing tube (2) is fixedly installed on the base (1), the static mixing tube (2) includes a tube body (21), a static mixer (22) is installed inside the tube body (21), and at least three feed ports (23) are provided on the side wall of the tube body (21). A first tubular reactor (3) and a second tubular reactor (4) are fixedly installed on the base (1). The inlet of the first tubular reactor (3) is connected to the outlet of the static mixing pipe (2), and the inlet of the second tubular reactor (4) is connected to the outlet of the first tubular reactor (3) through a first connecting pipe (5). A vacuum tank (6) is fixedly installed on the base (1). The inlet of the vacuum tank (6) is connected to the outlet of the second tubular reactor (4) through the second connecting pipe (7). An interface is provided on the top of the vacuum tank (6). A discharge pump (8) is fixedly installed on the base (1). The discharge pump (8) includes a pump body (81) and a pump drive motor (82). The drive shaft of the pump body (81) is connected to the output shaft of the pump drive motor (82). The inlet of the discharge pump (8) is connected to the bottom outlet of the vacuum tank (6). The outlet of the discharge pump (8) is connected to a discharge pipe (9). The base (1) is fixedly provided with a control module (11), and is equipped with an operation panel (111) and a power interface (112); the control module (11) is electrically connected to the discharge pump (8), the first tubular reactor (3) and the second tubular reactor (4).

2. The continuous tubular reaction apparatus for the synthesis of phosphate ester wetting and dispersing agents according to claim 1, characterized in that: The first tubular reactor (3) includes a tube body two (31), a temperature control jacket one (32) is provided on the outside of the tube body two (31), a stirring shaft one (33) is provided inside the tube body two (31), a motor one (34) is fixed at the end of the tube body two (31), one end of the stirring shaft one (33) is fixedly connected to the output shaft of the motor one (34) through a coupling, and multiple sets of stirring blades one (35) are provided on the stirring shaft one (33). The structure of the second tubular reactor (4) is the same as that of the first tubular reactor (3). The second tubular reactor (4) includes a tube body (41), a temperature control jacket (42), a stirring shaft (43), a motor (44), and multiple sets of stirring blades (45).

3. The continuous tubular reaction apparatus for the synthesis of phosphate ester wetting and dispersing agents according to claim 2, characterized in that: The control module (11) is equipped with an operation panel (111) and a power interface (112), and is electrically connected to the first motor (34), the second motor (44), the first temperature control jacket (32), the second temperature control jacket (42), the discharge pump (8) and its pump drive motor (82); the operation panel (111) integrates a temperature control unit for adjusting the reaction temperature and a speed control unit for adjusting the stirring speed.

4. The continuous tubular reaction apparatus for the synthesis of phosphate ester wetting and dispersing agents according to claim 1, characterized in that: It also includes an online detection unit (10) and a bypass tank (12) therewith; the online detection unit (10) includes a first online viscometer (101) installed on the first connecting pipe (5) and a second online viscometer (102) installed on the discharge pipe (9); the control module (11) is connected to the first online viscometer (101) and the second online viscometer (102) via a signal cable.

5. A continuous tubular reaction apparatus for the synthesis of phosphate ester wetting and dispersing agents according to claim 4, characterized in that: The first online viscometer (101) and the second online viscometer (102) are online rotary viscometers, and their sensors are respectively inserted into a bypass tank (12) with a stirrer. The bypass tank (12) is equipped with a stirrer.

6. A continuous tubular reaction apparatus for the synthesis of phosphate ester wetting and dispersing agents according to claim 1, characterized in that: The inlet ends of the at least three feed ports (23) are respectively connected to the outlets of three metering pumps.

7. A continuous tubular reaction apparatus for the synthesis of phosphate ester wetting and dispersing agents according to claim 1, characterized in that: The first connecting pipe (5) is an inverted U-shaped pipe with an exhaust valve (51) at its highest point; the outlet of the first tubular reactor (3) and the inlet of the second tubular reactor (4) are both connected to the first connecting pipe (5) through a reducing pipe joint (52).

8. A continuous tubular reaction apparatus for the synthesis of phosphate ester wetting and dispersing agents according to claim 1, characterized in that: A back pressure valve (13) is installed on the end pipe of the discharge pipe (9).

9. A continuous tubular reaction apparatus for the synthesis of phosphate ester wetting and dispersing agents according to claim 2, characterized in that: It also includes a mechanical seal system (14), which includes a first double-end mechanical seal (141) mounted on the first stirring shaft (33), a second double-end mechanical seal (142) mounted on the second stirring shaft (43), a third double-end mechanical seal (143) mounted on the drive shaft of the discharge pump (8), and a sealing liquid circulation station (144) connected to the above mechanical seals.

10. A continuous tubular reaction apparatus for the synthesis of phosphate ester wetting and dispersing agents according to claim 2, characterized in that: The first stirring blade (35) and the second stirring blade (45) are frame blades, and the outer edge contour of the frame blades is parallel to the inner wall contour of the tube of the reactor.

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