Integrated phosphonate continuous synthesis reaction device
By designing an integrated continuous synthesis reactor for phosphate esters, and utilizing a combination of multiple reactors and evaporators, continuous production of phosphate ester products has been achieved. This solves the problem of low production efficiency in existing technologies, improves production efficiency, and has wide applicability.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- SUZHOU CONCEPT MATERIAL TECHNOLOGY CO LTD
- Filing Date
- 2025-07-17
- Publication Date
- 2026-06-12
AI Technical Summary
Existing phosphate ester synthesis processes are difficult to achieve continuous production, resulting in low production efficiency, high costs, and intermittent operation at each stage, making it impossible to operate continuously and stably.
An integrated continuous synthesis reactor for phosphate esters was designed, comprising a vacuum pump structure, a reaction structure, an evaporation structure, a condensation structure, and a neutralization and sedimentation structure. Through the combination of multiple reactors and evaporators, continuous feeding of raw materials and temperature control are achieved, ensuring the continuous progress of the reaction.
It enables continuous production of phosphate ester products, improves production efficiency, has wide applicability and practicality, and can be applied in a variety of production scenarios.
Smart Images

Figure CN224345874U_ABST
Abstract
Description
Technical Field
[0001] This utility model relates to the field of phosphate ester synthesis, specifically an integrated continuous phosphate ester synthesis reaction device. Background Technology
[0002] Phosphate ester synthesis refers to the process of combining phosphorus-containing compounds with alcohols through chemical reactions to generate phosphate esters. Phosphoric acid, phosphorus pentoxide, etc., are generally used as phosphorus sources, and esterification or acylation reactions occur with alcohols of different structures (such as fatty alcohols and aromatic alcohols). During the reaction, the hydroxyl group on the phosphorus atom is replaced by the alkoxy group of the alcohol, forming a phosphate ester with a specific structure.
[0003] Currently, existing phosphate ester synthesis processes have significant limitations in their overall production model, making continuous production difficult. In the esterification stage, the reaction needs to be carried out under specific temperature, pressure, and catalyst conditions. Due to the properties of the reactants and the characteristics of reaction kinetics, the reaction can only be carried out in batches, and the reaction must be stopped and the product processed after reaching a certain extent. The same applies to the reflux stage, where parameters such as the reflux ratio must be adjusted according to the system state, making continuous and stable operation impossible. In the alcohol recovery stage, alcohols need to be separated by means such as distillation. Due to the constraints of separation efficiency and product purity requirements, the process can only be carried out intermittently. Each stage is carried out in segments and intermittently, resulting in low production efficiency and high costs. Utility Model Content
[0004] To solve the aforementioned technical problems, this utility model provides the following technical solution: an integrated phosphate ester continuous synthesis reaction device, comprising a vacuum pump structure, a reaction structure fixedly connected to one end of the vacuum pump structure, an evaporation structure fixedly connected to one end of the reaction structure, a condensation structure fixedly connected to one end of the evaporation structure, and a neutralization and sedimentation structure fixedly connected to one end of the condensation structure. The reaction structure includes a first reactor, a second reactor, and a third reactor, and a second connecting pipe is fixedly connected between the first reactor, the second reactor, and the third reactor.
[0005] Preferably, a third connecting pipe is fixedly connected to one side of the third reactor, a transfer pump is fixed in the middle section of the third connecting pipe, and one end of the third connecting pipe is fixedly connected to the evaporation structure.
[0006] Preferably, the evaporation structure includes a first evaporator, an evaporation pipe is fixedly connected to the top of the first evaporator, a fourth connecting pipe is fixedly connected to the bottom of the first evaporator, a second evaporator is fixedly connected to one end of the fourth connecting pipe, the second evaporator has the same structure as the first evaporator, and the second evaporator is fixedly connected to the condensation structure.
[0007] Preferably, the condensation structure includes a condenser, and a fifth connecting pipe is fixedly connected to the bottom end of the condenser. The fifth connecting pipe is fixedly connected to the neutralization and settling structure.
[0008] Preferably, the neutralization and sedimentation structure includes a neutralization vessel, a sixth connecting pipe is fixedly connected to the top of the neutralization vessel, a sedimentation pipe is fixedly connected to one end of the sixth connecting pipe, a filter is fixedly connected to the bottom end of the sedimentation pipe, and a drain pipe is fixedly connected to the bottom end of the filter.
[0009] Preferably, the vacuum pump structure includes a pump body, and a first connecting pipe is fixedly connected to the output end of the pump body, with one end of the first connecting pipe fixedly connected to the first reactor.
[0010] Compared with the prior art, the beneficial effects of this utility model are:
[0011] This invention proposes an integrated continuous synthesis reactor for phosphate esters. This reactor utilizes multiple built-in structures to achieve continuous feeding of raw materials for phosphate ester production, ensuring a stable supply of raw materials. Simultaneously, the reactor can adjust the temperature according to the needs of different reaction stages, enabling continuous reaction. From raw material input to final product output, the entire process is completed seamlessly, significantly improving production efficiency and demonstrating strong practicality. It can be widely applied in various related production scenarios, showcasing broad applicability. Attached Figure Description
[0012] The present invention will be further described below with reference to the accompanying drawings:
[0013] Figure 1 This is a schematic diagram of the structure of the present invention. Figure 1 ;
[0014] Figure 2 This is a schematic diagram of the structure of the present invention. Figure 2 .
[0015] In the diagram: 1. Vacuum pump structure; 11. Pump body; 12. First connecting pipe; 2. Reaction structure; 21. First reactor; 22. Second reactor; 23. Third reactor; 24. Second connecting pipe; 25. Third connecting pipe; 26. Transfer pump; 3. Evaporation structure; 31. First evaporator; 32. Evaporation gas pipe; 33. Fourth connecting pipe; 34. Second evaporator; 4. Condensation structure; 41. Condenser; 42. Fifth connecting pipe; 5. Neutralization and settling structure; 51. Neutralization vessel; 52. Sixth connecting pipe; 53. Settling pipe; 54. Filter; 55. Drain pipe. Detailed Implementation
[0016] To more clearly illustrate the overall concept of this utility model, a detailed description will be provided below with reference to the accompanying drawings.
[0017] Please see Figures 1 to 2 The present invention provides the following technical solution: an integrated phosphate ester continuous synthesis reaction device, including a vacuum pump structure 1, a reaction structure 2 fixedly connected to one end of the vacuum pump structure 1, an evaporation structure 3 fixedly connected to one end of the reaction structure 2, a condensation structure 4 fixedly connected to one end of the evaporation structure 3, a neutralization and sedimentation structure 5 fixedly connected to one end of the condensation structure 4, and a reaction structure 2 including a first reactor 21, a second reactor 22 and a third reactor 23, with a second connecting pipe 24 fixedly connected between the first reactor 21, the second reactor 22 and the third reactor 23;
[0018] This reaction device can utilize multiple built-in structures to achieve continuous feeding of raw materials for the production of phosphate esters, ensuring a stable supply of raw materials. At the same time, the device can adjust the temperature according to the needs of different reaction stages to achieve continuous reaction. From raw material input to final product output, the entire process is completed in one go, which not only greatly improves production efficiency, but also has strong practicality and can be widely used in a variety of related production scenarios, demonstrating broad applicability.
[0019] The vacuum pump structure 1 includes a pump body 11, and a first connecting pipe 12 is fixedly connected to the output end of the pump body 11. One end of the first connecting pipe 12 is fixedly connected to the first reactor 21.
[0020] A third connecting pipe 25 is fixedly connected to one side of the third reactor 23. A transfer pump 26 is fixedly connected to the middle section of the third connecting pipe 25. One end of the third connecting pipe 25 is fixedly connected to the evaporation structure 3.
[0021] Evaporation structure 3 includes a first evaporator 31, an evaporation pipe 32 is fixedly connected to the top of the first evaporator 31, a fourth connecting pipe 33 is fixedly connected to the bottom of the first evaporator 31, a second evaporator 34 is fixedly connected to one end of the fourth connecting pipe 33, the second evaporator 34 has the same structure as the first evaporator 31, and the second evaporator 34 is fixedly connected to the condensation structure 4.
[0022] In use, a feed pipe is connected to the surface of the first reactor 21 via a flange joint. The pump body 11 is started, and under negative pressure, phosphorus oxychloride and alcohols are fed into the first reactor 21 in a 1:4 ratio via the external feed pipe. At the same time, 0.1% of the metal halide of phosphorus oxychloride is added. All three reactors are equipped with built-in circulation pumps for cooling. When the vacuum degree in the first reactor 21 reaches above 0.09 MPa, the pressure in the system decreases. According to the principle of gas diffusion, hydrogen chloride, a byproduct of the reaction between phosphorus oxychloride and alcohols, is more likely to escape from the reaction liquid. At this time, the external hydrochloric acid absorption structure is started. The hydrochloric acid absorption structure consists of four hydrochloric acid absorption towers, four circulation tanks, and a vacuum pump to treat the hydrogen chloride gas, a byproduct of the reaction.
[0023] By adjusting the power of the circulating pump, the internal temperature of the first reactor 21 is controlled at around 10-20℃. When the liquid level in the first reactor 21 reaches a certain height, the liquid enters the second reactor 22 through the second connecting pipe 24 on the left, controlling the internal temperature of the second reactor 22 at around 30-40℃. When the liquid level in the second reactor 22 reaches a certain height, the liquid enters the third reactor 23 through the second connecting pipe 24 on the right, controlling the internal temperature of the third reactor 23 at around 60-90℃. When the liquid level in the third reactor 23 reaches a certain height, the transfer pump 26 is started to transfer the mixed liquid to the first evaporator 31 for evaporation and concentration. By adjusting the power of the evaporator, the temperature of the first evaporator 31 is maintained at around 100-120℃. The evaporated alcohol gas is subsequently recovered through the evaporation gas pipe 32. The mixed liquid enters the second evaporator 34 through the fourth connecting pipe 33 for further evaporation and concentration, maintaining the temperature of the second evaporator 34 at around 130-140℃. The remaining liquid after evaporation enters the condensation structure 4.
[0024] The condensing structure 4 includes a condenser 41, and a fifth connecting pipe 42 is fixedly connected to the bottom end of the condenser 41. The fifth connecting pipe 42 is fixedly connected to the neutralization and settling structure 5.
[0025] The neutralization and settling structure 5 includes a neutralization vessel 51, a sixth connecting pipe 52 fixedly connected to the top of the neutralization vessel 51, a settling pipe 53 fixedly connected to one end of the sixth connecting pipe 52, a filter 54 fixedly connected to the bottom end of the settling pipe 53, and a drain pipe 55 fixedly connected to the bottom end of the filter 54.
[0026] After evaporation, the remaining liquid enters the condenser 41 and is cooled to become a crude product. When a certain amount of crude product is collected, the electrically controlled valve installed on the surface of the fifth connecting pipe 42 will transfer a fixed amount of crude product through the fifth connecting pipe 42 into the neutralization tank 51 for neutralization to adjust the pH value of the liquid to about 12-13. By installing an electric heating element in the neutralization tank 51, electrical energy is converted into heat energy to heat the material to achieve dehydration of the liquid. Water vapor is discharged through the top of the neutralization tank 51. The temperature inside the neutralization tank 51 is controlled at about 120°C and maintained for one hour. After the liquid cools down, it enters the settling pipe 53 through the sixth connecting pipe 52 and is filtered by the filter 54 for 12 hours. After that, the liquid is transferred to the finished product receiving tank through the drain pipe 55 to complete the storage.
[0027] During the reaction, the design of three reactors ensures the reaction time, and the different temperatures in the three reactors ensure the reaction is complete and reduces side reactions. Both evaporators are negative pressure evaporators, which can recover and reuse excess alcohol raw materials.
[0028] The contents not described in detail in this specification do not improve upon this application and are all prior art known to those skilled in the art, and therefore are not described in detail.
[0029] Those skilled in the art should understand that the discussion of any of the above embodiments is merely exemplary and is not intended to imply that the scope of the present invention includes the claims being limited to these examples; within the framework of the present invention, the technical features of the above embodiments or different embodiments can also be combined, the steps can be implemented in any order, and there are many other variations of the different aspects of the present invention as described above, which are not provided in the details for the sake of brevity.
[0030] This utility model is intended to cover all such substitutions, modifications, and variations that fall within the broad scope of the appended claims. Therefore, any omissions, modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of this utility model should be included within the protection scope of this utility model.
Claims
1. An integrated continuous synthesis reactor for phosphate esters, characterized in that: The system includes a vacuum pump structure (1), one end of which is fixedly connected to a reaction structure (2), one end of which is fixedly connected to an evaporation structure (3), one end of which is fixedly connected to a condensation structure (4), and one end of which is fixedly connected to a neutralization and sedimentation structure (5). The reaction structure (2) includes a first reactor (21), a second reactor (22), and a third reactor (23). A second connecting pipe (24) is fixedly connected between the first reactor (21), the second reactor (22), and the third reactor (23).
2. The integrated phosphate ester continuous synthesis reaction apparatus according to claim 1, characterized in that: A third connecting pipe (25) is fixedly connected to one side of the third reactor (23), a transfer pump (26) is fixed in the middle section of the third connecting pipe (25), and one end of the third connecting pipe (25) is fixedly connected to the evaporation structure (3).
3. The integrated phosphate ester continuous synthesis reaction apparatus according to claim 2, characterized in that: The evaporation structure (3) includes a first evaporator (31), an evaporation pipe (32) is fixedly connected to the top of the first evaporator (31), a fourth connecting pipe (33) is fixedly connected to the bottom of the first evaporator (31), a second evaporator (34) is fixedly connected to one end of the fourth connecting pipe (33), the second evaporator (34) has the same structure as the first evaporator (31), and the second evaporator (34) is fixedly connected to the condensation structure (4).
4. The integrated phosphate ester continuous synthesis reaction apparatus according to claim 3, characterized in that: The condensation structure (4) includes a condenser (41), and a fifth connecting pipe (42) is fixedly connected to the bottom end of the condenser (41). The fifth connecting pipe (42) is fixedly connected to the neutralization and settling structure (5).
5. The integrated phosphate ester continuous synthesis reaction apparatus according to claim 4, characterized in that: The neutralization and settling structure (5) includes a neutralization vessel (51), a sixth connecting pipe (52) is fixedly connected to the top of the neutralization vessel (51), a settling pipe (53) is fixedly connected to one end of the sixth connecting pipe (52), a filter (54) is fixedly connected to the bottom end of the settling pipe (53), and a drain pipe (55) is fixedly connected to the bottom end of the filter (54).
6. The integrated phosphate ester continuous synthesis reaction apparatus according to claim 5, characterized in that: The vacuum pump structure (1) includes a pump body (11), and a first connecting pipe (12) is fixedly connected to the output end of the pump body (11). One end of the first connecting pipe (12) is fixedly connected to the first reactor (21).