High-efficiency separation equipment for top synthesis reaction based on vacuum dewatering
By using vacuum dehydration technology and high-temperature spraying of molecular sieves, the problems of low separation efficiency and large equipment footprint in traditional TOP synthesis reactions have been solved, achieving efficient and stable separation results and reducing energy consumption and the frequency of molecular sieve replacement.
Patent Information
- Application Number
- CN202522035347.6
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- Filing Date
- 2025-09-22
- Publication Date
- 2026-08-25
- Estimated Expiration
- 2035-09-22
AI Technical Summary
Traditional TOP synthesis reaction separation technology relies on precise control of pH value and ligand concentration, and the extraction efficiency is affected by emulsification, resulting in large fluctuations in yield. In addition, traditional equipment has a large footprint, high energy consumption, and high environmental pressure, and molecular sieves need to be disassembled and replaced regularly.
Vacuum dehydration technology is employed, using a vacuum pump, shut-off valve, and vacuum pipeline to ensure that the reaction group and separator components operate under the same vacuum level. The heating jacket and electrically controlled valve are used to achieve high-temperature scavenging of the molecular sieve, enabling in-situ regeneration of the molecular sieve and avoiding disassembly and replacement.
It achieves efficient separation, lowers the boiling point of water, promotes dehydration, reduces equipment footprint and energy consumption, saves molecular sieve replacement time, and improves the stability of yield.
Smart Images
Figure CN224672278U_ABST
Abstract
Description
Technical Field
[0001] This utility model relates to the field of high-efficiency separation technology, specifically a high-efficiency separation device for TOP synthesis reaction based on vacuum dehydration. Background Technology
[0002] Traditional separation techniques face significant challenges in the synthesis of TOP (trioctylphosphine oxide). Existing processes often employ liquid-liquid extraction, such as using di(2-ethylhexyl) phosphate (P204) as a complexing agent to separate rare earth ions from TOP through an acidic complexation system. However, this process relies on precise control of parameters such as pH and ligand concentration, and the extraction efficiency is significantly affected by emulsification, leading to large yield fluctuations. Furthermore, traditional thermal drying equipment requires multi-stage processing, resulting in large footprints, high energy consumption, and significant environmental impact. Additionally, the molecular sieves in the dryer need to be periodically disassembled and replaced, increasing costs and wasting time. Therefore, we propose a high-efficiency separation device for the TOP synthesis reaction based on vacuum dehydration. Utility Model Content
[0003] To address the aforementioned technical problems, this application provides a high-efficiency separation device for TOP synthesis reaction based on vacuum dehydration, comprising a vacuum pump, a shut-off valve fixedly connected to the output end of the vacuum pump, a vacuum pipeline fixedly connected to the input end of the shut-off valve, a reaction assembly fixedly connected to the right end of the vacuum pipeline, a support frame provided on the lower side of the outer surface of the reaction assembly, a separator component fixedly connected to the left end of the vacuum pipeline, an electrically controlled valve I fixedly connected to the lower end of the separator component, a collector I connected to the output end of the electrically controlled valve I, a separation mechanism provided on the left side of the outer surface of the separator component, and a collector II provided on the lower left side of the separation mechanism.
[0004] In some embodiments, the reaction assembly includes an upper tank, with two pipes (III) fixedly connected to the upper left side of the outer surface of the upper tank, a drive motor fixedly connected to the upper end of the upper tank, a pressure gauge (I) fixedly connected to the right side of the outer surface of the upper tank, a stirring roller fixedly connected to the output end of the drive motor, a lower tank fixedly connected to the lower end of the upper tank, a pipe (I) fixedly connected to the upper left side of the outer surface of the lower tank, an outer tank fixedly connected to the outer surface of the lower tank, three triangular fixing brackets fixedly connected in a ring array to the lower side of the outer tank, two pipes (II) fixedly connected to the right side of the outer tank, a pressure gauge (II) fixedly connected to the lower rear side of the outer tank, and a drain valve fixedly connected to both the lower end of the lower tank and the lower end of the outer tank.
[0005] In some embodiments, the outer surfaces of the three triangular fixing frames are all fixedly connected to the support frame by bolts, and the first pipe is fixedly connected to the right end of the overhead pipe by bolts.
[0006] In some embodiments, the separation mechanism includes a pipe four, a control component is provided in the middle of the outer surface of the pipe four, a drying group is fixedly connected to the lower end of the pipe four, a condenser is fixedly connected to the lower end of the drying group, and interfaces are provided on the left and right sides of the upper surface of the outer surface of the condenser.
[0007] In some embodiments, the right end of the fourth pipe is bolted to the left end of the vacuum pipe, and the output end of the condenser is bolted to the input end of the second collector.
[0008] In some embodiments, the drying assembly includes an upper shell, a lower shell fixedly connected to the lower end of the upper shell, a heating sleeve provided on the outer surface of the lower shell, a molecular sieve provided in the inner cavity of the lower shell and the inner cavity of the upper shell, a gas supply pipe fixedly connected to the upper left side of the outer surface of the lower shell, and an electrically controlled valve II fixedly connected to the left end of the gas supply pipe.
[0009] In some embodiments, the upper end of the upper housing is fixedly connected to the lower end of the pipe, and the lower end of the lower housing is fixedly connected to the condenser input end.
[0010] This utility model has at least the following beneficial effects: This invention utilizes the combined use of the upper shell, lower shell, and molecular sieve to enable the device to not only adsorb trace amounts of moisture in the solvent for drying, but also to perform high-temperature spraying of the molecular sieve through the combined use of the heating jacket, the second electrically controlled valve, the gas supply pipe, and helium gas. This achieves in-situ regeneration of the molecular sieve without the need for disassembly or replacement, saving time wasted on maintenance.
[0011] In the specific implementation process, the combined use of vacuum pumps, shut-off valves and vacuum pipelines plays a role in vacuuming the reaction group and separator components, ensuring that the reaction group and separator components are under the same vacuum level at the same time, maintaining the system pressure, lowering the boiling point of water to promote dehydration. Attached Figure Description
[0012] Figure 1 This is a schematic diagram of the overall structure of this utility model; Figure 2 This is a schematic diagram of the overall structure of this utility model from another perspective; Figure 3 This is a schematic diagram of the reaction assembly of this utility model; Figure 4 This is a schematic diagram of the reaction assembly of this utility model from another perspective; Figure 5 This is a schematic diagram of the separation mechanism of this utility model; Figure 6 This is a schematic diagram of the drying assembly of this utility model; Figure 7 This is a schematic diagram of the drying assembly of this utility model from another perspective.
[0013] In the diagram: 1. Vacuum pump; 2. Shut-off valve; 3. Vacuum pipeline; 4. Reaction group; 41. Upper tank; 42. Pipeline 1; 43. Lower tank; 44. Outer tank; 45. Stirring roller; 46. Drain valve; 47. Triangular fixing frame; 48. Pipeline 2; 49. Pipeline 3; 491. Pressure gauge 1; 492. Drive motor; 493. Pressure gauge 2; 5. Support frame; 6. Separator components; 7. Electrically controlled valve 1; 8. Collector 1; 81. Collector 2; 9. Separation mechanism; 91. Control components; 92. Pipeline 4; 93. Drying group; 931. Upper shell; 932. Lower shell; 933. Heating jacket; 934. Electrically controlled valve 2; 935. Gas supply pipe; 936. Molecular sieve; 94. Condenser; 95. Interface. Detailed Implementation
[0014] The technical solutions of the present utility model will be clearly and completely described below with reference to the accompanying drawings of the embodiments. Obviously, the described embodiments are only some embodiments of the present utility model, and not all embodiments. Based on the embodiments of the present utility model, all other embodiments obtained by those of ordinary skill in the art without creative effort are within the protection scope of the present utility model. Example 1:
[0015] Please see Figure 1-4 This utility model provides a technical solution: a high-efficiency separation device for TOP synthesis reaction based on vacuum dehydration, including a vacuum pump 1, characterized in that: a shut-off valve 2 is fixedly connected to the output end of the vacuum pump 1, a vacuum pipeline 3 is fixedly connected to the input end of the shut-off valve 2, a reaction group 4 is fixedly connected to the right end of the vacuum pipeline 3, a support frame 5 is provided on the lower side of the outer surface of the reaction group 4, a separator component 6 is fixedly connected to the left end of the vacuum pipeline 3, an electrically controlled valve 7 is fixedly connected to the lower end of the separator component 6, a collector 8 is connected to the output end of the electrically controlled valve 7, a separation mechanism 9 is provided on the left side of the outer surface of the separator component 6, and a collector 81 is provided on the lower left side of the separation mechanism 9.
[0016] It should be noted that the specific installation methods, circuit connections, and control methods of the vacuum pump 1, shut-off valve 2, and solenoid valve 7 in this utility model are all conventional designs, representing standard design practices for designers. The shut-off valve 2 consists of a vacuum gauge and a vacuum shut-off valve. The vacuum gauge is installed to monitor the system pressure in real time, and the vacuum shut-off valve facilitates isolation of the vacuum source during maintenance. The separator component 6 consists of a cylindrical glass container, a built-in coalescing filter element, and a liquid level sensor, among other components. When used in conjunction with the solenoid valve 7, it can automatically discharge the water layer and the upper layer... The solvent enters the separation unit 9 for oil-water separation. After drying and condensation in the separation unit 9, the solvent is collected by collector 81, which is equipped with a nitrogen protection device to prevent solvent oxidation. A vacuum pump 1, in conjunction with the shut-off valve 2 and vacuum pipeline 3, performs vacuum suction on the reaction group 4 and separator component 6, ensuring that both are under the same vacuum level. This maintains the system pressure, lowers the boiling point of water, and promotes dehydration. The addition of reaction group 4 facilitates the TOP synthesis reaction. The reaction group 4 includes an upper tank 41. Two pipes 49 are fixedly connected to the upper left side of the outer surface of the upper tank 41. A drive motor 492 is fixedly connected to the upper end of the upper tank 41. A pressure gauge 491 is fixedly connected to the right side of the outer surface of the upper tank 41. A stirring roller 45 is fixedly connected to the output end of the drive motor 492. A lower tank 43 is fixedly connected to the lower end of the upper tank 41. A pipe 42 is fixedly connected to the upper left side of the outer surface of the lower tank 43. An outer tank 44 is fixedly connected to the outer surface of the lower tank 43. Three triangular brackets 47 are fixedly connected to the lower side of the outer surface of the outer tank 44 in a ring array. Two pipes 48 are fixedly connected to the right side of the outer surface of the outer tank 44. A pressure gauge 493 is fixedly connected to the lower rear side of the outer surface of the outer tank 44. A drain valve 46 is fixedly connected to the lower end of the lower tank 43 and the lower end of the outer tank 44. The outer surfaces of the three triangular brackets 47 are all fixedly connected to the support frame 5 by bolts. Pipe 42 is fixedly connected to the right end of the vacuum pipe 3 by bolts.
[0017] It should be noted that the specific installation method, circuit connection method, and control method of the drive motor 492 in this utility model are all conventional designs and are standard design methods used by designers. Heat transfer oil is added between the lower tank 43 and the outer tank 44 and connected to external equipment through two pipes 48 to achieve heat transfer oil circulation and temperature control. Then, the drive motor 492 is started to drive the stirring roller 45 to rotate in the inner cavity of the lower tank 43 for the synthesis reaction of TOP. In addition, two pipes 49 are used for the low-temperature batch feeding of octanol and 2, respectively, to avoid local overheating. Example 2:
[0018] Please see Figure 5-7This utility model provides a technical solution: a high-efficiency separation device for TOP synthesis reaction based on vacuum dehydration. The separation mechanism 9 includes a pipe 4 92, a control component 91 is provided in the middle of the outer surface of the pipe 4 92, a drying group 93 is fixedly connected to the lower end of the pipe 4 92, a condenser 94 is fixedly connected to the lower end of the drying group 93, and interfaces 95 are provided on both the left and right sides of the upper side of the outer surface of the condenser 94. The right end of the pipe 4 92 is connected to the left end of the vacuum pipe 3 by bolts, and the output end of the condenser 94 is connected to the input end of the collector 2 81 by bolts. The drying unit 93 includes an upper shell 931, a lower shell 932 fixedly connected to the lower end of the upper shell 931, a heating sleeve 933 on the outer surface of the lower shell 932, a molecular sieve 936 in the inner cavity of the lower shell 932 and the inner cavity of the upper shell 931, a gas supply pipe 935 fixedly connected to the upper left side of the outer surface of the lower shell 932, an electric control valve 934 fixedly connected to the left end of the gas supply pipe 935, the upper end of the upper shell 931 fixedly connected to the lower end of the pipe 92, and the lower end of the lower shell 932 fixedly connected to the input end of the condenser 94.
[0019] It should be noted that control component 91 consists of a shut-off valve, a temperature sensor, and a pressure gauge. The shut-off valve facilitates module isolation during maintenance. The specific installation methods, circuit connections, and control methods of the shut-off valve, temperature sensor, solenoid valve 934, and heating jacket 933 are all conventional designs, representing standard design practices. The upper solvent enters pipe 92, then flows into the inner cavities of the upper and lower shells 931 and 932. It is dried by the adsorption of trace amounts of moisture by molecular sieve 936, and then enters the condenser 94. The condenser 94 is equipped with two ports 95 for easy connection to external equipment, allowing the -10°C chilled brine to circulate in the outer cavity of the condenser 94. This ensures that the HCl and solvent vapor in the inner cavity of the condenser 94 are fully condensed. In addition, the heating jacket 933 is activated to heat the inner cavities of the upper shell 931 and the lower shell 932. Then, the electronically controlled valve 934 is opened to allow nitrogen to enter the inner cavity of the lower shell 932 through the gas supply pipe 935 and purge the molecular sieve 936, achieving in-situ regeneration of the molecular sieve without the need to disassemble or replace it.
[0020] 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.
[0021] 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 high-efficiency separation device based on vacuum dehydration TOP synthesis reaction application, comprising a vacuum pump (1), characterized in that: The output end of the vacuum pump (1) is fixedly connected with a stop valve (2), the input end of the stop valve (2) is fixedly connected with a vacuum pipeline (3), the right end of the vacuum pipeline (3) is fixedly connected with a reaction group (4), the lower side of the outer surface of the reaction group (4) is provided with a support frame (5), the left end of the vacuum pipeline (3) is fixedly connected with a separator component (6), the lower end of the separator component (6) is fixedly connected with an electric control valve I (7), the output end of the electric control valve I (7) is connected with a collector I (8), the left side of the outer surface of the separator component (6) is provided with a separation mechanism (9), and the lower part of the left side of the separation mechanism (9) is provided with a collector II (81).
2. The high efficient separation apparatus for vacuum dehydration based TOP synthesis reaction according to claim 1, characterized in that: The reaction group (4) comprises an upper jar body (41), the left part of the upper side of the outer surface of the upper jar body (41) is fixedly connected with two pipeline threes (49), the upper end of the upper jar body (41) is fixedly connected with a driving motor (492), the right side of the outer surface of the upper jar body (41) is fixedly connected with a pressure gauge I (491), the output end of the driving motor (492) is fixedly connected with a stirring roller (45), the lower end of the upper jar body (41) is fixedly connected with a lower jar body (43), the upper left side of the outer surface of the lower jar body (43) is fixedly connected with a pipeline I (42), the outer surface of the lower jar body (43) is fixedly connected with an outer jar body (44), the lower side of the outer surface of the outer jar body (44) is fixedly connected with three triangular fixing frames (47) in an annular array, the right side of the outer surface of the outer jar body (44) is fixedly connected with two pipeline twos (48), the lower rear part of the outer surface of the outer jar body (44) is fixedly connected with a pressure gauge II (493), and the lower end of the lower jar body (43) and the lower end of the outer jar body (44) are fixedly connected with a drain valve (46) in common.
3. The high efficient separation device for vacuum dehydration based TOP synthesis reaction according to claim 2, characterized in that: The outer surfaces of the three triangular fixing frames (47) are fixedly connected with the support frame (5) in common through bolts, and the pipeline I (42) is fixedly connected with the right end of the vacuum pipeline (3) through bolts.
4. The high efficient separation apparatus for vacuum dehydration based TOP synthesis reaction of claim 1, wherein: The separation mechanism (9) comprises a pipeline four (92), the middle part of the outer surface of the pipeline four (92) is provided with a control component (91), the lower end of the pipeline four (92) is fixedly connected with a drying group (93), the lower end of the drying group (93) is fixedly connected with a condenser (94), and the upper side of the outer surface of the condenser (94) is provided with an interface (95) on the left and right.
5. The high efficient separation device for vacuum dehydration based TOP synthesis reaction according to claim 4, characterized in that: The right end of the pipeline four (92) is connected with the left end of the vacuum pipeline (3) through bolts, and the output end of the condenser (94) is connected with the input end of the collector II (81) through bolts.
6. The high efficient separation device for vacuum dehydration based TOP synthesis reaction of claim 4, wherein: The drying group (93) comprises an upper shell (931), the lower end of the upper shell (931) is fixedly connected with a lower shell (932), the outer surface of the lower shell (932) is provided with a heating jacket (933), the inner cavities of the lower shell (932) and the upper shell (931) are provided with a molecular sieve (936) in common, the upper left side of the outer surface of the lower shell (932) is fixedly connected with a gas conveying pipe (935), and the left end of the gas conveying pipe (935) is fixedly connected with an electric control valve II (934).
7. The high efficient separation apparatus for vacuum dehydration based TOP synthesis reaction of claim 6, wherein: The upper shell (931) is fixedly connected with the lower end of the pipeline four (92), and the lower shell (932) is fixedly connected with the input end of the condenser (94).