An intermediate catalytic device for the synthesis of o-phenylphenol
By employing a combination of reboiler, distillation column, condenser and water separator in the synthesis of o-phenylphenol, the problem of poor cooling in the cyclohexanone dimerization reactor was solved, achieving high reaction efficiency and low energy consumption, extending the service life of the filter and reducing production costs.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- JINING BANGDA COAL CHEM CO LTD
- Filing Date
- 2025-08-14
- Publication Date
- 2026-07-17
AI Technical Summary
In the existing technology, the cooling effect of the cyclohexanone dimerization reactor is not good, which leads to reduced reaction efficiency, increased energy consumption, and the direct participation of high-temperature catalyst in filtration will damage the filter and shorten its service life.
The device employs a combination of reboiler, distillation column, condenser and water separator. Through steam-water separation and heating plate filtration, the temperature influence of liquid cyclohexanone is reduced, the reaction efficiency is improved, and energy consumption is reduced and filter life is extended through a circulating heat exchange system.
It improved the efficiency of the o-phenylphenol synthesis reaction, reduced energy consumption, extended the service life of the filter, and reduced production costs through resource recycling.
Smart Images
Figure CN224507039U_ABST
Abstract
Description
Technical Field
[0001] This utility model relates to the field of o-phenylphenol production technology, specifically to an intermediate catalytic device for synthesizing o-phenylphenol. Background Technology
[0002] o-Phenylacetol (OPP) is an important fine chemical product and organic intermediate, widely used in sterilization and preservation, dyeing and printing auxiliaries, and surfactants. It is also used in the synthesis of new plastics, resins, and polymer materials as a stabilizer and flame retardant. Currently, the world's production and research on OPP mainly focuses on the preparation of OPP from cyclohexanone. Specifically, cyclohexanone is used as a raw material, and under acid catalysis, it undergoes condensation and dehydration to obtain the intermediates 2-(1-cyclohexenyl)cyclohexanone and 2-cyclohexylalkylenecyclohexanone, which are then dehydrogenated to synthesize o-phenylphenol.
[0003] Patent CN201420665565.7 discloses an intermediate device for producing o-phenylphenol, including a reactor connected to a water return mechanism and a catalyst recovery mechanism. The water return mechanism includes a cooler at the top of the reactor and a water distributor connected to the cooler, which splits the water flow into two paths: one connected to a drain pipe, and the other connected to and returning to the reactor. The catalyst recovery mechanism includes a circulation pump at the bottom of the reactor and a filter connected to the circulation pump, with the filter outlet connected to the top of the reactor. However, since the cyclohexanone dimerization process is exothermic, directly returning the cooled cyclohexanone to the reaction solution in this device lowers the reaction temperature, thus affecting the reaction process to some extent, leading to reduced reaction efficiency and increased energy consumption. Furthermore, because the catalyst temperature after the reaction in the reactor is high, directly pumping the high-temperature catalyst into the filter can damage the internal filter layer, shortening the filter's lifespan and increasing costs. Utility Model Content
[0004] This invention addresses the shortcomings of existing technologies by providing an intermediate catalytic device for the synthesis of o-phenylphenol. This device reduces the impact of low-temperature cyclohexanone on the temperature of the reaction solution, thereby ensuring reaction efficiency. Furthermore, it avoids the direct involvement of high-temperature catalysts in filtration, thus extending filter life and reducing energy consumption.
[0005] This utility model is achieved through the following technical solution: a catalytic device for synthesizing o-phenylphenol intermediates, comprising a reboiler, a distillation column, a condenser, and a water separator. The distillation column is fixed to the top of the reboiler, and its top outlet is connected to the steam inlet of the condenser. The condensate outlet of the condenser is connected to the inlet of the water separator. The distillation column includes a stripping section, a heating section, and a rectification section fixedly connected from bottom to top. The heating section is equipped with a steam-water separator, multiple heating plates, and a filter screen. The steam-water separator is fixed inside the heating section, and the multiple heating plates are fixed to the bottom of the steam-water separator, and the multiple heating plates are evenly distributed radially and extend vertically. The filter screen is fixed to the bottom of the multiple heating plates. The reflux outlet of the water separator is connected to the top inlet of the steam-water separator.
[0006] This process utilizes a reboiler to heat the reaction mixture for a condensation reaction. The vapor from the azeotropic reaction of water and cyclohexanone is drawn upwards through the stripping section. The upward-flowing vapor passes through the heating and rectification sections before condensing into liquid in the condenser. The liquid wastewater is separated and discharged by a water separator. The liquid cyclohexanone is recirculated to the steam-water separator in the heating section to separate it from the vapor. The liquid cyclohexanone flows downwards, is heated by heating plates, filtered through a filter, and then recirculated back into the reboiler to participate in the reaction again. This process, through the separation by the steam-water separator, prevents the liquid cyclohexanone from affecting the upward flow of vapor, ensuring efficient rectification. Heating the low-temperature liquid cyclohexanone with heating plates reduces the impact of the recirculated cyclohexanone on the reaction, thereby improving reaction efficiency and reducing energy consumption. Furthermore, the filter removes impurities from the liquid cyclohexanone, ensuring reaction quality and slowing down the recirculation rate, further guaranteeing the reaction effect within the reboiler. Therefore, the product quality is more stable and the process is more practical.
[0007] As an optimization, the heating plate has a serpentine curved structure. In this optimized solution, when liquid cyclohexanone is refluxed, the heating plate guides the flow of liquid cyclohexanone, and the serpentine curved structure of the heating plate increases the contact area, thereby increasing the heating temperature.
[0008] As an optimization, the filter screen is designed with a cone-shaped structure. This optimized cone-shaped filter screen can retain more impurities, extend the cleaning interval, and is more convenient to use.
[0009] As an optimization, the system also includes a cooler, a transfer pump, and a filter. The discharge port of the reboiler is connected to the feed inlet of the cooler, the feed outlet of the cooler is connected to the input of the transfer pump, the output of the transfer pump is connected to the inlet of the filter, and the outlet of the filter is connected to the return port of the reboiler. In this optimized scheme, the catalyst feed liquid in the reboiler is discharged through the discharge port. After the high-temperature feed liquid is cooled by the cooler, it is pumped into the filter for filtration by the transfer pump. The temperature of the catalyst feed liquid is reduced by the cooler, thereby avoiding damage to the filter layer and improving the filter life.
[0010] As an optimization, a preheater is also included, the outlet of which is connected to the inlet of the reboiler, and a heating coil is installed inside the preheater. This optimized scheme uses the preheater to remove residual heat from the reaction raw materials before introducing them into the reboiler for azeotrope, reducing the azeotropic time and thus further reducing energy consumption and improving reaction efficiency.
[0011] As an optimization, the heat exchange outlets of the cooler and condenser are both connected to the input port of the heating coil. This optimized solution utilizes the heat source after heat exchange within the cooler and condenser as the heating source for the heating coil, achieving resource recycling, reducing energy consumption, and saving resources.
[0012] As an optimization, a cooling tower is also included. The output port of the heating coil is connected to the input port of the cooling tower, and the heat exchange inlets of the cooler and condenser are both connected to the output port of the cooling tower. In this optimized solution, the heating source of the heating coil is cooled back into a cold source by the cooling tower, and the cold source is reused as the heat exchange medium of the cooler and condenser, thus forming a complete circulating heat exchange system, saving a lot of resources and greatly reducing costs.
[0013] The beneficial effects of this invention are as follows: The reaction mixture undergoes a condensation reaction via reboiler heating. The vapor from the azeotropic reaction of water and cyclohexanone is drawn upwards through the stripping section. The vapor then passes through the heating and rectification sections before entering the condenser and condensing into liquid. The liquid wastewater is separated and discharged by a water separator. The liquid cyclohexanone is returned to the steam-water separator in the heating section to separate from the vapor. The liquid cyclohexanone is discharged downwards, heated by a heating plate, filtered through a filter screen, and then returned to the reboiler to participate in the reaction again. This process, through the separation by the steam-water separator, avoids the liquid cyclohexanone affecting the upward flow of vapor, ensuring the rectification effect. Heating the low-temperature liquid cyclohexanone by the heating plate reduces the impact of the returned cyclohexanone on the reaction, thereby improving reaction efficiency and reducing energy consumption. Furthermore, the filter screen filters impurities from the liquid cyclohexanone, ensuring reaction quality and slowing down the reflux rate of the liquid cyclohexanone, further ensuring the reaction effect within the reboiler. Therefore, the product quality is more stable and the product is more practical. The catalyst liquid in the reboiler is discharged through the discharge port. After the high temperature of the liquid is cooled by the cooler, it is pumped into the filter by the transfer pump for filtration. The temperature of the catalyst liquid is reduced by the cooler, thereby avoiding damage to the filter layer and improving the filter life. The heat source after heat exchange in the cooler and condenser is used as the heat source for the heating coil. The heat source of the heating coil is cooled back into a cold source by the cooling tower. The cold source is reused as the heat exchange medium in the cooler and condenser, thus forming a complete circulating heat exchange system, saving a lot of resources and greatly reducing costs. Attached Figure Description
[0014] Figure 1 This is a flowchart of the present utility model; Figure 2 for Figure 1 Enlarged view of part A; As shown in the figure: 1. Reboiler; 2. Distillation column; 21. Stripping section; 22. Heating section; 23. Rectifying section; 24. Steam-water separator; 25. Heating plate; 26. Filter screen; 3. First pipeline; 4. Condenser; 5. Second pipeline; 6. Water separator; 7. Third pipeline; 8. Drain pipe; 9. Cooler; 10. Fourth pipeline; 11. Fifth pipeline; 12. Transfer pump; 13. Sixth pipeline; 14. Filter; 15. Seventh pipeline; 16. Preheater; 17. Heating coil; 18. Feed pipe; 19. Eighth pipeline; 31. Ninth pipeline; 32. Tenth pipeline; 33. Cooling tower; 34. Eleventh pipeline; 35. Make-up water pipe; 36. Twelfth pipeline; 37. Thirteenth pipeline. Detailed Implementation
[0015] To clearly illustrate the technical features of this solution, the following detailed implementation method will be used to explain the solution.
[0016] like Figures 1-2 As shown, a catalytic device for synthesizing o-phenylphenol intermediates includes a reboiler 1, a distillation column 2, a condenser 4, and a water separator 6. The reboiler 1 has a steam outlet at its top, a feed inlet and a return outlet on its sidewall, and a discharge outlet at its bottom. The distillation column 2 is fixedly connected to the top of the reboiler 1.
[0017] The distillation column 2 includes, from bottom to top, a stripping section 21, a heating section 22, and a rectification section 23, all fixedly connected. The top of the rectification section 23 has a steam outlet. The bottom of the stripping section 21 is fixedly connected to the steam outlet at the top of the reboiler 1. Both the stripping section 21 and the rectification section 23 are filled with corrugated packing. The corrugated packing in the stripping section 21 is BX500, and the corrugated packing in the rectification section 23 is AX250. The stripping section 21 and the rectification section 23 are conventional technologies used in existing distillation columns 2, and will not be described in detail here.
[0018] The heating section 22 is equipped with a steam-water separator 24, multiple heating plates 25, and a filter screen 26. The steam-water separator 24 is fixedly installed inside the heating section 22, the multiple heating plates 25 are fixedly connected to the bottom of the steam-water separator 24, and the multiple heating plates 25 are evenly distributed radially and extend vertically. The filter screen 26 is fixedly connected to the bottom of the multiple heating plates 25.
[0019] The steam-water separator 24 described in this embodiment is an MS9 type filled steam-water separator 24, which is commercially available. The heating plate 25 has a serpentine curved structure. The serpentine curved structure of the heating plate 25 increases the contact area, thereby increasing the heating temperature. Furthermore, the heating plate 25 is made of copper, which has strong heat absorption and conductivity, allowing it to absorb the heat from the rising high-temperature steam more quickly, thus heating the returning liquid cyclohexanone. The filter screen 26 has a conical shape. The conical shape of the filter screen 26 can retain more impurities, extending the cleaning interval and making it more convenient to use.
[0020] The condenser 4 is equipped with a steam inlet, a condensate outlet, a heat exchange inlet, and a heat exchange outlet. Cooling medium is introduced and discharged through the heat exchange inlet and heat exchange outlet. High-temperature steam enters the interior through the steam inlet, and after heat exchange with the cooling medium, condensate is formed and discharged from the condensate outlet.
[0021] The water separator 6 is equipped with an inlet, a return outlet, and a drain outlet. The return outlet is used to discharge the return liquid, the drain outlet is used to discharge the separated wastewater, and the drain outlet is connected to a drain pipe 8.
[0022] Specifically, the top outlet of the distillation column 2 is connected to the steam inlet of the condenser 4, the condensate outlet of the condenser 4 is connected to the inlet of the water separator 6, and the reflux outlet of the water separator 6 is connected to the top inlet of the steam-water separator 24.
[0023] In this embodiment, the top steam outlet of the rectification section 23 of the distillation column 2 is connected to the steam inlet of the condenser 4 via a first pipe 3. The condensate outlet of the condenser 4 is connected to the inlet of the water separator 6 via a second pipe 5. A balancing valve is installed on the second pipe 5 to balance the internal pressure and improve safety. The reflux outlet of the water separator 6 is connected to the top inlet of the steam-water separator 24 via a third pipe 7.
[0024] The reaction mixture undergoes a condensation reaction in reboiler 1. The high-temperature vapor formed by the azeotropic reaction of water and cyclohexanone rises sequentially through stripping section 21, heating section 22, and rectification section 23 before entering condenser 4. The high-temperature vapor is condensed into liquid by cooling and heat exchange in condenser 4 and sent to water separator 6. The liquid wastewater is separated by water separator 6 and discharged from the drain outlet. The liquid cyclohexanone flows back into heating section 22, where it is separated from the high-temperature vapor in steam-water separator 24. The liquid cyclohexanone flows downwards, is heated by heating plate 25, and is filtered by filter screen 26 before flowing back into reboiler 1 to participate in the reaction again.
[0025] This process utilizes a steam-water separator 24 to prevent liquid cyclohexanone from affecting the upward flow of steam, ensuring efficient distillation. Heating the low-temperature liquid cyclohexanone via a heating plate 25 reduces the impact of refluxed cyclohexanone on the reaction, thereby improving reaction efficiency and reducing energy consumption. Furthermore, the liquid cyclohexanone is filtered for impurities by a filter screen 26, ensuring reaction quality and slowing down the reflux rate of liquid cyclohexanone, further guaranteeing the reaction effect within the reboiler 1 and resulting in more stable product quality.
[0026] It also includes a cooler 9, a delivery pump 12, and a filter 14. The cooler 9 is provided with a liquid inlet, a liquid outlet, a heat exchange inlet, and a heat exchange outlet. The cooling medium is introduced and discharged through the heat exchange inlet and the heat exchange outlet. The catalyst liquid enters the interior through the liquid inlet, and after exchanging heat with the cooling medium, it is discharged from the liquid outlet.
[0027] The delivery pump 12 is a circulating pump, ensuring stable delivery. The filter 14 is a precision safety filter, providing higher filtration efficiency.
[0028] Specifically, the discharge port of the reboiler 1 is connected to the liquid inlet of the cooler 9, the liquid outlet of the cooler 9 is connected to the input end of the delivery pump 12, the output end of the delivery pump 12 is connected to the inlet of the filter 14, and the outlet of the filter 14 is connected to the return port of the reboiler 1.
[0029] In this embodiment, the discharge port of reboiler 1 is connected to the feed inlet of cooler 9 via the fourth pipe 10. The feed outlet of cooler 9 is connected to the input end of transfer pump 12 via the fifth pipe 11. The output end of transfer pump 12 is connected to the inlet of filter 14 via the sixth pipe 13. The outlet of filter 14 is connected to the return port of reboiler 1 via the seventh pipe 15.
[0030] The solid acid catalyst solution after reaction in reboiler 1 is discharged through the discharge port. After being cooled by heat exchange in cooler 9, it is then pumped by transfer pump 12 to filter 14 for filtration. The catalyst solution cooled by cooler 9 has a lower temperature, thus avoiding damage to the filter layer and extending the life of filter 14. The filtered catalyst solution is then recycled back into reboiler 1, saving resources.
[0031] It also includes a preheater 16 and a cooling tower 33. The preheater 16 is equipped with a heating coil 17 and has a discharge port and a feed port, with the feed port connected to a feed pipe 18. Both the input and output ports of the heating coil 17 extend to the outside of the preheater 16. Reactants are added to the preheater 16 through the feed port and discharged through the discharge port. Preheating the reactants in the preheater 16 by the heating coil 17 before introducing them into the reboiler 1 for azeotrope reduces the azeotropic time, thereby further reducing energy consumption and improving reaction efficiency.
[0032] The cooling tower 33 is provided with an input end, an output end, and a water supply end, with a water supply pipe 35 connected to the water supply end. The heat exchange medium is input through the input end, cooled, and then output through the output end. Cooling medium is replenished into the cooling tower 33 through the water supply end.
[0033] Specifically, the outlet of the preheater 16 is connected to the inlet of the reboiler 1. The heat exchange outlets of the cooler 9 and the condenser 4 are both connected to the input port of the heating coil 17. The output port of the heating coil 17 is connected to the input end of the cooling tower 33, and the heat exchange inlets of the cooler 9 and the condenser 4 are both connected to the output end of the cooling tower 33.
[0034] In this embodiment, the outlet of the preheater 16 is connected to the inlet of the reboiler 1 via the eighth pipeline 19.
[0035] The heat exchange outlet of the cooler 9 is connected to the ninth pipe 31, and the heat exchange outlet of the condenser 4 is connected to the tenth pipe 32. The ninth pipe 31 and the tenth pipe 32 are connected to the input port of the heating coil 17 through a tee fitting.
[0036] The output port of the heating coil 17 is connected to the input port of the cooling tower 33 through the eleventh pipe 34.
[0037] The heat exchange inlet of the cooler 9 is connected to the twelfth pipe 36, and the heat exchange inlet of the condenser 4 is connected to the thirteenth pipe 37. The twelfth pipe 36 and the thirteenth pipe 37 are connected to the output end of the cooling tower 33 through a tee fitting. A delivery pump 12 is also installed on the twelfth pipe 36 and the thirteenth pipe 37 to facilitate the pumping of the cooling medium.
[0038] Cooling medium is introduced into cooling tower 33 through water supply pipe 35, and then pumped into cooler 9 and condenser 4 by transfer pump 12 to exchange heat and cool the high-temperature catalyst liquid and high-temperature steam, respectively. After heat exchange, the cooling medium becomes a high-temperature medium, which is transported to heating coil 17 to preheat the reaction raw materials in preheater 16. Finally, the high-temperature medium flows back into cooling tower 33 for recooling, thus forming a complete circulating heat exchange system, saving a lot of resources and greatly reducing costs.
[0039] To facilitate the control of the flow rate in each pipeline, a flow regulating valve (not shown in the figure) is installed on each of the first pipeline 3 to the thirteenth pipeline 37 to facilitate the control of pipeline opening and closing and flow rate.
[0040] Of course, the above description is not limited to the examples above. Technical features of this utility model not described can be implemented by or using existing technology, and will not be repeated here. The above embodiments and drawings are only used to illustrate the technical solution of this utility model and are not intended to limit this utility model. This utility model has been described in detail with reference to preferred embodiments. Those skilled in the art should understand that any changes, modifications, additions or substitutions made by those skilled in the art within the scope of this utility model do not depart from the spirit of this utility model and should also fall within the protection scope of the claims of this utility model.
Claims
1. A catalytic device for synthesizing o-phenylphenol intermediates, comprising a reboiler (1), a distillation column (2), a condenser (4), and a water separator (6), wherein the distillation column (2) is fixed to the top of the reboiler (1), the top outlet of the distillation column (2) is connected to the steam inlet of the condenser (4), and the condensate outlet of the condenser (4) is connected to the inlet of the water separator (6), characterized in that: The distillation column (2) includes a stripping section (21), a heating section (22) and a rectification section (23) fixedly connected from bottom to top. The heating section (22) is equipped with a steam-water separator (24), multiple heating plates (25) and a filter screen (26). The steam-water separator (24) is fixedly installed in the heating section (22). The multiple heating plates (25) are fixedly connected to the bottom of the steam-water separator (24) and are evenly distributed radially and extended vertically. The filter screen (26) is fixedly connected to the bottom of the multiple heating plates (25). The reflux outlet of the water separator (6) is connected to the top inlet of the steam-water separator (24).
2. The intermediate catalytic apparatus for synthesizing o-phenylphenol according to claim 1, characterized in that: The heating plate (25) has a serpentine curved structure.
3. The intermediate catalytic apparatus for synthesis of o-phenylphenol according to claim 1, characterized by: The filter screen (26) has a cone-shaped structure.
4. The intermediate catalytic apparatus for synthesis of o-phenylphenol according to claim 1, characterized by: It also includes a cooler (9), a delivery pump (12) and a filter (14). The discharge port of the reboiler (1) is connected to the liquid inlet of the cooler (9), the liquid outlet of the cooler (9) is connected to the input end of the delivery pump (12), the output end of the delivery pump (12) is connected to the inlet of the filter (14), and the outlet of the filter (14) is connected to the return port of the reboiler (1).
5. The intermediate catalytic apparatus for synthesis of o-phenylphenol according to claim 4, characterized by: It also includes a preheater (16), the outlet of which is connected to the inlet of the reboiler (1).
6. The intermediate catalytic apparatus for synthesis of o-phenylphenol according to claim 5, characterized by: The preheater (16) is equipped with a heating coil (17), and the heat exchange outlet of the cooler (9) and the heat exchange outlet of the condenser (4) are connected to the input port of the heating coil (17).
7. The intermediate catalytic apparatus for synthesis of o-phenylphenol according to claim 6, characterized by: It also includes a cooling tower (33), the output port of the heating coil (17) is connected to the input end of the cooling tower (33), and the heat exchange inlet of the cooler (9) and the heat exchange inlet of the condenser (4) are both connected to the output end of the cooling tower (33).