An automatic phase separation pump backflow to a reaction rectifying device
By introducing an automatic phase-separating pump reflux mechanism into the reactive distillation unit, the problems of complex processes and low conversion rates in existing units have been solved, achieving efficient utilization of raw materials and improved reaction conversion rates. It is suitable for reactions such as esterification and etherification, and reduces energy consumption.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- TIANJIN GOLDEN EAGLE TECH
- Filing Date
- 2025-06-30
- Publication Date
- 2026-05-29
AI Technical Summary
Existing reactive distillation units suffer from problems such as complex processes, inconvenient operation, low utilization of unreacted raw materials, and insufficient reaction conversion during the reaction and separation process.
A reactive distillation apparatus is designed with an automatic phase-splitting pump to return the feed to the reaction section. The aqueous and oil phases are separated by an automatic phase separator, and the oil phase is returned to the reaction section. Unreacted feed is forced back to the reaction section by a reflux pump. The molar ratio of feed to reflux material is optimized by a reflux ratio controller to achieve efficient utilization of feed and improve reaction conversion rate.
It achieves a simple process and convenient operation, improves raw material utilization and reaction conversion rate, reduces energy consumption, and is suitable for reversible reactions such as esterification and etherification. It is especially suitable for reaction systems in which products and by-products form heterogeneous azeotropes.
Smart Images

Figure CN224292554U_ABST
Abstract
Description
Technical Field
[0001] This utility model relates to a reactive distillation device with an automatic phase-separating pump that returns the water to the reaction section, belonging to the field of chemical reaction and separation coupling technology. Background Technology
[0002] Reactive distillation is a process enhancement technology that couples chemical reactions with distillation separation. By removing products or byproducts (such as water) in situ, it breaks the chemical equilibrium limitations of the reaction, which can significantly improve reaction conversion and selectivity, reduce the proportion of raw materials, and reduce energy consumption and equipment investment. It is widely used in reversible reaction processes such as esterification, etherification, hydrolysis, and alkylation.
[0003] A reactive distillation column is a special type of column that couples chemical reactions and distillation separation within the same device. The spontaneous phase separation of the condensate at the top of the column enables in-situ selective separation of products. At the same time, by optimizing the reflux strategy, the reaction conversion rate can be improved, achieving a triple synergy of reaction, separation and energy utilization. It is especially suitable for reaction systems in which products and byproducts (such as water) form heterogeneous azeotropes (such as esterification and etherification). Summary of the Invention
[0004] The technical problem to be solved by this utility model is to provide a reaction distillation device with a simple process, convenient operation, automatic phase separation pump to return unreacted raw materials to the reaction section for re-reaction after distillation, high raw material utilization rate, high reaction conversion rate, and automatic phase separation of aqueous and oil phases for collection and return to the distillation and reaction sections.
[0005] The present invention discloses an automatic phase-splitting pump refluxing to the reaction section of a reactive distillation apparatus, comprising a reactive distillation column (1), a heater (2), a column top condenser (3), an automatic phase separator (4), an aqueous phase collection tank (5), an oil phase collection tank (6), a reflux ratio controller (7), a reflux pump (8), a feed pump A (9), a feed valve A (10), a feed pump B (11), and a feed valve B (12). The reactive distillation column (1) consists of a rectification section (13), a reaction section (14), and a stripping section (15) from top to bottom. A heater (2) is connected to the bottom of the reactive distillation column (1), and the top of the reactive distillation column (1) is connected to the column via pipelines. The top condenser (3) and the automatic phase separator (4) are connected. After the material is condensed by the top condenser (3), it forms an incompletely miscible water phase and an oil phase. After automatic phase separation in the automatic phase separator (4), it is divided into a water phase and an oil phase. The water phase flows out automatically and continuously from the top of the automatic phase separator (4) into the water phase collection tank (5), and the oil phase flows out automatically and continuously from the bottom of the automatic phase separator (4). The oil phase is divided into two parts. One part is returned to the rectification section (13) through the reflux ratio controller (7), and the other part flows out automatically and continuously into the oil phase collection tank (6). The oil phase collected in the oil phase collection tank (6) is forcibly transported back to the reaction section (14) by the reflux pump (8) to continue to participate in the reaction.
[0006] The operating temperature of the reactive distillation column (1) is -20℃ to 300℃, and the operating pressure is vacuum, atmospheric pressure, or pressurized pressure.
[0007] The reaction section (14) contains one or two kinds of reaction raw materials, which are fed by feed pump A (9) or feed pump B (11). Feed pump A (9) is connected to feed valve A (10) and reaction section (14) in sequence through pipelines, and feed pump B (11) is connected to feed valve B (12) and reaction section (14) in sequence through pipelines.
[0008] The catalyst packed in the reaction section (14) is either a homolytic catalyst or an insoluble solid catalyst. The solid catalyst is fixed by packing bags, granules, or bulk loading on trays.
[0009] The beneficial effects of this utility model are:
[0010] 1. This device can distill the water produced by dehydration reactions (esterification, etherification, condensation, etc.) from the top of the reactive distillation column (1), and continuously and stably extract the water through the automatic phase separator (4). The low-boiling-point products (such as water in the esterification reaction) are continuously removed through distillation, which promotes the reaction in the positive direction and thus breaks the equilibrium conversion rate.
[0011] 2. The automatic phase separator (4) will continuously and stably discharge the unreacted raw material oil phase. The unreacted raw material is forcibly transported back to the reaction section (14) by the reflux pump (8) to participate in the reaction again, thereby improving the raw material utilization rate and the reaction conversion rate, so that the reaction conversion rate exceeds the equilibrium conversion rate. At the same time, the flow rate of the reflux pump (8) can be set arbitrarily, and the molar ratio of raw material and reflux material can be arbitrarily adjusted under the premise of ensuring consistent liquid space velocity, so as to obtain optimized process conditions.
[0012] 3. Reactive distillation integrates the reactor with the distillation column, achieving a synergistic effect of reaction-driven separation and separation-promoted reaction, which is particularly suitable for reversible reactions (such as esterification, etherification, and hydrolysis). Simultaneously, the exothermic reaction can be directly used for distillation vaporization, reducing heater energy consumption, and the efficient contact between the gas and liquid phases on the catalyst surface enhances the reaction rate. Attached Figure Description
[0013] Figure 1 This is a schematic diagram of a reactive distillation apparatus with an automatic phase-separating pump that returns water to the reaction section. Detailed Implementation
[0014] The present invention will now be described in further detail with reference to the accompanying drawings:
[0015] like Figure 1The reactive distillation apparatus shown comprises an automatic phase-splitting pump refluxing to the reaction section, including a reactive distillation column (1), a heater (2), a column top condenser (3), an automatic phase separator (4), an aqueous phase collection tank (5), an oil phase collection tank (6), a reflux ratio controller (7), a reflux pump (8), a feed pump A (9), a feed valve A (10), a feed pump B (11), and a feed valve B (12). The reactive distillation column (1) consists of a rectification section (13), a reaction section (14), a reflux section (15), and a reaction section (16). The distillation section (14) and the stripping section (15) are connected to a heater (2) at the bottom of the reactive distillation column (1). The top of the reactive distillation column (1) is connected to the top condenser (3) and the automatic phase separator (4) in sequence through pipelines. After the material is condensed by the top condenser (3), it forms an incompletely miscible water phase and an oil phase. After automatic phase separation in the automatic phase separator (4), it is divided into a water phase and an oil phase. The water phase flows out automatically and continuously from the top of the automatic phase separator (4) into the water phase collection tank (5). The oil phase flows out continuously from the top of the automatic phase separator (4) into the water phase collection tank (5). The phase flows out automatically and continuously from the bottom of the automatic phase separator (4). The oil phase is divided into two parts. One part is returned to the rectification section (13) through the reflux ratio controller (7), and the other part flows out automatically and continuously into the oil phase collection tank (6). The oil phase collected in the oil phase collection tank (6) is forcibly transported back to the reaction section (14) by the reflux pump (8) to continue participating in the reaction. The reaction section (14) has one or two kinds of raw materials, which are fed by the feed pump A (9) or the feed pump B (11). The feed pump A (9) The feed pump B (11) is connected to the feed valve B (12) and the reaction section (14) in sequence through pipelines. The catalyst packed in the reaction section (14) is a homolytic catalyst or an insoluble solid catalyst. The solid catalyst is fixed by packing bags or granules or in bulk on the tray. The operating temperature of the reactive distillation column (1) is -20℃~300℃, and the operating pressure is vacuum or atmospheric pressure or pressurized.
[0016] The description and application of this utility model herein are illustrative and are not intended to limit the scope of this utility model to the above embodiments. Therefore, this utility model is not limited to the embodiments described herein, and any technical solution obtained by equivalent substitution is within the protection scope of this utility model.
Claims
1. A reactive distillation apparatus with an automatic phase-splitting pump refluxing to the reaction section, comprising a reactive distillation column (1), a heater (2), a column top condenser (3), an automatic phase separator (4), an aqueous phase collection tank (5), an oil phase collection tank (6), a reflux ratio controller (7), a reflux pump (8), a feed pump A (9), a feed valve A (10), a feed pump B (11), and a feed valve B (12), characterized in that: The reactive distillation column (1) consists of a rectification section (13), a reaction section (14), and a stripping section (15) from top to bottom. A heater (2) is connected to the bottom of the reactive distillation column (1). The top of the reactive distillation column (1) is connected to the top condenser (3) and the automatic phase separator (4) via pipelines. After the material is condensed by the top condenser (3), it forms an incompletely miscible water phase and an oil phase. After automatic phase separation in the automatic phase separator (4), it is divided into a water phase and an oil phase. The water phase flows out automatically and continuously from the top of the automatic phase separator (4) into the water phase collection tank (5). The oil phase flows out automatically and continuously from the bottom of the automatic phase separator (4). The oil phase is divided into two parts. One part is returned to the rectification section (13) through the reflux ratio controller (7), and the other part flows out automatically and continuously into the oil phase collection tank (6). The oil phase collected in the oil phase collection tank (6) is forcibly transported back to the reaction section (14) by the reflux pump (8) to continue participating in the reaction.
2. The reactive distillation apparatus with an automatic phase-separating pump refluxing to the reaction section according to claim 1, characterized in that: The operating temperature of the reactive distillation column (1) is -20℃ to 300℃, and the operating pressure is vacuum, atmospheric pressure, or pressurized pressure.
3. The reactive distillation apparatus with an automatic phase-separating pump refluxing to the reaction section according to claim 1, characterized in that: The reaction section (14) contains one or two kinds of reaction raw materials, which are fed by feed pump A (9) or feed pump B (11). Feed pump A (9) is connected to feed valve A (10) and reaction section (14) in sequence through pipelines, and feed pump B (11) is connected to feed valve B (12) and reaction section (14) in sequence through pipelines.
4. The reactive distillation apparatus with an automatic phase-separating pump refluxing to the reaction section according to claim 1, characterized in that: The catalyst packed in the reaction section (14) is either a homolytic catalyst or an insoluble solid catalyst. The solid catalyst is fixed by packing bags, granules, or bulk loading on trays.