An automatic phase separation refluxing reaction rectifying device
By introducing an automatic phase separator and reflux control into the reactive distillation unit, automatic reflux and efficient phase separation of unreacted raw materials are achieved, solving the problems of low raw material utilization and insufficient conversion rate, and improving reaction efficiency and energy utilization efficiency. It is particularly suitable for reactions such as esterification and etherification.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- TIANJIN GOLDEN EAGLE TECH
- Filing Date
- 2025-06-27
- Publication Date
- 2026-06-23
Smart Images
Figure CN224388088U_ABST
Abstract
Description
Technical Field
[0001] This utility model relates to an automatic phase-separation reflux reactive distillation device, 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 and reflux of unreacted raw materials after distillation to the reaction section to participate in the reaction again, high raw material utilization rate, high reaction conversion rate, and automatic phase separation and reflux of aqueous and oil phases to the distillation section and the reaction section.
[0005] The present invention discloses an automatic phase separation and reflux reaction distillation device, comprising a reaction distillation column (1), a heater (2), a column top condenser (3), an automatic phase separator (4), an aqueous phase collection tank (5), a reflux ratio controller (6), a feed pump A (7), a feed valve A (8), a feed pump B (9), and a feed valve B (10). The device is characterized in that the reaction distillation column (1) consists of a rectification section (11), a reaction section (12), and a stripping section (13) from top to bottom. A heater (2) is connected to the bottom of the reaction distillation column (1). The top of the column 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), 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 (11) through the reflux ratio controller (6), and the other part is automatically refluxed back to the reaction section (12) by the liquid level to continue 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 (12) contains one or two kinds of raw materials, which are fed by feed pump A (7) or feed pump B (9). Feed pump A (7) is connected to feed valve A (8) and reaction section (12) in sequence through pipelines, and feed pump B (9) is connected to feed valve B (10) and reaction section (12) in sequence through pipelines.
[0008] The catalyst packed in the reaction section (12) 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 will automatically flow back to the reaction section (12) to participate in the reaction again by the liquid level, thereby improving the raw material utilization rate and the reaction conversion rate, so that the reaction conversion rate exceeds the equilibrium conversion rate.
[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 that automatically separates phases and refluxes them 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 reaction distillation apparatus shown is an automatic phase separation and reflux device for the reaction section, consisting of a reaction distillation column (1), a heater (2), a column top condenser (3), an automatic phase separator (4), an aqueous phase collection tank (5), a reflux ratio controller (6), a feed pump A (7), a feed valve A (8), a feed pump B (9), and a feed valve B (10). The reaction distillation column (1) consists of a rectification section (11), a reaction section (12), and a stripping section (13) from top to bottom. The bottom of the reaction distillation column (1) is connected to... There is a heater (2). 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 in 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 and the other part. A portion of the feedstock is returned to the rectification section (11) via the reflux ratio controller (6), while another portion is automatically returned to the reaction section (12) by the liquid level to continue the reaction. The reaction involves one or two feedstocks. Feed pump A (7) is connected to feed valve A (8) and reaction section (12) via pipelines, and feed pump B (9) is connected to feed valve B (10) and reaction section (12) via pipelines. The reaction section (12) contains one or two feedstocks, which are fed by feed pump A (7) or feed pump B (9). Feed pump A (7) is connected to feed valve A (8) and reaction section (12) in sequence through pipelines. Feed pump B (9) is connected to feed valve B (10) and reaction section (12) in sequence through pipelines. The catalyst packed in reaction section (12) is a homolytic catalyst or an insoluble solid catalyst. The solid catalyst is fixed by packing bags, granules, or bulk on trays. The operating temperature of the reactive distillation column (1) is -20℃ to 300℃, and the operating pressure is vacuum, atmospheric pressure, or pressurized pressure.
[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 automatic phase separation and reflux 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), a reflux ratio controller (6), a feed pump A (7), a feed valve A (8), a feed pump B (9), and a feed valve B (10), characterized in that: The reactive distillation column (1) consists of a rectification section (11), a reaction section (12), and a stripping section (13) 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) 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 automatically and continuously from the bottom of the automatic phase separator (4). The oil phase is divided into two parts. One part returns to the rectification section (11) through the reflux ratio controller (6), and the other part automatically flows back to the reaction section (12) to continue the reaction based on the liquid level.
2. The reactive distillation apparatus for automatic phase separation and reflux 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 for automatic phase separation and reflux to the reaction section according to claim 1, characterized in that: The reaction section (12) contains one or two kinds of raw materials, which are fed by feed pump A (7) or feed pump B (9). Feed pump A (7) is connected to feed valve A (8) and reaction section (12) in sequence through pipelines, and feed pump B (9) is connected to feed valve B (10) and reaction section (12) in sequence through pipelines.
4. The reactive distillation apparatus for automatic phase separation and reflux to the reaction section according to claim 1, characterized in that: The catalyst packed in the reaction section (12) is either a homolytic catalyst or an insoluble solid catalyst. The solid catalyst is fixed by packing bags, granules, or bulk loading on trays.