Reactive rectification device and method for automatically separating phases and refluxing to reaction section
By designing a reaction distillation device that automatically separates and refluxes to the reaction section, the problems of complex processes and low raw material utilization in the prior art are solved, and efficient reaction conversion and energy consumption reduction are achieved.
Patent Information
- Application Number
- CN202510882568.9
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-06-27
- Publication Date
- 2025-08-01
AI Technical Summary
In the prior art, the reaction distillation device has problems such as complex process, inconvenient operation, low raw material utilization rate and insufficient reaction conversion rate during separation and reaction.
A reaction distillation device is designed to automatically divide and reflow into the reaction section, including a reaction distillation tower, heater, overhead condenser, automatic phase separator, aqueous phase collection tank and reflow ratio controller. The automatic phase separator realizes continuous separation and reflow of the aqueous phase and oil phase, and improves raw material utilization and reaction conversion rate.
It achieves simple process, convenient operation, high raw material utilization rate, high reaction conversion rate, and automatic phase separation and recovery of the aqueous phase and oil phase can be produced and refluxed to the reaction section, which improves the reaction conversion rate and reduces energy consumption.
Smart Images
Figure CN120393458A_ABST
Abstract
Description
Technical Field
[0001] The present invention relates to a reactive distillation apparatus and method for automatically separating phases and refluxing to a reaction section, belonging to the technical field of chemical reaction and separation coupling. Background Art
[0002] Reactive distillation is a process intensification technology that couples chemical reaction with distillation separation. By removing products or by-products (such as water) in situ, it can break the limitations of reaction chemical equilibrium, significantly improve reaction conversion and selectivity, reduce the ratio of raw materials, and at the same time 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 column that couples chemical reaction and distillation separation in the same equipment. Through the spontaneous phase separation of the overhead condensate, in-situ selective separation of products can be achieved. At the same time, by optimizing the reflux strategy, the reaction conversion can be improved, realizing the triple coordination of reaction, separation, and energy utilization. It is especially suitable for reaction systems where products and by-products (such as water) form heterogeneous azeotropes (such as esterification, etherification, etc.). Summary of the Invention
[0004] The technical problem to be solved by the present invention is to provide a reactive distillation apparatus and method with a simple process, convenient operation, in which unreacted raw materials are automatically phase-separated and refluxed to the reaction section to participate in the reaction again after rectification, with high raw material utilization rate, high reaction conversion rate, and the ability to automatically phase-separate and withdraw the aqueous phase and oil phase and reflux them to the reaction section.
[0005] The reactive distillation apparatus for automatically separating phases and refluxing to the reaction section according to the present invention includes a reactive distillation column (1), a heater (2), an overhead 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), and is characterized in that: the reactive distillation column (1) is successively a rectification section (11), a reaction section (12), and a stripping section (13) from top to bottom. The bottom of the reactive distillation column (1) is connected to a heater (2). The top of the reactive distillation column (1) is connected to the overhead condenser (3) and the automatic phase separator (4) in sequence through a pipeline. After the material is condensed by the overhead condenser (3), an immiscible aqueous phase and oil phase are formed. After automatic phase separation in the automatic phase separator (4), they are separated into an aqueous phase and an oil phase. The aqueous phase continuously flows out automatically from the upper part of the automatic phase separator (4) into the aqueous phase collection tank (5), and the oil phase continuously flows out automatically from the lower part of the automatic phase separator (4). The oil phase is divided into two parts, one part returns to the rectification section (1) through the reflux ratio controller (6), and one part automatically refluxes to the reaction section (12) by the liquid level to continue the reaction.
[0006] The reaction distillation column (1) described above is used at a temperature of -20°C to 300°C and a pressure of vacuum, atmospheric pressure or increased pressure.
[0007] There is one or two reaction raw materials in the reaction section (12), which are fed through 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 filled in the reaction section (12) is a homogeneous miscible catalyst or an insoluble solid catalyst. The solid catalyst is fixed in the form of a packing bag, granular filling, or bulk loading on a tray, etc.
[0009] A reaction distillation method with automatic phase separation and reflux to the reaction section, characterized by including the following steps: Step 1: One or two reaction raw materials are introduced into the reaction section (12) through feed pump A (7) or feed pump B (9). The raw materials undergo etherification, esterification or dehydration reactions in the reaction section (12) of the reaction distillation column (1). The reaction products include oil phases such as esters, ethers, ketones, aldehydes, and an aqueous phase. Step 2: The water, products with a boiling point lower than water, or unreacted raw materials generated by the reaction are taken out from the top of the column after passing through the rectifying section (11), condensed by the top condenser (3), and then separated into an aqueous phase and an oil phase in the automatic phase separator (4). Depending on the internal components of the automatic phase separator (4), the aqueous phase and the oil phase can flow out continuously and stably. The aqueous phase automatically flows into the aqueous phase collection tank (5) by the liquid level, and a part of the oil phase automatically flows back to the reaction section (12) by the liquid level, and a part flows back to the rectifying section (12) after being controlled by the reflux ratio controller (6). Step 3: The products with a boiling point higher than water or unreacted raw materials are taken out from the bottom of the column after passing through the stripping section (13).
[0010] The reaction distillation device and method with automatic phase separation and reflux to the reaction section provided by the present invention have the following advantages: 1. This device can distill the water generated by the dehydration reaction (esterification, etherification, condensation, etc.) from the top of the reaction distillation column (1), continuously and stably extract the water through the automatic phase separator (4), continuously remove low-boiling products (such as water in the esterification reaction) through rectification, and promote the reaction to proceed in the positive direction, thereby breaking the equilibrium conversion rate.
[0011] 2. The automatic phase separator (4) will continuously and stably flow out the unreacted raw material oil phase. The unreacted raw materials automatically flow back into the reaction section (12) by the liquid level to participate in the reaction again, thereby improving the raw material utilization rate and the conversion rate of the reaction, and making the conversion rate of the reaction exceed the equilibrium conversion rate.
[0012] 3. Reactive distillation integrates a reactor with a distillation column, achieving the synergistic effect of reaction-promoted separation and separation-promoted reaction, and is particularly suitable for reversible reactions (such as esterification, etherification, hydrolysis, etc.). At the same time, the heat released by the reaction can be directly used for distillation vaporization, reducing the energy consumption of the heater. The gas-liquid two-phase contacts efficiently on the catalyst surface, enhancing the reaction rate. Description of the Drawings
[0013] Figure 1 It is a schematic structural diagram of a reactive distillation device with automatic phase separation and reflux to the reaction section. Detailed Embodiments
[0014] To make the present invention more obvious and understandable, preferred embodiments are hereby described in detail in conjunction with the accompanying drawings as follows, but the present invention is not limited thereto.
[0015] Example 1: In this embodiment, as Figure 1 shown, a reactive distillation device with automatic phase separation and reflux to the reaction section is composed of a reactive distillation column (1), a heater (2), a 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 reactive distillation column (1) is successively divided into a rectification section (11), a reaction section (12), and a stripping section (13) from top to bottom. The bottom of the reactive distillation column (1) is connected to 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 by the top condenser (3), an immiscible aqueous phase and an oil phase are formed. After automatic phase separation in the automatic phase separator (4), they are separated into an aqueous phase and an oil phase. The aqueous phase continuously flows out automatically from the upper part of the automatic phase separator (4) into the aqueous phase collection tank (5), and the oil phase continuously flows out automatically from the lower part 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 one part automatically refluxes to the reaction section (12) depending on the liquid level to continue the reaction. There is one or two reaction raw materials. The feed pump A (7) is connected to the reaction section (12) through pipelines in sequence via the feed valve A (8). The feed pump B (9) is connected to the reaction section (12) through pipelines in sequence via the feed valve B (10). There is one or two reaction raw materials in the reaction section (12), and they are fed through the feed pump A (7) or the feed pump B (9). The feed pump A (7) is connected to the reaction section (12) through pipelines in sequence via the feed valve A (8). The feed pump B (9) is connected to the reaction section (12) through pipelines in sequence via the feed valve B (10). The catalyst filled in the reaction section (12) is a homogeneous soluble catalyst or an insoluble solid catalyst. The solid catalyst is fixed in the form of a packing bag, granular filling, or bulk loading on a tray, etc. The operating temperature of the reactive distillation column (1) is: -20°C to 300°C, and the operating pressure is: vacuum, atmospheric pressure, or pressurization.
[0016] In this embodiment, according to the structure of the reactive distillation apparatus with automatic phase separation and reflux to the reaction section described above, the reactive distillation method with automatic phase separation and reflux to the reaction section includes the following steps: Step 1: One or two reaction raw materials are introduced into the reaction section (12) through the feed pump A (7) or the feed pump B (9). The raw materials undergo etherification, esterification, or dehydration reactions in the reaction section (12) of the reactive distillation column (1). The reaction products include oil phases such as esters, ethers, ketones, aldehydes, etc. and an aqueous phase. Step 2: Water, products with boiling points lower than water, or unreacted raw materials produced by the reaction are taken out from the top of the column after passing through the rectifying section (11), condensed by the top condenser (3), and then separated into an aqueous phase and an oil phase in the automatic phase separator (4). Depending on the internal components of the automatic phase separator (4), the aqueous phase and the oil phase can flow out continuously and stably. The aqueous phase automatically flows into the aqueous phase collection tank (5) by the liquid level, part of the oil phase automatically refluxes to the reaction section (12) by the liquid level, and part of it flows back to the rectifying section (12) after being controlled by the reflux ratio controller (6). Step 3: Products with boiling points higher than water or unreacted raw materials are taken out from the bottom of the column after passing through the stripping section (13).
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 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 described reactive distillation column (1) from top to bottom is successively a rectifying section (11), a reaction section (12), and a stripping section (13). The bottom of the reactive distillation column (1) is connected to a heater (2). The top of the reactive distillation column (1) is successively connected to a top condenser (3) and an automatic phase separator (4) through pipelines. After the material is condensed by the top condenser (3), an immiscible water phase and oil phase are formed. After automatic phase separation in the automatic phase separator (4), it is separated into a water phase and an oil phase. The water phase automatically and continuously flows out from the upper part of the automatic phase separator (4) into the water phase collection tank (5), and the oil phase automatically and continuously flows out from the lower part of the automatic phase separator (4). The oil phase is divided into two parts. One part returns to the rectifying section (11) through a reflux ratio controller (6), and one part automatically returns to the reaction section (12) by liquid level to continue the reaction.
2. The reactive distillation apparatus according to claim 1, which automatically separates phases and refluxes to the reaction section, is characterized in that: The operating temperature of the described reactive distillation column (1) is: -20°C to 300°C, and the operating pressure is: vacuum or atmospheric pressure or pressurization.
3. The reactive distillation apparatus according to claim 1, which automatically separates phases and refluxes to the reaction section, is characterized in that: There is one or two reaction raw materials in the reaction section (12), and they are fed through a feed pump A (7) or a feed pump B (9). The feed pump A (7) is successively connected to a feed valve A (8) and the reaction section (12) through pipelines. The feed pump B (9) is successively connected to a feed valve B (10) and the reaction section (12) through pipelines.
4. The reactive distillation apparatus for automatically separating phases and refluxing to the reaction section according to claim 1, wherein: The catalyst filled in the reaction section (12) is a homogeneous miscible catalyst or an insoluble solid catalyst. The solid catalyst is fixed in forms such as packing bags, particle filling, or bulk loading on trays.
5. A reactive distillation method for automatically separating phases and refluxing to the reaction section, characterized in that, It includes the following steps: Step 1: One or two reaction raw materials are introduced into the reaction section (12) through a feed pump A (7) or a feed pump B (9). The raw materials undergo etherification, esterification, or dehydration reactions in the reaction section (12) of the reactive distillation column (1). The reaction products include an oil phase and a water phase such as esters, ethers, ketones, and aldehydes. Step 2: The water, products with boiling points lower than water, or unreacted raw materials generated by the reaction are taken out from the top of the column after passing through the rectifying section (11), condensed by the top condenser (3), and separated into a water phase and an oil phase in the automatic phase separator (4). Due to the internal components in the automatic phase separator (4), the water phase and the oil phase can flow out continuously and stably. The water phase automatically flows into the water phase collection tank (5) by liquid level, and one part of the oil phase automatically returns to the reaction section (12) by liquid level, and one part returns to the rectifying section (12) after being controlled by the reflux ratio controller (6). Step 3: The products with boiling points higher than water or unreacted raw materials are taken out from the bottom of the column after passing through the stripping section (13).