Three-phase multi-stage fluidized bed reactor coupled with rectification continuous esterification reaction rectification device

Abstract

The utility model discloses a three -phase multistage fluidized bed reactor and rectification coupling continuous esterification reaction rectification device belongs to chemical industry reaction and separation coupling technical field. The device is coupled by multistage fluidized bed reactor (1) and rectifying column (2), and the top of multistage fluidized bed reactor (1) is connected with the bottom of rectifying column (2), and multistage fluidized bed reactor (1) is as the kettle of rectifying column (2), provides the heating heat source for rectifying column (2), and after the separation of reaction product through rectifying column (2), the water produced in reaction is automatically extracted, and the unreacted raw material will rely on gravity and reflow into multistage fluidized bed reactor (1) again to participate in the reaction again, promotes the reaction to the positive direction, improves raw material utilization and reaction conversion rate. The utility model has the advantages of simple process, big operation flexibility, energy saving and consumption reduction, high raw material utilization, high reaction conversion rate and the like.

Description

Technical Field

[0001] This utility model relates to a three-phase multi-stage fluidized bed reactor coupled with distillation for continuous esterification reaction distillation, belonging to the field of chemical reaction and separation coupling technology. Background Technology

[0002] A fluidized bed reactor is a highly efficient multiphase reaction device that achieves efficient mass transfer, heat transfer, and chemical reactions by suspending solid particles (such as catalysts or reactants) in flowing gas or liquid to form a gas-solid, liquid-solid, or gas-solid-liquid "fluidization".

[0003] Distillation columns are one of the most critical pieces of equipment in chemical separation processes. They are used to achieve efficient separation of mixtures through mass and heat transfer between the vapor and liquid phases, and are widely used in petroleum refining, chemical production, pharmaceuticals, food processing, and environmental protection.

[0004] Combining fluidized bed reactors with distillation columns is an enhanced technology that couples chemical reactions with process separation. Distillation columns enable in-situ selective separation of products, while optimized reflux strategies can significantly improve reaction conversion rate, product selectivity, and energy utilization, achieving a triple synergy of reaction, separation, and energy utilization, thus achieving the goal of energy conservation and emission reduction. Summary of the Invention

[0005] The technical problem to be solved by this utility model is to provide a three-phase multi-stage fluidized bed reactor coupled with distillation for continuous esterification reaction distillation, which has a simple process, high operational flexibility, energy saving and consumption reduction, high raw material utilization rate and high reaction conversion rate.

[0006] The three-phase multi-stage fluidized bed reactor coupled with distillation continuous esterification reaction distillation device of this utility model includes a multi-stage fluidized bed reactor (1), a distillation column (2), reaction section 1 (3), reaction section 2 (4), reaction section 3 (5), a heater for reaction section 1 (6), a heater for reaction section 2 (7), a heater for reaction section 3 (8), a column top condenser (9), an automatic phase separator (10), an aqueous phase collection tank (11), a reflux ratio controller (12), a material reflux valve (13), a nitrogen inlet valve (14), and a raw material feed pump. (15) Raw material feed valve (16) and product outlet valve (17), characterized in that: the esterification reaction distillation device coupled with the three-phase multi-stage fluidized bed reactor and distillation consists of a multi-stage fluidized bed reactor (1) and a distillation column (2), the top of the multi-stage fluidized bed reactor (1) is connected to the bottom of the distillation column (2), the multi-stage fluidized bed reactor (1) is divided into reaction section 1 (3), reaction section 2 (4) and reaction section 3 (5) from bottom to top, the reaction section 1 (3) is provided with a reaction section 1 heater (6) outside the reaction section 1 (3), the reaction section 1 heater (6) is provided outside the reaction section 1 (3), the reaction section 1 heater (6) is provided outside the reaction section 1 (3) The external part of the reaction section 2 (4) is equipped with a heater (7) for the reaction section 2, and the external part of the reaction section 3 (5) is equipped with a heater (8) for the reaction section 3. The top of the distillation column (2) is connected to the top condenser (9) and the automatic phase separator (10) in sequence through pipelines. After the material is condensed by the top condenser (9), it is divided into two streams. One stream flows back to the distillation column (2) through the reflux ratio controller (12) to maintain the normal operation of the distillation column (2). The other stream flows to the automatic phase separator (10), where a water phase and an oil phase are formed. The phase is automatically and continuously extracted and flows into the aqueous phase collection tank (11). The oil phase is automatically and continuously extracted and flows back to the reaction section 1 (3) of the multi-stage fluidized bed reactor (1) through the material return valve (13) to continue participating in the reaction. N2 enters from the bottom of the reaction section 1 (3) through the nitrogen inlet valve (14). The reaction raw materials are fed through the raw material feed pump (15). The outlet of the raw material feed pump (15) is connected to the raw material feed valve (16) and the reaction section 1 (3) in sequence through pipelines. The high-boiling point product is extracted from the reaction section 3 (5) through the product extraction valve (17).

[0007] The multi-stage fluidized bed reactor (1) is formed by gas-liquid-solid three-phase fluidization of solid, liquid and N2 to carry out esterification reaction. The solid includes: catalyst or raw material solid acid, the liquid includes: raw material liquid acid or raw material liquid fatty alcohol with more than 4 carbons, the boiling point of the raw material alcohol and raw material acid is higher than that of water, the catalyst is a solid particulate catalyst or a catalyst miscible with liquid raw material, and N2 is used as a fluidization gas.

[0008] Based on the density of the solid material and the catalyst particles, reaction sections 1 (3), 2 (4) and 3 (5) with different diameters are designed. The materials with different particle sizes have different fluidization velocities in each section and participate in the reaction in different reaction sections.

[0009] The three-phase multi-stage fluidized bed reactor coupled with distillation for continuous esterification reaction distillation unit operates at temperatures ranging from 50℃ to 300℃ and pressures ranging from vacuum to atmospheric pressure or pressurized pressure.

[0010] The beneficial effects of this utility model are:

[0011] 1. This device can automatically extract the water produced by the esterification reaction through an automatic phase separator (10), pushing the reaction in the positive direction and thus breaking the equilibrium conversion rate.

[0012] 2. This device can condense the unreacted raw materials during the esterification process through the top of the distillation column (2), automatically separate the phases, and then automatically reflux them back into the reaction section (1) by gravity to continue the reaction, thereby improving the utilization rate of raw materials and the conversion rate of the reaction, so that the conversion rate of the reaction exceeds the equilibrium conversion rate.

[0013] 3. The diameters of reaction sections 1 (3), 2 (4) and 3 (5) are different. Based on the density of the solid material and the design of the catalyst particles, the different particles of the material have different fluidization velocities in each section. At the same time, each reaction section is equipped with an independent heater. The temperature of the heater is set according to the different reactions in each section, and the device has great operational flexibility.

[0014] 4. This device integrates a multi-stage fluidized bed reactor (1) and a distillation column (2). The multi-stage fluidized bed reactor (1) serves as the bottom of the distillation column (2), providing a heat source for the column. The unreacted raw materials separated by the distillation column (2) are then returned to the reaction section 1 (3) of the multi-stage fluidized bed reactor (1) by gravity to participate in the reaction again. This achieves a synergistic effect of reaction driving separation and separation promoting reaction, further improving the reaction rate. At the same time, it reduces reaction energy consumption and saves equipment space and construction investment. Attached Figure Description

[0015] Figure 1 This is a schematic diagram of a continuous esterification reaction distillation unit coupled with a three-phase multi-stage fluidized bed reactor and distillation. Detailed Implementation

[0016] The present invention will now be described in further detail with reference to the accompanying drawings:

[0017] like Figure 1The three-phase multi-stage fluidized bed reactor coupled with distillation continuous esterification reaction distillation device shown consists of a multi-stage fluidized bed reactor (1), a distillation column (2), reaction section 1 (3), reaction section 2 (4), reaction section 3 (5), reaction section 1 heater (6), reaction section 2 heater (7), reaction section 3 heater (8), column top condenser (9), automatic phase separator (10), aqueous phase collection tank (11), reflux ratio controller (12), material reflux valve (13), nitrogen inlet valve (14), raw material feed pump (15), raw material feed valve (16), and product outlet valve (17). The three-phase multi-stage fluidized bed reactor coupled with distillation esterification reaction distillation device consists of a multi-stage fluidized bed reactor. (1) and distillation column (2) are composed of a multi-stage fluidized bed reactor (1) and a distillation column (2). The top of the multi-stage fluidized bed reactor (1) is connected to the bottom of the distillation column (2). The multi-stage fluidized bed reactor (1) consists of reaction section 1 (3), reaction section 2 (4) and reaction section 3 (5) from bottom to top. The reaction sections 1 (3), 2 (4) and 3 (5) with different diameters are designed according to the density of the solid material and the catalyst particles. The material with different particles has different fluidization velocities in each section and participates in the reaction in different reaction sections. The reaction section 1 (3) is equipped with a reaction section 1 heater (6), the reaction section 2 (4) is equipped with a reaction section 2 heater (7), and the reaction section 3 (5) is equipped with a reaction section 3 heater (8). The distillation column ( 2) The top of the material is connected to the top condenser (9) and the automatic phase separator (10) in sequence through pipelines. After the material is condensed by the top condenser (9), it is divided into two streams. One stream flows back to the distillation column (2) through the reflux ratio controller (12) to maintain the normal operation of the distillation column (2). The other stream flows to the automatic phase separator (10), where an aqueous phase and an oil phase are formed. The aqueous phase is automatically and continuously collected and flows into the aqueous phase collection tank (11). The oil phase is automatically and continuously collected and flows back to the reaction section 1 (3) of the multi-stage fluidized bed reactor (1) through the material reflux valve (13) to continue participating in the reaction. N2 enters from the bottom of the reaction section 1 (3) through the nitrogen inlet valve (14). The reaction raw materials are fed through the raw material feed pump ( 15) Feeding: The outlet of the raw material feed pump (15) is connected to the raw material feed valve (16) and the reaction section 1 (3) in sequence through pipelines. The high-boiling point product is collected from the reaction section 3 (5) through the product collection valve (17). The multi-stage fluidized bed reactor (1) is formed by gas-liquid-solid three-phase fluidization of solid, liquid and N2 to carry out esterification reaction. The solid includes: catalyst or raw material solid acid. The liquid includes: raw material liquid acid or raw material liquid fatty alcohol with more than 4 carbons. The boiling point of the raw material alcohol and raw material acid is higher than that of water. The catalyst is a solid particulate catalyst or a catalyst that is miscible with the liquid raw material. N2 is used as a fluidizing gas. The operating temperature of the device is 50℃~300℃. The operating pressure is vacuum or atmospheric pressure or pressurized.

[0018] 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 continuous esterification reaction distillation device coupled with a three-phase multi-stage fluidized bed reactor and a rectifying column, comprising a multi-stage fluidized bed reactor (1), a rectifying column (2), a reaction stage 1 (3), a reaction stage 2 (4), a reaction stage 3 (5), a reaction stage 1 heater (6), a reaction stage 2 heater (7), a reaction stage 3 heater (8), a top condenser (9), an automatic phase separator (10), a water phase collection tank (11), a reflux ratio controller (12), a material reflux valve (13), a nitrogen gas inlet valve (14), a raw material feeding pump (15), a raw material feeding valve (16), and a product extraction valve (17), characterized in that: The esterification reaction distillation device coupled with a three-phase multi-stage fluidized bed reactor consists of a multi-stage fluidized bed reactor (1) and a distillation column (2). The top of the multi-stage fluidized bed reactor (1) is connected to the bottom of the distillation column (2). The multi-stage fluidized bed reactor (1) consists of reaction section 1 (3), reaction section 2 (4), and reaction section 3 (5) from bottom to top. The reaction section 1 (3) is equipped with a reaction section 1 heater (6), the reaction section 2 (4) is equipped with a reaction section 2 heater (7), and the reaction section 3 (5) is equipped with a reaction section 3 heater (8). The top of the distillation column (2) is connected to the top condenser (9) and the automatic phase separator (10) in sequence through pipelines. After the material is condensed by the top condenser (9), it is divided into two phases. One stream flows back to the distillation column (2) through the reflux ratio controller (12) to maintain the normal operation of the distillation column (2), and the other stream flows to the automatic phase separator (10) to form an aqueous phase and an oil phase. The aqueous phase is automatically and continuously collected and flows to the aqueous phase collection tank (11). The oil phase is automatically and continuously collected and flows back to the reaction section 1 (3) of the multi-stage fluidized bed reactor (1) through the material reflux valve (13) to continue to participate in the reaction. N2 enters from the bottom of the reaction section 1 (3) through the nitrogen inlet valve (14). The reaction raw materials are fed through the raw material feed pump (15). The outlet of the raw material feed pump (15) is connected to the raw material feed valve (16) and the reaction section 1 (3) in sequence through pipelines. The high-boiling point product is collected from the reaction section 3 (5) through the product collection valve (17).

2. The three-phase multi-stage fluidized bed reactor coupled with distillation continuous esterification reaction distillation apparatus according to claim 1, characterized in that: Based on the density of the solid material and the catalyst particles, reaction sections 1 (3), 2 (4) and 3 (5) with different diameters are designed. The materials with different particle sizes have different fluidization velocities in each section and participate in the reaction in different reaction sections.

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