CN215026071U - Reaction rectifying tower with built-in reflux device - Google Patents

Reaction rectifying tower with built-in reflux device Download PDF

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Publication number
CN215026071U
CN215026071U CN202120914544.4U CN202120914544U CN215026071U CN 215026071 U CN215026071 U CN 215026071U CN 202120914544 U CN202120914544 U CN 202120914544U CN 215026071 U CN215026071 U CN 215026071U
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built
tower body
tower
condenser
gas
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CN202120914544.4U
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陈坤
魏天荣
薛耘芸
於国伟
孙苏红
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Hubei Sanning Carbon Phosphorus Based New Material Industry Technology Research Institute Co ltd
Hubei Sanning Chemical Co Ltd
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Hubei Sanning Carbon Phosphorus Based New Material Industry Technology Research Institute Co ltd
Hubei Sanning Chemical Co Ltd
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  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

The utility model discloses a reaction rectifying tower with a built-in reflux device, which comprises a tower body, wherein a built-in condenser is arranged at the upper part in the tower body, a gas baffle is arranged above the built-in condenser, and a gas-liquid distributor is arranged below the built-in condenser; the tower body below the gas-liquid distributor is sequentially provided with a phenol feed port and a dimethyl carbonate feed port from top to bottom, and the bottom of the tower body is provided with a product outlet; a reboiler is arranged outside the tower body, and the reboiler and the bottom of the tower body form a circulation loop. Adopt the utility model discloses, can make the mixed gas that the boiling point is little constantly flow back in the tower, improve separation efficiency, save the energy consumption, and the temperature is controlled more easily.

Description

Reaction rectifying tower with built-in reflux device
Technical Field
The utility model belongs to the fine chemical industry field relates to chemical industry equipment, specifically is a reaction rectifying column of built-in reflux unit.
Background
In the reactive distillation column, the transesterification of dimethyl carbonate and phenol and the separation of dimethyl carbonate from the resultant methanol are carried out simultaneously. In the kettle connected with the bottom of the tower, dimethyl carbonate and phenol react under high temperature and catalyst to produce low-boiling-point methanol, high-boiling-point methyl phenyl carbonate and diphenyl carbonate. By utilizing the property that the vapor pressures of the components in the mixture are different, the low-boiling-point substance methanol in the liquid phase is transferred to the gas phase, and the high-boiling-point substance dimethyl carbonate in the gas phase is transferred to the liquid phase, thereby realizing the purpose of separation. The condenser and the reboiler of the conventional reaction rectifying tower are arranged outside the tower, the contact time of reaction materials is short, the reaction cycle time is long, the separation effect of reactants and products for inhibiting the reaction from moving to the right is poor, and the efficiency is relatively low.
The ester exchange reaction of phenol and dimethyl carbonate is an endothermic reaction, the equilibrium is moved to the positive reaction direction by the high temperature, but the boiling point of dimethyl carbonate is lower, the dimethyl carbonate is vaporized by the high temperature, and is separated from the reaction system, and the dimethyl carbonate is difficult to contact with another reactant phenol. This reduces the conversion of the equilibrium reaction and reduces the efficiency.
Disclosure of Invention
The utility model provides a built-in reflux unit's reaction rectifying column, under high temperature environment, can be furthest avoid the dimethyl carbonate vaporization to break away from the reaction system.
The technical scheme of the utility model is that the reaction rectifying tower with the built-in reflux device comprises a tower body, wherein a built-in condenser is arranged at the upper part in the tower body, a gas baffle plate is arranged above the built-in condenser, and a gas-liquid distributor is arranged below the built-in condenser; the tower body below the gas-liquid distributor is sequentially provided with a phenol feed port and a dimethyl carbonate feed port from top to bottom, and the bottom of the tower body is provided with a product outlet; a reboiler is arranged outside the tower body, and the reboiler and the bottom of the tower body form a circulation loop.
Further, an external condenser is connected to the outer side of the top of the tower body.
Furthermore, the built-in condenser is a U-shaped pipe, is uniformly distributed in the upper space of the tower body, and is provided with a water inlet and a water outlet which extend out of the tower.
Furthermore, the gas baffle is uniformly distributed with gas holes.
Furthermore, a thermometer is arranged at the bottom of the tower body above and below the built-in condenser, and a temperature sensor is arranged on a pipeline of the built-in condensation water inlet.
Furthermore, the tower body is a packed tower or a plate tower, and the inner wall of the tower body and the outer wall of the built-in condenser are both provided with an anticorrosive coating.
One of the products of the reaction of phenol and dimethyl carbonate is methanol, which is dissolved in the reaction system, and the existence of methanol can make the reaction difficult to move in the positive reaction direction. Therefore, methanol is removed in time during the reaction. Methanol and dimethyl carbonate can form an azeotrope, and the dimethyl carbonate can be separated from a reaction system along with the removal of the methanol, so that the reaction is not facilitated. The invention can make the dimethyl carbonate stay in the reaction system as much as possible by making the mixed gas continuously reflux in the tower and simultaneously extracting the low-boiling point gas methanol. Methanol and dimethyl carbonate can be better separated by arranging the belt pressure reflux in the rectifying tower, the methanol is separated from a reaction system by rectification, and the dimethyl carbonate refluxes into the reaction system. In a general rectifying tower, a condenser is arranged at the top end outside the tower to condense liquid, and then a pump is used for pumping the liquid back to the rectifying tower to realize reflux, but in this way, the contact time of a low-boiling point reactant dimethyl carbonate and a reaction system can be reduced, and the separation effect of methanol in the rectifying tower is not good, so that the equilibrium reaction is not completely carried out, and the reaction yield is reduced. The invention arranges the condensation pipe of the reflux device in the rectifying tower, so that the tower is continuously lifted, and the dimethyl carbonate gas to be separated from the reaction system is continuously and repeatedly refluxed into the reaction zone in time, thereby increasing the reaction time of the dimethyl carbonate, the phenol and the catalyst, better separating the methanol and the dimethyl carbonate, being more beneficial to the reaction, saving the energy consumption and improving the conversion rate. Moreover, the temperature of each section in the tower is easier to control.
The built-in condenser of the utility model is used for cooling the ascending mixture of dimethyl carbonate and methanol, part of the mixture with high dimethyl carbonate content is changed into liquid to return to the tower, and the liquid falls to continue the reaction, and the other part of the mixture with high methanol content continues to ascend until the mixture is condensed and collected by the external condenser; and the reboiler at the bottom of the tower body is used for vaporizing the liquid falling to the bottom of the tower again to form high-temperature gas, the high-temperature gas returns to the tower, and the high-temperature gas rises to continuously react with the materials, so that the reaction efficiency is improved.
Drawings
Fig. 1 is a schematic structural diagram of the system provided by the present invention.
Detailed Description
Embodiments of the present invention will be described in detail below with reference to examples, but those skilled in the art will understand that the following examples are only for illustrating the present invention and should not be construed as limiting the scope of the present invention.
Example 1: a reaction rectifying tower with a built-in reflux device comprises a tower body 1, wherein a built-in condenser 2 is arranged at the upper part in the tower body, a gas baffle 3 is arranged above the built-in condenser, and a gas-liquid distributor 4 is arranged below the built-in condenser; a phenol feeding hole 5 and a dimethyl carbonate feeding hole 6 are sequentially arranged on the tower body below the gas-liquid distributor from top to bottom, and a product outlet 7 is arranged at the bottom; a reboiler 8 is arranged outside the tower body 1, and the reboiler 8 and the bottom of the tower body 1 form a circulation loop.
In a preferred scheme, an external condenser 9 is connected to the outer side of the top of the tower body 1.
In a preferable scheme, the built-in condenser is a U-shaped pipe, is uniformly distributed in the upper space of the tower body, and is provided with a water inlet 10 and a water outlet 11 which extend out of the tower.
In a preferable scheme, the gas baffle plate is uniformly distributed with gas holes.
In the preferred scheme, built-in condenser top and below, the bottom of tower body all is equipped with the thermometer, and installs flow control valve and temperature sensor on the pipeline of built-in condensation water inlet. The flow control valve is used for controlling the flow of the built-in condensation water inlet, and the temperature sensor is used for monitoring the temperature above the built-in condenser. For the convenience of implementation of a person skilled in the art, the model of the temperature sensor can be selected from AD7417ARZ, and the model of the flow regulating valve can be selected from V130D05 self-operated flow regulating valve.
In a preferable scheme, the tower body 1 is a packed tower or a plate tower, and the inner wall of the tower body and the outer wall of the built-in condenser are both provided with an anticorrosive coating.
During the operation, phenol (containing catalyst) and dimethyl carbonate at certain temperature are made to flow back into the tower and produce ester exchange reaction at high temperature and in the presence of catalyst to produce methanol with low boiling point, methyl phenyl carbonate with high boiling point and diphenyl carbonate. Dimethyl carbonate and methanol with low boiling points can easily rise to the top of the tower. The condensate enters a built-in condenser in the reactive distillation column through a flow regulating valve, exchanges heat with gas liquid of the ascending dimethyl carbonate and methanol in the distillation column, a part of the dimethyl carbonate and the methanol are cooled into liquid and flow back to a kettle at the bottom of the column, and the liquid contacts with a reaction system in the column again to continue the reaction. And a part of the dimethyl carbonate and the methanol continuously rise to the top in the rectifying tower, and are completely condensed into liquid through an external condenser at the top, so that the liquid is removed out of the rectifying tower. The temperature at the top of the internal condenser is controlled by the flow of condensate. The pressure in the tower is controlled by an external condenser, and the temperature in the tower is controlled by the flow of condensate of a condensing pipe in the tower and a reboiler at the tower kettle. The product flows out of a discharge pipe at the bottom of the tower.

Claims (6)

1. A reaction rectifying tower with a built-in reflux device is characterized by comprising a tower body (1), wherein a built-in condenser (2) is arranged at the upper part in the tower body, a gas baffle (3) is arranged above the built-in condenser, and a gas-liquid distributor (4) is arranged below the built-in condenser; a phenol feeding hole (5) and a dimethyl carbonate feeding hole (6) are sequentially arranged on the tower body below the gas-liquid distributor from top to bottom, and a product outlet (7) is arranged at the bottom; a reboiler (8) is arranged outside the tower body (1), and the reboiler (8) and the bottom of the tower body (1) form a circulation loop.
2. The reactive distillation column with a built-in reflux device as set forth in claim 1, wherein: the outer side of the top of the tower body (1) is connected with an external condenser (9).
3. The reactive distillation column with a built-in reflux device as set forth in claim 1, wherein: the built-in condenser is a U-shaped pipe, is uniformly distributed in the upper space of the tower body, and is provided with a water inlet (10) and a water outlet (11) which extend out of the tower.
4. The reactive distillation column with a built-in reflux device as set forth in claim 1, wherein: the gas baffle is evenly distributed with gas holes.
5. The reactive distillation column with a built-in reflux device as set forth in claim 3, wherein: the bottom of the tower body is provided with a thermometer above and below the built-in condenser, and a flow regulating valve is arranged on a pipeline of the built-in condensation water inlet.
6. The reactive distillation column with a built-in reflux device as set forth in claim 1, wherein: the tower body (1) is a packed tower or a plate tower, and the inner wall of the tower body and the outer wall of the built-in condenser are both provided with an anticorrosive coating.
CN202120914544.4U 2021-04-29 2021-04-29 Reaction rectifying tower with built-in reflux device Active CN215026071U (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202120914544.4U CN215026071U (en) 2021-04-29 2021-04-29 Reaction rectifying tower with built-in reflux device

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202120914544.4U CN215026071U (en) 2021-04-29 2021-04-29 Reaction rectifying tower with built-in reflux device

Publications (1)

Publication Number Publication Date
CN215026071U true CN215026071U (en) 2021-12-07

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Family Applications (1)

Application Number Title Priority Date Filing Date
CN202120914544.4U Active CN215026071U (en) 2021-04-29 2021-04-29 Reaction rectifying tower with built-in reflux device

Country Status (1)

Country Link
CN (1) CN215026071U (en)

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