CN209778708U - Ethanol can retrieve formula ethyl maltol preparation system in succession - Google Patents

Abstract

The utility model provides an ethyl maltol preparation system with ethanol capable of being continuously recovered, which comprises a sublimation device, a crystallization device and an ethanol mother liquor recovery device, the sublimation device comprises a sublimation kettle, a rectifying tower and a product tank, the crystallization device comprises a crystallizer and a centrifuge, the ethanol mother liquor recovery device comprises a crude product ethanol tank, an ethanol feeding pump, a distillation tower, a tower bottom reboiler, a waste liquid tank, a tower top condenser, a fractionating tank and a finished product tank for recovering ethanol, in the utility model, after the ethyl maltol crude product is crystallized by adding a proper amount of ethanol in a crystallization kettle, centrifuging by a centrifuge, wherein the solid obtained by centrifuging is ethyl maltol, the obtained liquid is ethanol mother liquor containing ethyl maltol, the ethanol mother liquor is distilled to recover ethanol, and the ethanol obtained after distillation can be further added into a crystallizer for crystallization with the ethyl maltol crude product for reuse. The distillation raffinate can also be returned to a sublimation working section for reprocessing, thereby recovering the ethyl maltol.

Description

Ethanol can retrieve formula ethyl maltol preparation system in succession

Technical Field

The utility model relates to an ethyl maltol preparation technical field especially relates to a formula ethyl maltol preparation system can be retrieved in succession to ethanol.

Background

Ethyl maltol is a commonly used flavoring agent, has sweet flavor, and is widely applied to the chemical fields of daily chemicals, beverages, foods, medicines, cigarettes and the like.

Ethyl maltol is called ethyl wheat for short, the conventional production process is to sublimate and crystallize the prepared ethyl wheat crude product in sequence to obtain ethyl wheat refined product solid, and in the process, ethanol is needed to wash the ethyl wheat during crystallization, so that a large amount of ethanol mother liquor containing the ethyl wheat is generated.

Disclosure of Invention

There is a need for a continuous ethanol recovery system for ethyl maltol production.

The utility model provides a but ethyl maltol preparation system of ethanol continuous recovery formula, includes sublimation device, crystallization device, ethanol mother liquor recovery unit, the sublimation device includes sublimation cauldron, rectifying column, product groove, and the entry that supplies second wheat crude to get into is seted up at sublimation cauldron top, and sublimation cauldron top is passed through the pipeline and is connected with the rectifying column to send second wheat gas into the rectifying column along the gas phase entry, and the rectifying column includes fractionating tower and condensation segment, sets up gas phase entry and liquid phase export on the lateral wall of fractionating tower, and rectifying column bottom liquid phase export passes through the pipeline and is connected with the product groove, in order to collect liquid phase second wheat refined product, and the condensation segment sets up the top of fractionating tower, sets up the gas phase export at the top of condensation segment, the bottom of product groove pass through the pipeline with crystallization device connects, crystallization device includes crystallizer, centrifuge, and the top of crystallizer sets up new ethanol and adds the pipeline, adding new ethanol into a crystallizer, wherein the bottom of the crystallizer is connected with a centrifuge through a pipeline, a liquid phase outlet of the centrifuge is connected with an ethanol mother liquor recovery device, the ethanol mother liquor recovery device comprises a crude ethanol tank, an ethanol feeding pump, a distillation tower, a tower bottom reboiler, a waste liquid tank, a tower top condenser, a fractionation tank and a finished ethanol recovery tank, a liquid phase outlet of the centrifuge is connected with the crude ethanol tank to store the ethanol mother liquor recovered after crystallization, the ethanol mother liquor contains a large amount of ethanol and ethyl maltol, a bottom outlet of the crude ethanol tank is connected with an inlet of the ethanol feeding pump, an outlet of the ethanol feeding pump is connected with a first liquid phase inlet at the upper part of the side wall of the distillation tower through a pipeline to pump the ethanol into the distillation tower, and the distillation tower further comprises a first liquid phase inlet at the upper part of the side wall, a gas phase inlet at the lower, The liquid phase export of bottom, the liquid phase entry of tower bottom reboiler and the liquid phase exit linkage of distillation column, the gas phase export of tower bottom reboiler and the gas phase entry linkage of distillation column, in order to send the ethanol steam after reboiling into the distillation column, the entry of waste liquid groove and the liquid phase exit linkage of distillation column bottom, in order to collect the discharged waste liquid at the bottom of the tower, the gas phase entry of overhead condenser and the gas phase exit linkage at distillation column top, the liquid phase export of overhead condenser and the entry linkage of fraction groove, the export of fraction groove passes through the fraction trunk line and is connected with recovery ethanol finished product groove, in order to collect the ethanol liquid of collecting.

In the invention, after the ethyl maltol crude product is crystallized in a crystallization kettle by adding a proper amount of ethanol, the ethyl maltol crude product is centrifuged by a centrifuge, the solid obtained by centrifugation is ethyl maltol, and the liquid obtained is ethyl maltol-containing ethanol mother liquor. The ethanol mother liquor is distilled to recover ethanol, and the ethanol obtained after distillation can be added into a crystallizer and the ethyl maltol crude product for crystallization for repeated use. The distillation raffinate can also be returned to a sublimation working section for reprocessing, thereby recovering the ethyl maltol.

Drawings

FIG. 1 is a schematic structural diagram of the ethyl maltol production system capable of continuously recovering ethanol.

Fig. 2 is a schematic structural view of the sublimation apparatus.

FIG. 3 is a schematic structural view of a crystallization apparatus.

FIG. 4 is a schematic structural diagram of an ethanol mother liquor recovery device.

Fig. 5 is a control block diagram of the control valve.

In the figure: the ethanol mother liquor recovery device 10, a crude ethanol tank 11, an ethanol feed pump 12, a distillation tower 13, a first liquid phase inlet 131, a gas phase inlet 132, a gas phase outlet 133, a liquid phase outlet 134, a second liquid phase inlet 135, a second liquid level meter 136, a pipeline 137 for discharging residual liquid, a temperature detector 138, a tower bottom reboiler 14, a first flow control valve 141, a waste liquid tank 15, an overhead condenser 16, a fraction tank 17, a fraction main pipeline 171, a first liquid level meter 172, a concentration detector 173, a finished ethanol recovery tank 18, a sublimation device 20, a sublimation kettle 21, a rectification tower 22, a fractionation tower 221, a liquid phase reflux inlet 2211, a liquid phase flow outlet 2212, a three-way control valve 2213, a condensation section 222, a product tank 23, a vacuum tank 24, a sublimation process fractionation tank 25, a crystallization device 30, a crystallizer 31, a centrifuge 32 and a recovered ethanol pipeline 33.

Detailed Description

In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings required to be used in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and it is obvious for those skilled in the art that other drawings can be obtained according to these drawings without creative efforts.

Referring to fig. 1 to 5, the embodiment of the present invention provides a continuous ethanol recovery type ethyl maltol preparation system, which includes a sublimation device 20, a crystallization device 30, and an ethanol mother liquor recovery device 10.

Sublimation device 20 is including sublimating cauldron 21, rectifying column 22, product groove 23, the entry that supplies second wheat crude product to get into is seted up at sublimating cauldron 21 top, sublimating cauldron 21 top is passed through the pipeline and is connected with rectifying column 22, send second wheat gas into rectifying column 22 along the gaseous phase entry, rectifying column 22 includes fractionating tower 221 and condensation segment 222, set up gaseous phase entry and liquid phase export on fractionating tower 221's lateral wall, rectifying column 22 bottom liquid phase export passes through the pipeline and is connected with product groove 23, in order to collect liquid phase second wheat refined product, condensation segment 222 sets up in fractionating tower 221's top, set up gaseous phase export at condensation segment 222's top, the bottom of product groove 23 pass through the pipeline with crystallization device 30 connects.

The crystallizing device 30 comprises a crystallizer 31 and a centrifuge 32, wherein a new ethanol adding pipeline is arranged at the top of the crystallizer 31 to add new ethanol into the crystallizer 31, the bottom of the crystallizer 31 is connected with the centrifuge 32 through a pipeline to centrifugally treat crystallized ethyl wheat concentrate so as to separate ethanol from ethyl wheat, the separated ethyl wheat is sent to a drying device for treatment, the separated ethanol forms ethanol mother liquor, and a liquid phase outlet of the centrifuge 32 is connected with an ethanol mother liquor recovery device 10.

The liquid recovery device 10 comprises a crude ethanol tank 11, an ethanol feeding pump 12, a distillation tower 13, a tower bottom reboiler 14, a waste liquid tank 15, a tower top condenser 16, a fraction tank 17 and a finished product tank 18 for recovering ethanol, wherein the crude ethanol tank 11 stores crystallized and recovered ethanol mother liquid which contains a large amount of ethanol and ethyl maltol, the bottom outlet of the crude ethanol tank 11 is connected with the inlet of the ethanol feeding pump 12, the outlet of the ethanol feeding pump 12 is connected with a first liquid phase inlet 131 at the upper part of the side wall of the distillation tower 13 through a pipeline so as to feed ethanol into the distillation tower 13, the distillation tower 13 further comprises a first liquid phase inlet 131 at the upper part of the side wall, a gas phase reboiler 132 at the lower part of the side wall, a gas phase outlet 133 at the top and a liquid phase outlet 134 at the bottom, the liquid phase inlet of the tower bottom 14 is connected with the liquid phase outlet 134 of the distillation tower 13, the gas phase outlet 133 of, so as to send the ethanol vapor after reboiling into the distillation tower 13, the inlet of the waste liquid tank 15 is connected with the liquid phase outlet 134 at the bottom of the distillation tower 13 to collect the waste liquid discharged from the bottom of the distillation tower, the gas phase inlet 132 of the overhead condenser 16 is connected with the gas phase outlet 133 at the top of the distillation tower 13, the liquid phase outlet 134 of the overhead condenser 16 is connected with the inlet of the fraction tank 17, and the outlet of the fraction tank 17 is connected with the finished product tank 18 for recovering ethanol through the main fraction pipeline 171 to collect the collected ethanol liquid.

Further, the outlet of the fraction tank 17 is also connected to a second liquid-phase inlet 135 of the side wall of the distillation column 13 through a fraction reflux line, the second liquid-phase inlet 135 being near the top of the distillation column 13, the second liquid-phase inlet 135 being located above the first liquid-phase inlet 131.

Because the ethanol mother liquor is pumped into the distillation tower 13 through the ethanol feed pump 12, the ethanol mother liquor has higher pressure when entering the tower body, the second liquid phase port flows into the tower through self-flowing and is not provided with pressure, if the two liquid phase ports adopt one inlet, the two liquid phase ports are closer, the pressure of the ethanol mother liquor entering can push the ethanol liquid in the fraction tank 17 back to the fraction main pipeline 171 along a backflow pipeline, and backflow under pressure is caused, so that not only the potential safety hazard exists, but also impurities in the distillation tower 13 are brought into the fraction main pipeline 171, and therefore, the purity of the ethanol liquid in the ethanol finished product tank 18 is recovered.

Further, still set up first level gauge 172 in fraction groove 17 for detect the minimum liquid level height in the fraction groove 17, still set up the control valve on fraction trunk line 171, first level gauge 172 is connected with the control valve, and the control valve accepts the liquid level signal that first level gauge 172 provided, and the basis liquid level signal action, in order to open or shut off fraction trunk line 171.

In order to ensure that the liquid part in the fraction tank 17 naturally flows back to the distillation tower 13, the liquid level is monitored by a first liquid level meter 172 to be not lower than a certain position, if the liquid level is lower than a certain set position, a control valve is closed, the liquid in the fraction tank 17 is not pumped out to a finished product tank, and therefore the liquid in the fraction tank 17 meets the requirement of partial backflow.

The implementation of this scheme may be: the first liquid level meter 172 monitors the liquid level degree height in real time, and provides the height to the control valve, the control valve comprises a controller and an electromagnetic valve, the controller is internally preset with a height reference value representing a set position in the fraction tank 17, the controller compares the received real-time liquid level height with the height reference value, if the height reference value is higher than the height reference value, the controller sends an action signal to the electromagnetic valve, the electromagnetic valve acts to open the fraction main pipeline 171, and if the height reference value is lower than the height reference value, the controller does not send the action signal to the electromagnetic valve to ensure that part of liquid in the fraction tank 17 flows back stably.

Further, a concentration detector 173 for detecting the concentration of the liquid phase ethanol in the fractionation tank is provided outside the fractionation tank. The concentration detector 173 may be provided at a lower position, and the liquid-phase ethanol in the fractionating tank may be sampled by a branch line, and the concentration detector 173 may be connected to the branch line.

Further, still set up second level gauge 136 at the bottom of distillation column 13, second level gauge 136 is used for detecting the minimum liquid level height of the inside bottom raffinate of distillation column 13, still sets up the control valve on the pipeline 137 of still discharging the raffinate at distillation column 13 bottom liquid phase export 134, second level gauge 136 is connected with the control valve, and the control valve accepts the liquid level signal that second level gauge 136 provided, and according to the action of liquid level signal, with the pipeline 137 that discharges the raffinate open or shut down.

In order to ensure that the reboiler 14 at the bottom of the column has enough liquid to reboil to form a gas phase and maintain the dynamic balance of gas and liquid in the distillation column 13, the second level gauge 136 detects the lowest liquid level in the column, and when the detected liquid level is lower than the lowest liquid level, the control valve is closed and no residual liquid is discharged, and when the detected liquid level is higher than the highest liquid level, the control valve is opened to discharge the excessive residual liquid in the column.

The control valve provided on the pipe 137 for discharging the residual liquid may be composed of a controller and an electromagnetic valve, or may be an intelligent control valve combining two into one, the lowest liquid level is pre-stored in the controller in advance, and the electromagnetic valve is provided on the pipe 137 for discharging the residual liquid to perform the opening and closing actions.

Further, the tower bottom reboiler 14 is further provided with a gas phase inlet 132 and a liquid phase outlet 134, the gas phase inlet 132 is connected with external high temperature steam, the liquid phase outlet 134 is used for discharging condensed water, a first flow control valve 141 is further arranged on a pipeline of the reboiler connected with the gas phase inlet 132, a temperature detector 138 is further arranged at the bottom of the distillation tower 13, the temperature detector 138 is used for detecting the tower bottom temperature at the bottom of the distillation tower 13 and providing the tower bottom temperature to the first flow control valve 141, and the first flow control valve 141 controls the temperature entering the gas phase inlet 132 at the bottom of the distillation tower 13 according to the temperature information of the temperature detector 138.

When the gas phase in the distillation tower 13 is insufficient, the temperature at the bottom inside the distillation tower 13 will decrease, and more gas phase needs to be supplemented in time at this time, so the temperature detector 138 detects the real-time temperature at the bottom inside the distillation tower 13, the first flow control valve 141 can be internally integrated with a controller and a flow valve, a reference temperature is preset inside the controller, the controller compares the real-time temperature with the reference temperature, and when the real-time temperature is lower than the reference temperature, the flow of the flow valve is controlled by the controller to increase, so that more gas phase is generated inside the reboiler, more gas phase enters the distillation tower 13, and the temperature inside the distillation tower 13 also rises along with the increase, thereby maintaining dynamic balance.

Further, a recovered ethanol pipeline 33 is arranged at the top of the crystallizer 31 to be connected with the ethanol mother liquor recovery device 10 so as to recycle the recovered ethanol.

The scheme can pump the recovered ethanol into the crystallizer 31 again for use, not only reduces the storage capacity of the ethanol, but also realizes recycling, and the recovered ethanol pipeline 33 of the crystallizer 31 is connected with the recovered ethanol finished product groove.

Further, the sublimation device 20 further includes a vacuum tank 24 and a sublimation process fractionating tank 25, wherein a gas phase outlet at the top of the condensation section 222 of the rectifying tower 22 is connected with the vacuum tank 24, and an outlet is further arranged at the top of the vacuum tank 24 to be connected with the fractionating tank, so as to send the buffered gas phase into the fractionating tank.

Vacuum tank 24 passes through vacuum pump treatment, and inside formation vacuum does benefit to other entering, and gaseous process vacuum tank 24 buffering back, mobility is stable, in getting into sublimation process fraction groove 25, is absorbed.

Further, a liquid phase reflux port 2211 is further disposed at the top of the fractionating tank of the sublimation apparatus 20, a liquid phase reflux port 2211 is disposed on the side wall of the fractionating tower 221 between the packing section and the condensing section 222 of the rectifying tower 22, and the liquid phase reflux port 2211 of the fractionating tower 221 is connected to the liquid phase reflux port 2211 of the fractionating tank through a pipeline, so as to realize reflux of the liquid phase ethyl barley and maintain stable circulation of the rectifying tower 22.

Furthermore, a three-way control valve 2213 is further arranged on a pipeline between the fractionating tower 221 and the fraction tank, a liquid phase outlet 2212 is further formed in the side wall of the fractionating tower 221, two channels of the three-way control valve 2213 are respectively connected with the liquid phase outlet 2212 and the liquid phase return port 2211 on the fractionating tower 221 so as to control whether the liquid phase ethyl wheat flows back or not and discharge the liquid phase ethyl wheat, and the height of the liquid phase outlet 2212 on the fractionating tower 221 is higher than that of the liquid phase return port 2211 and the two are farthest away from each other in the diameter direction of the side wall of the fractionating tower 221.

The liquid phase outflow port 2212 naturally flows out, and the liquid phase return port 2211 is pumped in by a pump, so that the liquid phase outflow port and the liquid phase return port are far away from each other, and the impact of liquid at the return port on the liquid at the outflow port is avoided.

Temperature detector 138 may be a temperature sensor and concentration detector 173 may be a sensor for detecting concentration, such as those commercially available. The first flow control valve 141 may be implemented by a logic circuit, specifically by a comparison circuit, for example, a comparator.

The embodiment of the utility model provides a module or unit in the device can merge, divide and delete according to actual need.

While the invention has been described with reference to a preferred embodiment, it will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the invention.

Claims (10)

1. A ethanol can retrieve formula ethyl maltol preparation system in succession which characterized in that: comprises a sublimation device, a crystallization device and an ethanol mother liquor recovery device, wherein the sublimation device comprises a sublimation kettle, a rectification tower and a product groove, the top of the sublimation kettle is provided with an inlet for crude ethane and wheat products to enter, the top of the sublimation kettle is connected with the rectification tower through a pipeline so as to send ethane and wheat gases into the rectification tower along a gas phase inlet, the rectification tower comprises a fractionating tower and a condensation section, the side wall of the fractionating tower is provided with a gas phase inlet and a liquid phase outlet, the liquid phase outlet at the bottom of the rectification tower is connected with the product groove through a pipeline so as to collect liquid phase refined ethane and wheat products, the condensation section is arranged above the fractionating tower, the top of the condensation section is provided with a gas phase outlet, the bottom of the product groove is connected with the crystallization device through a pipeline, the crystallization device comprises a crystallizer and a centrifuge, the top of the crystallizer is provided with a new ethanol adding pipeline so as to add new ethanol into the, the liquid phase outlet of the centrifuge is connected with an ethanol mother liquor recovery device, the ethanol mother liquor recovery device comprises a crude ethanol tank, an ethanol feeding pump, a distillation tower, a tower bottom reboiler, a waste liquid tank, a tower top condenser, a fractionation tank and a recovered ethanol finished product tank, the liquid phase outlet of the centrifuge is connected with the crude ethanol tank to store the recovered ethanol mother liquor after crystallization, the ethanol mother liquor contains a large amount of ethanol and ethyl maltol, the bottom outlet of the crude ethanol tank is connected with the inlet of the ethanol feeding pump, the outlet of the ethanol feeding pump is connected with a first liquid phase inlet at the upper part of the side wall of the distillation tower through a pipeline to pump the ethanol into the distillation tower, the distillation tower also comprises a first liquid phase inlet at the upper part of the side wall, a gas phase inlet at the lower part of the side wall, a gas phase outlet at the top and a liquid phase outlet at the bottom, the gas phase outlet of the tower bottom reboiler is connected with the gas phase inlet of the distillation tower so as to send the reboiled ethanol steam into the distillation tower, the inlet of the waste liquid tank is connected with the liquid phase outlet at the bottom of the distillation tower so as to collect the waste liquid discharged from the bottom of the distillation tower, the gas phase inlet of the tower top condenser is connected with the gas phase outlet at the top of the distillation tower, the liquid phase outlet of the tower top condenser is connected with the inlet of the fraction tank, and the outlet of the fraction tank is connected with the ethanol finished product recovery tank through a fraction main pipeline so as to collect the collected ethanol liquid.

2. The system for continuously recovering ethyl maltol according to claim 1, wherein: the outlet of the distillate tank is also connected to a second liquid phase inlet in the side wall of the distillation column near the top of the distillation column via a distillate reflux conduit, the second liquid phase inlet being located above the first liquid phase inlet.

3. The system for continuously recovering ethyl maltol according to claim 2, wherein: still set up first level gauge in the fraction groove for detect the minimum liquid level height in the fraction groove, still set up the control valve on the trunk line of fraction, first level gauge is connected with the control valve, and the control valve accepts the liquid level signal that first level gauge provided, and the basis liquid level signal moves, in order to open or shut off the trunk line of fraction.

4. The system for continuously recovering ethyl maltol according to claim 2, wherein: and a concentration detector is also arranged outside the fraction tank and used for detecting the concentration of the liquid-phase ethanol in the fraction tank.

5. The system for continuously recovering ethyl maltol according to claim 1, wherein: still set up the second level gauge in the bottom of distillation column, the second level gauge is used for detecting the minimum liquid level height of the raffinate of the inside bottom of distillation column, still sets up the control valve on the pipeline of the liquid phase export discharge raffinate of distillation column bottom, the second level gauge is connected with the control valve, and the control valve accepts the liquid level signal that the second level gauge provided, and the basis liquid level signal moves to open or shut off the pipeline of discharge raffinate.

6. The system for continuously recovering ethyl maltol according to claim 1, wherein: the tower bottom reboiler is further provided with a gas phase inlet and a liquid phase outlet, the gas phase inlet is connected with external high-temperature steam, the liquid phase outlet is used for discharging condensed water, a first flow control valve is further arranged on a pipeline, connected with the gas phase inlet, of the reboiler, a temperature detector is further arranged at the bottom of the distillation tower, the temperature detector is used for detecting the temperature of the tower bottom of the distillation tower and providing the temperature of the tower bottom to the first flow control valve, and the first flow control valve controls the temperature of the gas phase inlet, entering the bottom of the distillation tower, according to temperature information of the temperature detector.

7. The system for continuously recovering ethyl maltol according to claim 1, wherein: and the top of the crystallizer is also provided with a recovered ethanol pipeline to be connected with an ethanol mother liquor recovery device so as to recycle the recovered ethanol.

8. The system for continuously recovering ethyl maltol according to claim 1, wherein: the sublimation device further comprises a vacuum tank and a sublimation process fractionating groove, the gas phase outlet at the top of the condensation section of the rectifying tower is connected with the vacuum tank, and an outlet is arranged at the top of the vacuum tank to be connected with the fractionating groove so as to send the buffered gas phase into the fractionating groove.

9. The system for continuously recovering ethyl maltol according to claim 1, wherein: still set up liquid phase backward flow mouth at the top of sublimation device's fractionation groove, set up liquid phase backward flow mouth on the lateral wall of fractionating tower between the filler section of rectifying column and condensation segment, the liquid phase backward flow mouth of fractionating tower passes through the pipeline and is connected with the liquid phase backward flow mouth of fractionation groove to realize the backward flow of liquid phase second wheat, maintain the stable cycle of rectifying column.

10. The system for continuously recycling ethyl maltol for ethanol according to claim 9, wherein: the pipeline between the fractionating tower and the fraction groove is provided with a three-way control valve, the side wall of the fractionating tower is provided with a liquid phase outflow port, two channels of the three-way control valve are respectively connected with the liquid phase outflow port and the liquid phase reflux port on the fractionating tower to control whether the liquid phase ethyl wheat flows back or not and discharge the liquid phase ethyl wheat, the height of the liquid phase outflow port on the fractionating tower is higher than that of the liquid phase reflux port, and the liquid phase outflow port and the liquid phase reflux port are farthest away from each other in the diameter direction of the side wall of the fractionating tower.