CN218357428U - Serial-type rectification recovery device - Google Patents
Serial-type rectification recovery device Download PDFInfo
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- CN218357428U CN218357428U CN202222295134.3U CN202222295134U CN218357428U CN 218357428 U CN218357428 U CN 218357428U CN 202222295134 U CN202222295134 U CN 202222295134U CN 218357428 U CN218357428 U CN 218357428U
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Abstract
The utility model discloses a serial-type rectification recovery unit, serial-type rectification recovery unit includes the distillation subassembly, the rectifying column, reboiler and top of the tower condenser, the distillation subassembly includes a plurality of stills and feed liquor pump, a plurality of stills series connection, be connected with the feed liquor pump between the adjacent stills respectively, connect the discharging pipe at the bottom of last stills's the cauldron in order to be used for the ejection of compact, each stills's top is all through pipe connection in the rectifying column, the rectifying column is used for collecting the steam of distillation subassembly and carries out the fractionation, the reboiler is connected in the bottom of rectifying column in order to be used for reboiling to heavy fraction, the top of the tower condenser is connected in the top of rectifying column in order to be used for condensing the light fraction of rectifying column. The recovery device can achieve the purposes of saving equipment, saving energy, keeping the intake components basically constant, ensuring the rectification quality, realizing continuous operation, gathering all concentrated products in one discharging kettle for automatic discharging and saving the operation labor.
Description
Technical Field
The utility model relates to a medicine, chemical industry technical field especially relate to a serial-type rectification recovery unit.
Background
The solvent containing the solid mother liquor is required to be recovered in pharmaceutical factories and chemical factories, and the solvent containing the solid mother liquor has the general property that the solid is usually dissolved in the solvent. The solid in the initial state of the mother liquor is not separated out, the content of the solvent is gradually reduced along with the rectification, the solid originally dissolved in the liquid is completely separated out, and at the moment, if the continuous rectification is carried out, the separated solid can be accumulated on a tower plate of a rectification tower or in a gas-liquid channel of a regular packing, so that the tower body of the rectification tower is blocked. Therefore, the traditional treatment method for recovering the solvent containing the solid mother liquor has two kinds, one is to evaporate the solvent from the mother liquor by a simple evaporation mode, then to collect the condensate containing the solvent and not containing the solid and the mother liquor containing the solid and not containing the solvent respectively, and then to treat the solvent and the solid respectively. Another method is batch rectification, which leaves the solid in a kettle while rectifying, and the method needs more towers and kettles, often more than ten. The two traditional treatment methods have the advantages and the disadvantages respectively, the common disadvantages are that the energy consumption is large, the equipment investment is large, the process of multiple times of evaporation and condensation is adopted, the consumption of steam and circulating cooling water is large, the energy consumption of the whole product is large, the process is discontinuous, the operation switching treatment is required to be continuously carried out by operators, and the manpower is greatly consumed.
SUMMERY OF THE UTILITY MODEL
Based on this, the series connection type rectification recovery device is provided aiming at the problems that the traditional treatment method has large energy consumption, large equipment investment, multiple evaporation and condensation processes, large consumption of steam and circulating cooling water and large labor consumption for discontinuous operation. The utility model discloses a serial-type rectification recovery unit directly utilizes the enthalpy of steam, and the energy saving merges a plurality of independent intermittent type rectifying column into a continuous rectifying column, changes original independent intermittent type rectifying still into a plurality of stills and establishes ties, and the linkage setting ensures that the steam component proportion that gets into the rectifying column in the overall process is invariable basically to each item setting and the adjustment parameter of rectifying column can be fixed basically, and the saving equipment improves the rectification quality. Meanwhile, continuous operation can be realized, all concentrated products are gathered in a discharging kettle, discharging is automatically performed, and operating manpower is greatly saved.
The utility model provides a serial-type rectification recovery unit, includes distillation subassembly, rectifying column, reboiler and top of the tower condenser, the distillation subassembly includes a plurality of stills and feed liquor pump, and is a plurality of the stills series connection is adjacent be connected with respectively between the stills the feed liquor pump, last connect the discharging pipe in order to be used for the ejection of compact at the bottom of stills's the cauldron, each still's top all through the pipe connection in the rectifying column, the rectifying column is used for collecting the steam of distillation subassembly is fractionated and is formed light fraction and heavy fraction, the reboiler connect in the bottom of rectifying column is in order to be used for reboiling heavy fraction, the top of the tower condenser connect in the top of rectifying column is in order to be used for right the light fraction of rectifying column condenses.
In some of these embodiments, the in-line distillation recovery apparatus further comprises a product storage tank connected to the still pot for collecting the concentrated solids-containing feed liquid at the bottom of the still pot.
In some embodiments, the in-line distillation recovery device further comprises a discharge pump connected to the discharge pipe, and the product storage tank is connected to the discharge pump for collecting the concentrated solid-containing liquid at the bottom of the distillation still.
In some of these embodiments, the number of stills is 5 to 8.
In some of these embodiments, the distillation still has a volume of 2m 3 ～12m 3 。
In some of the embodiments, a liquid level meter is arranged in each distillation kettle.
In some embodiments, a steam cooling detection sampling port and/or a kettle material detection sampling port are/is arranged in each distillation kettle.
In some embodiments, the pipeline connecting the top of each distillation still to the rectifying tower is provided with a control valve.
In some embodiments, a stirring mechanism is respectively arranged in each distillation still.
In some embodiments, a program-controlled heating device is arranged outside the distillation still.
The series-connection type rectification recovery device combines a plurality of batch rectifications into one continuous rectification, saves equipment, utilizes the vaporization heat of a general distilled solvent to directly enter the rectifying tower, does not need the processes of condensation and reboiling, saves energy, is arranged in a linkage manner, keeps the air inflow and the contained component proportion basically constant, facilitates the rectification arrangement, and ensures the rectification quality. Meanwhile, continuous operation can be realized, all concentrated products are gathered in a discharging kettle, discharging is automatically carried out, and operation labor is greatly saved.
Drawings
In order to more clearly illustrate the technical solutions in the embodiments of the present application, the drawings used in the description of the embodiments will be briefly described below. It is obvious that the drawings in the following description are only some embodiments of the application, and that other drawings can be derived from these drawings by a person skilled in the art without inventive effort.
For a more complete understanding of the present application and its advantages, reference is now made to the following descriptions taken in conjunction with the accompanying drawings. Wherein like reference numerals refer to like parts in the following description.
Fig. 1 is a schematic view of a series-type rectification recovery device according to an embodiment of the present invention;
description of the reference numerals
10. A series rectification recovery device; 100. a distillation kettle; 101. a liquid inlet pump; 200. a discharge pump; 300. a rectifying tower; 400. a reboiler; 500. a tower top condenser; 600. and (5) a product storage tank.
Detailed Description
In order to make the above objects, features and advantages of the present invention more comprehensible, embodiments of the present invention are described in detail below with reference to the accompanying drawings. In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention. The present invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein, as those skilled in the art will be able to make similar modifications without departing from the spirit and scope of the present invention.
In the description of the present invention, it is to be understood that the terms "center", "longitudinal", "lateral", "length", "width", "thickness", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", "clockwise", "counterclockwise", "axial", "radial", "circumferential", and the like, indicate the orientation or positional relationship based on the orientation or positional relationship shown in the drawings, and are only for convenience of description and simplicity of description, and do not indicate or imply that the device or element referred to must have a particular orientation, be constructed and operated in a particular orientation, and therefore, should not be construed as limiting the present invention.
Furthermore, the terms "first", "second" and "first" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include at least one such feature. In the description of the present invention, "a plurality" means at least two, e.g., two, three, etc., unless explicitly defined otherwise.
In the present invention, unless otherwise explicitly specified or limited, the terms "mounted," "connected," "secured," and the like are to be construed broadly, e.g., as being fixedly connected, detachably connected, or integrated; can be mechanically or electrically connected; they may be directly connected or indirectly connected through intervening media, or they may be connected internally or in any other suitable relationship, unless expressly stated otherwise. The specific meaning of the above terms in the present invention can be understood according to specific situations by those skilled in the art.
In the present application, unless expressly stated or limited otherwise, the first feature may be directly on or directly under the second feature or indirectly via intermediate members. Also, a first feature "on," "above," and "over" a second feature may be directly on or obliquely above the second feature, or simply mean that the first feature is at a higher level than the second feature. A first feature being "under," "below," and "beneath" a second feature may be directly under or obliquely under the first feature, or may simply mean that the first feature is at a lesser elevation than the second feature.
It will be understood that when an element is referred to as being "secured to" or "disposed on" another element, it can be directly on the other element or intervening elements may also be present. When an element is referred to as being "connected" to another element, it can be directly connected to the other element or intervening elements may also be present. The terms "vertical," "horizontal," "upper," "lower," "left," "right," and the like as used herein are for illustrative purposes only and do not denote a unique embodiment.
In the description of the present invention, a plurality of means is one or more, a plurality of means is two or more, and the terms greater than, less than, more than, etc. are understood as excluding the term, and the terms greater than, less than, etc. are understood as including the term. If the first and second are described for the purpose of distinguishing technical features, they are not to be understood as indicating or implying relative importance or implicitly indicating the number of technical features indicated or implicitly indicating the precedence of the technical features indicated.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used herein in the description of the invention is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.
The embodiment of the application provides a serial rectification recovery device 10, which is used for solving the problems that the traditional treatment method is high in energy consumption, large in equipment investment, multiple in evaporation and condensation processes, large in consumption of steam and circulating cooling water, discontinuous in operation and high in labor consumption. The following description will be made with reference to the accompanying drawings.
Fig. 1 shows an exemplary serial rectification recovery device 10 provided in an embodiment of the present application, and fig. 1 is a schematic structural diagram of the serial rectification recovery device 10 provided in the embodiment of the present application. The serial rectification recovery device 10 can be used for industrial waste liquid recovery treatment.
In order to more clearly illustrate the structure of the cascaded rectification recovery device 10, the cascaded rectification recovery device 10 will be described with reference to the accompanying drawings.
Fig. 1 is a schematic structural diagram of a serial rectification recovery device 10 according to an embodiment of the present disclosure. A series connection type rectification recovery device 10 comprises a distillation component, a discharge pump 200, a rectification column 300, a reboiler 400 and an overhead condenser 500.
The distillation assembly comprises a plurality of stills 100 and a liquid inlet pump 101. A plurality of stills 100 are connected in series, and a liquid inlet pump 101 is connected between adjacent stills 100. The discharging pump 200 is connected with the last distillation still 100 through a discharging pipe for discharging solid-containing liquid concentrated at the bottom of the distillation still 100. The top of each still 100 is connected to a rectifying column 300 through a pipe.
The rectification column 300 is used for collecting vapor of the distillation assembly and performing fractionation to form a light fraction and a heavy fraction.
A reboiler 400 is connected to the bottom of the rectification column 300 for reboiling the heavy fraction.
An overhead condenser 500 is connected to the top of the rectifying tower 300 for condensing the light ends of the rectifying tower 300.
In some of these embodiments, the in-line distillation recovery apparatus 10 further comprises a product storage tank 600. A product tank 600 is connected to the discharge pump 200 for collecting the concentrated product pumped by the discharge pump 200.
In some of these embodiments, the number of stills 100 is 5 to 8. Preferably, referring to fig. 1, the number of stills 100 shown in fig. 1 is 5.
In some of these embodiments, still 100 has a volume of 2m 3 ～12m 3 . The volume of the distillation still 100 can be set according to actual needs.
In some of these embodiments, a level gauge is disposed within each still 100. The liquid level gauge is used to detect the liquid level in the distillation still 100.
In some embodiments, a steam cooling detection sampling port is disposed in each distillation still 100. The steam cooling detection sampling port is used for detecting the steam in the distillation kettle 100 after cooling and sampling so as to match each distillation kettle 100 for switching stage heating.
In some embodiments, each distillation still 100 is provided with a sampling port for detecting the material in the distillation still. The material detection sampling port in the kettle is used for detecting the liquid material in the kettle of the distillation kettle 100 after sampling so as to match each distillation kettle 100 for switching stage heating.
In some embodiments, the pipeline connecting the top of each distillation still 100 to the rectifying tower 300 is provided with a control valve.
In some embodiments, each of the stills 100 is provided with a stirring mechanism therein. The stirring mechanism is used for stirring the liquid in the distillation kettle 100.
In some embodiments, a temperature-raising heating device with program control is arranged outside each distillation still 100. The program-controlled heating device is used for accurately controlling the temperature of the distillation kettle 100 at different stages, so that the steam components are more uniform.
The utility model also aims to provide a serial rectification recovery method.
A series connection type rectification recovery method uses a series connection type rectification recovery device 10, and comprises the following steps:
step 1, allowing a solution to be treated containing a solvent to enter a first distillation kettle 100 for kettle distillation, allowing a concentrated product produced in the first distillation kettle 100 to enter a next distillation kettle 100 for kettle distillation, pumping solid-containing liquid at the bottom of the last distillation kettle 100 out by a discharge pump 200, and allowing steam produced in each distillation kettle 100 to enter a rectifying tower 300; and
and 2, fractionating the steam by using the rectifying tower 300 to form a light fraction and a heavy fraction.
In some embodiments, step 1 specifically includes the following steps: controlling the distillation temperature T1 in the first distillation kettle 100, allowing a solution containing a solvent to be treated to enter the first distillation kettle 100 for kettle distillation, performing online sampling detection to detect that the content of a distilled vapor solvent in the first distillation kettle 100 is a first vapor solvent preset value or the content of a material solvent in the distillation kettle is a first material solvent preset value, starting constant liquid level discharging after reaching a preset liquid level, and keeping the dynamic balance of liquid phase feeding amount, gas phase evaporation amount and liquid phase discharging amount of the first distillation kettle 100;
controlling the distillation temperature T2 in the second distillation kettle 100, allowing the solid-containing liquid at the bottom of the first distillation kettle 100 to enter the second distillation kettle 100 for kettle distillation, performing online sampling detection to detect whether the content of the distilled vapor solvent in the second distillation kettle 100 is a preset value of a second vapor solvent or the content of the material solvent in the distillation kettle is a preset value of a second material solvent, starting constant liquid level discharge after reaching a preset liquid level, and keeping the dynamic balance of the liquid phase feed quantity, the gas phase evaporation quantity and the liquid phase discharge quantity of the second distillation kettle 100;
and analogizing in turn, controlling the distillation temperature Tn in the last distillation kettle 100, allowing the solid-containing liquid at the bottom of the (n-1) th distillation kettle 100 to enter the last distillation kettle 100 for kettle distillation, performing online sampling detection until the content of the distilled vapor solvent in the last distillation kettle 100 is the nth vapor solvent preset value or the content of the material solvent in the distillation kettle is the nth material solvent preset value, starting constant liquid level discharge after reaching the preset liquid level, and keeping the dynamic balance of the liquid phase feed quantity, the gas phase evaporation quantity and the liquid phase discharge quantity of the last distillation kettle 100.
In this embodiment, the first distillation still 100 evaporates first, and evaporates and discharges the vapor phase simultaneously at a constant rate, and the liquid level of the evaporated concentrate gradually rises to reach a predetermined liquid level, and then the first distillation still 100 discharges the vapor to the next distillation still (the second distillation still 100). The evaporation capacity and the feeding speed of the serial rectification recovery device 10 need to be calculated theoretically in advance according to the actual situation of the feed liquid to be evaporated, the feed liquid is fed while the constant liquid level is kept after the liquid level in the first distillation kettle 100 is actually reached, the concentration of the solvent in the kettle does not deviate too much at the moment, if the concentration of the solvent deviates slightly, the evaporation capacity is adjusted by adjusting the amount of the heating steam, the actual feeding speed is kept basically unchanged, and the next kettle is discharged after the liquid level in the first distillation kettle 100 reaches a set value. The solvent concentration of waiting the liquid phase ejection of compact in the sample detection cauldron on line, if the concentration is too high just increases the heating steam quantity, if the concentration is too low just adjusts the heating steam quantity, as long as the liquid phase input speed of first stills 100 is fixed, liquid phase ejection of compact concentration reaches the default, then the gas phase evaporation capacity is fixed, and the heating steam is also fixed, reaches continuous stable operation, later need not operate the regulating parameter again. The liquid phase feed to the second still 100 is from the liquid phase discharge from the previous still 100. As mentioned above, after the parameters of the first still 100 are stabilized, the liquid phase discharge from the first still 100 is also the liquid phase feed to the second still 100. After the parameters of the second still 100 are stabilized, no additional feed from other sources is available. The second distillation kettle 100 is operated as the first distillation kettle 100, the solvent concentration of liquid phase discharging is detected by sampling, if the solvent concentration is too high, the heating steam dosage is increased, if the solvent concentration is too low, the heating steam dosage is decreased, stable evaporation capacity and stable liquid phase concentration are reached, finally, discharging is started after the liquid level is preset, the whole process is consistent with the operation process of the first distillation kettle 100, and the third distillation kettle 100, the fourth distillation kettle 100 and the fifth distillation kettle 100 are analogized in turn.
In some of these embodiments, the liquid phase feed rate V1= { V1 gas + V2 gas +. + V (n-1) gas + Vn liquid }/t for the first still 100 after the system equilibrium is stabilized; wherein, V1 gas represents the gas phase discharge amount in the first distillation still 100, and so on, vn gas represents the gas phase discharge amount in the nth distillation still 100, and Vn liquid represents the liquid phase discharge amount of the nth distillation still 100.
The liquid phase feed rate V2= V1 liquid/t of the second still 100, V1 liquid represents the liquid phase discharge amount of the first still 100; it should be noted that the liquid-phase feed rate V2 of the second distillation still 100 can also be expressed as V2= { V2 gas +. + V (n-1) gas + Vn liquid }/t.
The liquid phase feeding speed V (n-1) = V (n-2) liquid/t of the (n-1) distillation kettle 100, and the V (n-2) liquid represents the liquid phase discharging amount of the (n-2) distillation kettle 100; it should be noted that the liquid-phase feed rate V3 of the third distillation still 100 can also be expressed as V3= { V3 gas +. + V (n-1) gas + Vn liquid }/t.
The liquid phase feed rate vn of the nth still 100 = V (n-1) liquid/t, where V (n-1) liquid represents the liquid phase discharge amount of the nth still 100; note that the liquid-phase feed rate Vn of the nth still 100 can also be expressed as Vn = { Vn gas + Vn liquid }/t.
Every t hours, the evaporation amount of the gas phase entering the rectifying tower 300 is V1 gas + V2 gas +. + Vn gas, and the discharge amount of the liquid phase of the last distillation kettle 100 is Vn liquid.
Another embodiment of the present invention is to provide an application of the serial-type rectification recovery method.
An application of a serial rectification recovery method in solvent recovery in D/L-panthenoyl lactone mother liquor.
The series-connection type rectification recovery device 10 combines a plurality of batch rectifications into one continuous rectification, saves equipment, utilizes the vaporization heat of a general distilled solvent to directly enter the rectifying tower 300, does not need the processes of condensation and reboiling, saves energy, is arranged in a linkage manner, keeps the air inflow and the contained component proportion basically constant, facilitates the rectification arrangement, and ensures the rectification quality. Meanwhile, continuous operation can be realized, all concentrated products are gathered in a discharging kettle, discharging is automatically performed, and operating manpower is greatly saved.
Example 1
The present embodiment provides a series rectification recovery apparatus 10.
The serial rectification recovery device 10 of the embodiment comprises a distillation assembly, a discharge pump 200, a rectification column 300, a reboiler 400, an overhead condenser 500 and a product storage tank 600.
The distillation assembly includes five stills 100 and four feed pumps 101. Volume of the distillation still 100Is 5m 3 . Each distillation still 100 is provided with a liquid level meter, a material detection sampling port in the still and a steam cooling detection sampling port. Each of the stills 100 is provided therein with a stirring mechanism. Five stills 100 are connected in series, and a program-controlled heating device is arranged outside each stills 100. And a liquid inlet pump 101 is respectively connected between the adjacent stills 100.
The discharging pump 200 is connected with the last distillation kettle 100 for discharging the solid-containing liquid at the bottom of the kettle. Product storage tank 600 is connected to discharge pump 200 for collecting solids-containing liquid at the bottom of the tank pumped by discharge pump 200. The top of each of the five stills 100 is connected to a rectifying column 300. The top of each distillation still 100 is connected to the pipeline of the rectifying tower 300 and is provided with a control valve.
The rectifying tower 300 is used for collecting vapor of the distillation assembly and performing fractionation to form light fraction and heavy fraction.
A reboiler 400 is connected to the bottom of the rectification column 300 for reboiling the heavy fraction.
An overhead condenser 500 is connected to the top of the rectifying tower 300 for condensing the light fraction of the rectifying tower 300.
Example 2
The embodiment provides a serial rectification recovery method.
The serial rectification recovery method of the embodiment uses the serial rectification recovery device 10 of the embodiment, and comprises the following steps:
step 1, the solution to be treated containing the solvent enters a first distillation kettle 100 for kettle distillation, the concentrated product produced in the first distillation kettle 100 enters the next distillation kettle 100 for kettle distillation, the solid-containing liquid at the bottom of the last distillation kettle 100 is pumped out, and the steam produced in each distillation kettle 100 enters a rectifying tower 300.
Specifically, the distillation temperature T1 in the first distillation kettle 100 is controlled, the solution to be treated containing the solvent enters the first distillation kettle 100 for kettle distillation, when the content of the material solvent in the first distillation kettle 100 is detected by online sampling, the constant liquid level discharge is started after the preset liquid level is reached, and the dynamic balance among the liquid phase feed amount, the gas phase evaporation amount and the liquid phase discharge amount of the first distillation kettle 100 is maintained;
controlling the distillation temperature T2 in the second distillation kettle 100, allowing solid-containing liquid at the bottom of the first distillation kettle 100 to enter the second distillation kettle 100 through a liquid inlet pump 101 for kettle-type distillation, performing online sampling detection on the content of a material solvent in the second distillation kettle 100 to be a preset value of a second material solvent, starting constant liquid level discharge after reaching a preset liquid level, and keeping the dynamic balance of the liquid-phase feeding amount, the gas-phase evaporation amount and the liquid-phase discharge amount of the second distillation kettle 100;
and analogizing in turn, controlling the distillation temperature T5 in the fifth distillation kettle 100, allowing solid-containing liquid at the bottom of the fourth distillation kettle 100 to enter the fifth distillation kettle 100 through the liquid inlet pump 101 for kettle-type distillation, performing online sampling detection until the content of the material solvent in the fifth distillation kettle 100 is a fifth material solvent preset value, starting constant liquid level discharging after reaching a preset liquid level, and keeping the dynamic balance of liquid phase feeding amount, gas phase evaporation amount and liquid phase discharging amount of the fifth distillation kettle 100.
After the system is in stable equilibrium, the liquid phase feed rate V1= (V1 gas + V2 gas +. + V5 gas + V5 liquid)/t of the first distillation still 100; v1 gas indicates the amount of gas discharged from the first distillation still 100. V5 gas indicates the amount of gas discharged from the fifth distillation still 100, and V5 liquid indicates the amount of liquid discharged from the fifth distillation still 100.
The liquid-phase feed rate V2= (V2 gas +.. + V5 gas + V5 liquid)/t for the second still 100;
the liquid phase feed rate V3= (V3 gas + V4 gas + V5 liquid)/t of the third still 100;
the liquid phase feed rate V4= (V4 gas + V5 liquid)/t of the fourth still 100;
the liquid phase feed rate V5= (V5 gas + V5 liquid)/t of the fifth distillation still 100;
every t hours, the evaporation amount of the gas phase entering the rectifying tower 300 is V1 gas + V2 gas +. + V5 gas, and the discharge amount of the liquid phase of the last (fifth) distillation kettle 100 is V5 liquid.
And 2, when the last distillation kettle 100 is discharged in a liquid phase, solid-containing material liquid at the bottom of the distillation kettle is pumped out, and when the distillation kettle 100 is discharged in a gas phase, the produced steam enters the rectifying tower 300.
And 3, fractionating the steam by using the rectifying tower 300 to form a light fraction and a heavy fraction.
Example 3
The serial rectification recovery method of the embodiment is used for treating D/L-pantolactone process wastewater: the process wastewater is extracted with ethyl acetate to obtain a recovered extract, and the recovered extract is treated by using the serial rectification recovery method of the embodiment.
The recovered extract was introduced into a first distillation still 100 (volume 5 m) 3 ) The liquid phase feed rate v1=1000kg/h, and the recovered extract components and approximate contents of D/L pantolactone are 5%, 5% water, and 90% ethyl acetate. The data after reaching stable equilibrium are as follows:
the feeding speed V1 of the first distillation still 100 is =1000kg/h, the gas phase discharging speed V1 gas is =230kg/h, the liquid phase discharging speed V1 liquid is =770kg/h, and the distillation temperature T1 in the first distillation still 100 is controlled to be =82 ℃.
The feeding speed V2=770kg/h, the gas phase discharging speed V2 gas =210kg/h, and the liquid phase discharging speed V2 liquid =560kg/h of the second distillation still 100, and the distillation temperature T2=85 ℃ in the second distillation still 100 is controlled.
The feeding speed V3=560kg/h, the gas phase discharging speed V3 gas =200kg/h, the liquid phase discharging speed V3 liquid =360kg/h, and the distillation temperature T3=88 ℃ in the third distillation still 100 are controlled.
The feeding speed V1 of the fourth distillation still 100 is =360kg/h, the gas phase discharging speed V4 gas is =150kg/h, the liquid phase discharging speed V4 liquid is =210kg/h, and the distillation temperature T4 in the fourth distillation still 100 is controlled to be =93 ℃.
The fifth distillation still 100 has a feeding speed V5=210kg/h, a gas phase discharging speed V5 gas =140kg/h, and a liquid phase discharging speed V5 liquid =70kg/h, and the distillation temperature T5=101 ℃ in the fifth distillation still 100 is controlled.
In example 3, the D/L-pantolactone solution to be treated initially contained 5% lactone, 90% ethyl acetate solvent, and 5% water, and in the example, five distillation vessels 100 were provided, and the concentrations of ethyl acetate discharged from the phase solvent per vessel were set to 65%,45%,25%,10%, and 0.05%, respectively (the data can be adjusted according to actual equipment conditions). Even if the concentration of the ethyl acetate in the last two kettles is very low, the lactone cannot be precipitated in a solid state due to the existence of water, and the lactone is also a liquid solution and can be pumped out through the liquid inlet pump 101. (As applied to other cases with solid precipitation, preferably, the solid content is controlled to be not more than 20% so as to smoothly pump the feed liquid out of the kettle and transfer the feed liquid).
Therefore, the gas phase discharge speed, i.e. the feeding speed of the rectifying tower 300, is V fine =930kg/h (V1 gas + V2 gas + V3 gas + V4 gas + V5 gas, component ethyl acetate 900kg/h, water 30kg/h, water content 3.2%).
Through detection and calculation, the rectifying tower 300 discharges light fractions, v is light =899kg/h (the component is ethyl acetate 899kg/h, and the content is more than 99.8%); the rectification column 300 discharges a heavy fraction, v weight =29.9kg/h (composition water 29.9kg/h, content > 99.9%).
In the foregoing embodiments, the descriptions of the respective embodiments have respective emphasis, and for parts that are not described in detail in a certain embodiment, reference may be made to related descriptions of other embodiments.
All possible combinations of the technical features of the above embodiments may not be described for the sake of brevity, but should be considered as within the scope of the present disclosure as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only represent some embodiments of the present invention, and the description thereof is specific and detailed, but not to be construed as limiting the scope of the present invention. It should be noted that, for those skilled in the art, without departing from the spirit of the present invention, several variations and modifications can be made, which are within the scope of the present invention. Therefore, the protection scope of the present invention should be subject to the appended claims.
Claims (10)
1. The series connection type rectification recovery device is characterized by comprising a distillation assembly, a rectification tower, a reboiler and an overhead condenser, wherein the distillation assembly comprises a plurality of distillation kettles and a liquid inlet pump, the distillation kettles are connected in series, the liquid inlet pump is connected between the adjacent distillation kettles respectively, a discharge pipe is connected to the bottom of the last distillation kettle for discharging, the top of each distillation kettle is connected to the rectification tower through a pipeline, the rectification tower is used for collecting steam of the distillation assembly and conducting fractionation to form light fraction and heavy fraction, the reboiler is connected to the bottom of the rectification tower for reboiling the heavy fraction, and the overhead condenser is connected to the top of the rectification tower for condensing the light fraction of the rectification tower.
2. The tandem rectification recovery device according to claim 1 further comprising a product storage tank connected to the still pot for collecting the concentrated solids-laden liquid at the bottom of the still pot.
3. The tandem rectification recovery device according to claim 2, further comprising a discharge pump connected to the discharge pipe, wherein the product storage tank is connected to the discharge pump for collecting the concentrated solids-containing liquid at the bottom of the distillation still.
4. The tandem type rectification recovery device according to any one of claims 1 to 3, wherein the number of the distillation kettles is 5 to 8.
5. The tandem type rectification recovery device according to any one of claims 1 to 3, wherein the volume of the distillation kettle is 2m 3 ～12m 3 。
6. The series connection type rectification recovery device according to any one of claims 1 to 3, wherein a liquid level meter is arranged in each distillation kettle.
7. The series connection type rectification recovery device according to any one of claims 1 to 3, wherein a steam cooling detection sampling port and/or a material detection sampling port in the distillation kettle is/are arranged in each distillation kettle.
8. The series connection type rectification recovery device according to any one of claims 1 to 3, wherein a control valve is respectively arranged on a pipeline connecting the top of each distillation still to the rectification tower.
9. The tandem type rectification recovery device according to any one of claims 1 to 3, wherein a stirring mechanism is arranged in each distillation kettle.
10. The series connection type rectification recovery device according to any one of claims 1 to 3, wherein a program-controlled temperature rise heating device is arranged outside the distillation kettle.
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| CN202222295134.3U CN218357428U (en) | 2022-08-29 | 2022-08-29 | Serial-type rectification recovery device |
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