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EP4072697A1 - Procédé pour faire fonctionner une colonne de distillation - Google Patents

Procédé pour faire fonctionner une colonne de distillation

Info

Publication number
EP4072697A1
EP4072697A1 EP20819765.7A EP20819765A EP4072697A1 EP 4072697 A1 EP4072697 A1 EP 4072697A1 EP 20819765 A EP20819765 A EP 20819765A EP 4072697 A1 EP4072697 A1 EP 4072697A1
Authority
EP
European Patent Office
Prior art keywords
temperature
distillation column
transfer medium
heat transfer
sump
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
EP20819765.7A
Other languages
German (de)
English (en)
Inventor
Klaus Mertens
Sabine Pegel
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Covestro Deutschland AG
Original Assignee
Covestro Deutschland AG
Covestro Intellectual Property GmbH and Co KG
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Covestro Deutschland AG, Covestro Intellectual Property GmbH and Co KG filed Critical Covestro Deutschland AG
Publication of EP4072697A1 publication Critical patent/EP4072697A1/fr
Pending legal-status Critical Current

Links

Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
    • B01D3/42—Regulation; Control
    • B01D3/4211—Regulation; Control of columns
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
    • B01D3/42—Regulation; Control
    • B01D3/4211—Regulation; Control of columns
    • B01D3/425—Head-, bottom- and feed stream
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C201/00—Preparation of esters of nitric or nitrous acid or of compounds containing nitro or nitroso groups bound to a carbon skeleton
    • C07C201/06—Preparation of nitro compounds
    • C07C201/16—Separation; Purification; Stabilisation; Use of additives

Definitions

  • the present invention relates to a method for continuously operating a distillation column which is set up to separate a substance mixture S which essentially contains a substance A and a substance B which has a significantly higher boiling point than substance A.
  • the reverse ratio is changed as a function of the feed stream and, at the same time, the energy input via the heat transfer medium is proactively changed (so-called feed-forward control) by switching on the feed stream.
  • the sump temperature is monitored and the control structure is changed if the sump temperature drops too far when the heat transfer medium is reduced via the feed stream.
  • the control concept described provides for keeping the ratio of the bottom stream withdrawn from the distillation column to this fed feed stream as constant as possible, controlling the quality of the top stream withdrawn in such a way that its content of (comparatively) high-boiling compounds must not be too high, and to achieve these two goals in such a way that the distillation column can be operated as energy-efficiently as possible.
  • a large number of process parameters are measured and entered into a computer, which calculates signals from these and from previously set target values, which are transmitted to actuators (especially valves) for the return flow rate, sump withdrawal rate and the like.
  • the computer is used to control the amount of fuel fed to the evaporator of the distillation column (the evaporator is operated by burning fuel oil) and the absolute amount of reflux (to be distinguished from the backward ratio) at the top of the distillation column.
  • the two parameters in turn influence the amount of bottom discharge and the composition of the top product.
  • the values for the amount of fuel oil and reflux to be fed should be kept as low as possible in order to operate the distillation column as energy-efficiently as possible.
  • the manipulated variable of the valve for the supply of fuel is determined from the difference between the target value for the mass flow of fuel and its measured actual value, the target value for the mass flow of fuel from the computer, taking into account the feed flow rate, the flow rate of the withdrawn bottom product and the temperature of the feed, the temperature of the top product after its condensation (which is a measure of the composition of the top product under the particular conditions of the separation task described) and the temperature of the evaporator Distillation column fed proportion of the bottom product is determined.
  • the manipulated variable of the return valve is determined from the difference between the target value for the return and its measured actual value, the target value for the return from the computer taking into account the inflow flow rate, the flow rate of the withdrawn bottom product and the temperature of the top product removed in gaseous form and the temperature of the top product after its condensation (which is a measure of the composition of the top product under the particular conditions of the separation task described) is determined.
  • control concept described here is not applicable to a separation task as described at the beginning - separation of a substance mixture S consisting essentially of a substance A and a substance B with significantly different boiling points, because here the temperature profile of the distillation column is due to the lack of a "smooth transition" of the boiling points Individual components do not run essentially linearly in one another and, furthermore, the temperature of the distillate does not allow any particular statements about its composition (at least not in the same way as in the case of the distillation of a hydrocarbon mixture).
  • US Pat. No. 3,905,873 relates to a method and a device for controlling a process with three variable and linked conditions, in particular for controlling a fractionation tower.
  • the described control unit comprises four control systems, namely (1) a distribution system, (2) a reverse flow control system, (3) a pressure control system, and (4) an advance system.
  • the main function of the distribution system is to control the division between distillate and bottoms. As the feed stream flow rate increases or decreases, this manifold system ensures that the distillate and bottoms draw will increase or decrease in exact proportion. If the composition changes, this distribution system can change the division between the distillate and bottoms and thus ensure that the product conditions be maintained.
  • the reverse flow control system regulates the reverse flow rate.
  • a new feature of this system is the use of the return flow temperature to change the return flow rate when the return flow temperature deviates from a predetermined standard temperature.
  • This system further comprises means which (a) prevent the tower from running completely dry when the feed flow is being determined and which (b) minimize the risk of the tower being flooded, i.e. filled with liquid.
  • the pressure control system ensures that the tower pressure remains essentially constant. It includes a control mechanism that regulates the heating current throughput. The heating current is increased or weakened and thus keeps the tower pressure constant in accordance with the pressure changes that occur.
  • This system comprises a device for the operator to switch between automatic and manual control mode. In the case of manual control, automatic switching enables easy switching to automatic control.
  • the advance system ensures that the material balance in the tower is maintained. This is achieved by continuously monitoring the liquid level at the bottom of the tower.
  • the liquid can move within predetermined limits (positions 490 and 492 in the figures) without a correction being made, provided that the mirror limits are not in danger of being exceeded, as can be seen from the relationship between a control signal that has a function feed stream flow rate, feed composition, both optionally, and a liquid level signal.
  • distillation column From an economic point of view, it is of great importance to operate a distillation column as energy-efficiently as possible and to keep the quality of the distillation products as constant and at a high level as possible.
  • Another aim is to make the operation of a distillation column as user-friendly as possible, ie in a way that requires manual intervention by the operating personnel only as rarely as possible and, if possible, without the need to carry out complex processes, in particular even in states dated Deviate from normal operation, for example in the event of a sudden change in the feed rate into the distillation column.
  • the invention provides the following:
  • a vertically arranged column body comprising a stripping part (110) and an amplifier part (120) arranged above, wherein (at least) the stripping part has a temperature measuring device for measuring the stripping part temperature T (AT);
  • a column bottom (130) below the stripping section for receiving a liquid bottom product B 1 at a bottom temperature T (B1) up to a bottom H (B1);
  • (V) a circulation evaporator (200) for heating the column bottom by indirect heating of a first part Bll of the liquid bottom product Bl, the circulation evaporator being supplied with a heat transfer medium W with a flow rate m (W) and the circulation evaporator being supplied via a heat transfer medium valve (210) Adjustment of the flow rate m (W) has;
  • a target value rsoix within a range from rl to r2 is specified for the return flow ratio r and the return flow controller (410) from the specified value rsoix and the value for the mass flow m (S) (preferably determined with a flow measuring device (460 )) the setting of the return valve (320) is calculated taking into account the minimum permissible value rl for r;
  • a target value H (B1) TARGET within the range from H (B1) 1 to H (B1) 2 is specified for the sump level H (B1) and the sump level controller (420) uses this target value H (B 1) SOLL, the current value for the sump level present at a given point in time, H (B1) MOM, and the value for the mass flow m (S), the setting of the sump extraction valve (230) is calculated;
  • a target value T (AT) SOLL within the range from T (AT) 1 to T (AT) 2 is specified for the stripping section temperature T (AT) and the stripping section temperature controller (430) uses this setpoint Value T (AT) SOLL, the current value for the stripping section temperature at a given point in time, T (AT) MOM, and the flow rate m (S) the setting of the heat transfer medium valve (210) calculated and the setting of the heat transfer medium valve (210) calculated in this way is transmitted to it by means of the volume flow controller (450); and
  • a target value T (B 1) TARGET within the range from T (B1) 1 to T (B1) 2 is specified for the sump temperature T (B1) and the sump temperature limiting controller (440) is set up in such a way that if the temperature falls below T (B1) 1, the setting of the heat transfer medium valve (210) is changed, disabling the setting of the heat transfer medium valve (210) according to (iii), so that the flow rate m (W) is increased, the setting of the Heat transfer medium valve (210) according to (iii) is activated again as soon as the sump temperature T (B1) is again within the range from T (B1) 1 to T (B1) 2.
  • Feed stream is changed (steps (ii) and (iii)), which leads to more efficient operation of the column. This requires simultaneous observation of the sump temperature and a change in the control structure if the sump temperature drops too far when the heat transfer medium is reduced as a result of changes in the feed flow (feed-forward control) (step (iv)).
  • steps (i) to (iv) in their entirety represent a complex multivariable control or a multivariate system, with steps (i) to (iv) interacting synergistically in the following way in particular: a) steps (i) and (iii ) determine the internal column flows and ensure that they are balanced and coordinated with one another so that the required
  • Distillation quality can be achieved.
  • the high temperature sensitivity of the distillation column compared to other separation tasks (such as the separation of hydrocarbon mixtures discussed at the beginning) is taken into account by measuring the temperature of the stripping section.
  • Step (iv) ensures that the distillation column is robust and around the in its
  • step (iv) Design of the specified working range (in particular with regard to the temperature window in which the distillation column is to be operated, specified work area) can be operated around.
  • the control operation of step (iv) intervenes if the work or design area is significantly left, so that the safe operation of the column can no longer be guaranteed.
  • the working range is reached again (as soon as the sump temperature T (B1) is again within the range from T (B1) 1 to T (B 1) 2), the mode described under point a is used again.
  • Steps (ii) and (iii) regulate the relationship between external and internal volume flows. Both controls are coordinated in particular with one another and the control parameters are designed together and in combination with one another.
  • step (i) is thus also determined and the internal flow rates are brought into equilibrium both in the buoyancy and in the stripping section and the desired quality of the distillation is established.
  • the distillation column (1000) is set up to separate a mixture of substances S comprising a substance A and a substance B boiling higher than substance A (under the pressure conditions selected for operating the distillation column) must be sufficiently large to enable the separation of one substance (namely A) at the top and the separation of the other substance (namely B) in the bottom of the distillation column.
  • a boiling point difference between A and B at 1.01 bar of 10 ° C. or more, particularly preferably of 25 ° C. or more, very particularly preferably of 50 ° C. or more.
  • the boiling point difference between A and B will not exceed 250 ° C.
  • substance A Since substance A has a lower boiling point than substance B under the pressure conditions selected for operating the distillation column, substance A is also referred to below as a low boiler. It is conceivable, and does not go beyond the scope of the present invention, for the substance mixture S to have, in addition to the low-boiling point A, further compounds A 'which boil more than substance B (i.e. further low-boiling components), in particular low-boiling impurities. These are separated off together with substance A at the top of the distillation column and are therefore part of the top product A1. In an analogous manner, the mixture of substances S can also contain comparatively high-boiling impurities B ', which are in the bottom of the Enrich the distillation column and become part of the bottom product Bl.
  • the total mass fraction of substance A and substance B in mixture S is at least 90%, preferably at least 95%, particularly preferably at least 98%, based on the total mass of substance mixture S.
  • stripping part (AT) is used in the terminology of the present The invention is understood as the area below the feed point (150) of the substance mixture S to be separated, which comprises the entirety of all separating internals present in this area (for example floors or one or more packings) (cf. also FIG. 1 and FIG. 2 , there 110).
  • the stripping section temperature T (AT) is measured in the stripping section understood in this way. The most suitable position for this temperature measuring point can, if necessary, be determined by a person skilled in the art in simple preliminary tests to optimize the control.
  • Packings are preferably used as separating internals, preferably 1 to 3 packs, in particular 1 (exactly one) pack.
  • T stripping section temperature
  • amplifier part is understood in the terminology of the present invention as the area above the feed point (150), which comprises the entirety of all separating internals in this area (see also FIG. 1 and FIG. 2, there 120).
  • packs are preferred, particularly preferably 1 to 3 packs, in particular 1 (exactly one) pack.
  • the bottom stand H (B1) denotes the height of the liquid level of the liquid bottom product B1 measured from the lower limit of the distillation column (see also FIGS. 1 and 2).
  • the expression “lower limit of the distillation column” relates here and in the entire terminology of the present invention to the lowest point of the internal volume of the distillation column which comes into contact with liquid bottom product during operation.
  • the method according to the invention regulates the sump level to the specified target value H (B1) SOLL ⁇ This target value lies within the limits H (B 1) 1 to H (B1) 2.
  • H (B 1) MOM is therefore regulated back to this value in the event of deviations from the target value H (B1) SOLL and does not fluctuate freely between H (B1) 1 to H (B1) 2, as is the case in the regulation according to US Pat. No. 3,905,873 discussed above (there between positions 490 and 492) is the case.
  • the sump level is kept constant in the method according to the invention (ie regulated back to this in the event of deviations from the setpoint value H (B 1) SETPOINT).
  • the target values to be determined in the context of the present invention are of course dependent on the nature of the separation task and the distillation column available for this. The same applies to the specific values to be calculated from the nominal values (such as the setting of the sump extraction valve (220)). Therefore, these values cannot be generalized and must be determined by a person skilled in the art for the given boundary conditions, which, however, represents a purely routine task. Typical values for the preferred application of the separation of benzene as substance A and nitrobenzene as substance B are disclosed further below in the description and in the examples.
  • FIG. 1 shows a schematic representation of a distillation column (1000), the operation of which can be regulated with the method according to the invention
  • FIG. 2 the distillation column from FIG. 1 taking into account process control equipment according to the invention
  • FIG. 3 the benzene content in the bottom product of a distillation column for separating benzene from nitrobenzene and the temperature in the middle of the column at a
  • control unit comprises a flow measuring device (460) for the mixture of substances S fed to the distillation column, with which the mass flow m (S) is determined in step (i).
  • the heat transfer medium is steam.
  • the mixture of substances S comprises benzene as substance A and nitrobenzene as substance B.
  • H (130) denotes the height of the column bottom measured from the lower limit of the distillation column to the lower end of the stripping section
  • T (AT) 1 166 ° C
  • T (AT) 2 172 ° C
  • FIG. 1 shows an example of a distillation column (1000), the operation of which can be regulated in an advantageous manner with the method according to the invention.
  • the mixture of substances S to be separated is fed in from the side between the amplifier part (120) and the stripping part (110).
  • the distillation column can also have other auxiliary devices and peripheral devices known to the person skilled in the art (for example Liquid collectors, liquid distributors, pumps and the like).
  • the gaseous top product A1 is condensed in the top condenser (300), part of the condensate (A21) being returned as reflux to the distillation column and another part (A22) being removed from the distillation column as top product.
  • the mass flow ratio of return to withdrawal, m (A21) / m (A22) is called
  • the return ratio is set using a return valve (320).
  • the top capacitor can also differ from FIG. 1 be integrated into the column body (100).
  • the liquid bottom product B1 fills the column bottom up to the level H (B1), indicated by the dashed line.
  • the distillation column (1000) is heated by means of a circulation evaporator (200), in which a first part of the discharged column bottom (namely B1) is indirectly heated with a heat transfer medium (W) and returned to the column bottom (130). Steam, condensate and other liquid and gaseous heat carriers are suitable as heat transfer media.
  • the mass flow of the heat transfer medium m (W) is set by means of the heat transfer medium valve (210).
  • a second part of the column bottom (namely B12) is discharged as bottom product, the flow rate of the discharged portion being set via the bottom withdrawal valve (230).
  • FIG. 2 shows the process control systems to be used within the scope of the present invention.
  • the mixture of substances S to be separated is first recorded by means of a flow measuring device (460). This mass flow is used to calculate the setpoint value for the return controller (410) via a specified return ratio (in the range r1 to r2).
  • the setpoint value for the reflux ratio rsoix is determined in particular in the design of the distillation column in such a way that the best possible separation can be achieved with as little use of energy as possible.
  • a minimum return flow I WegI (A21) MIN
  • the minimum return (I ⁇ I (A21) MIN) is defined when designing the distillation column by selecting suitable design parameters.
  • the level in the bottom of the column is also regulated as a function of the feed stream via the level controller (420); this is done by adding a disturbance variable to the feed stream S.
  • the temperature of the stripping section T (AT), which determines the quality of the bottom product, is ensured by a temperature controller (430).
  • This controller calculates the target value for the volume flow controller (450) of the heat transfer medium from the specified target value and the inflow flow S. Since it can happen with strong changes in the feed flow that the sump temperature falls below the required minimum temperature due to an insufficient amount of the heat transfer medium, the necessary minimum temperature is ensured via a temperature control (440) in the sump of the column.
  • This temperature controller intervenes when the temperature falls below the minimum, deactivates the control according to (iii) and reactivates it as soon as the sump temperature is again in the range T (B1) 1 to T (B1) 2.
  • Steam is preferably used as the heat transfer medium W.
  • other heat transfer media such as heat transfer oils can also be used.
  • the process according to the invention is suitable for operating distillation columns in which a low boiler A must be separated off from a higher-boiling product B.
  • Benzene is usually used in a stoichiometric excess over nitric acid, especially in the adiabatically operated nitration processes customary today, so that it has to be separated off in the course of working up the nitration product.
  • the work-up of the nitration product is usually done by separating the reaction mixture (nitration product) containing nitrobenzene, unreacted benzene and sulfuric acid into an aqueous sulfuric acid phase and an organic nitrobenzene phase in a first step, followed by a second step multi-stage washing of the nitrobenzene phase, followed by a third step in which the excess benzene is separated from the washed nitrobenzene phase.
  • the excess benzene is usually recycled into the nitration, with the result that the originally used benzene impurities that go through the nitration process essentially unchanged (such as aliphatic organic compounds in particular) accumulate. Since these impurities boil more easily than nitrobenzene, they are distilled off together with the benzene. Excessive accumulation of these impurities is prevented by discharging purge streams and / or by decomposing the impurities after some time.
  • H (B 1) 1 to H (B 1) 2 corresponds to 18% to 42% of the column bottom height H (130) measured from the lower limit of the distillation column to the lower end of the stripping section - see also FIG. 1 and 2;
  • ⁇ Stripping section temperature: T (AT) 1 to T (AT) 2 corresponds to 166 ° C to 172 ° C;
  • T (B1) 1 to T (B1) 2 corresponds to 168 ° C to 173 ° C.
  • the results of the following examples were achieved with a distillation column for separating excess benzene from nitrobenzene.
  • the basic structure of the distillation column corresponded to FIG. 1.
  • the feed stream S consisted of crude nitrobenzene, which had only been separated from the nitrating acid and washed.
  • FIG. 3 shows on the ordinate axis the feed stream S (thick dashed line, in kg / h), the temperature T in the middle of the column (at tray 20, thick solid line, in ° C) and the concentration of benzene (the benzene content c (Bz) expressed as mass fraction) in the column bottom (thin dotted line, in kg benzene / kg column bottom) as a function of the time t indicated on the abscissa axis (in h).
  • FIG. 3 shows, in the same way as for example 1, the feed stream S (thick dashed line), the temperature T in the middle of the column (thin solid line) and the concentration of benzene in the column bottom c (Bz) (thick dotted line).

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

La présente invention concerne un procédé pour faire fonctionner en continu une colonne de distillation, qui est conçu pour séparer un mélange S, qui contient essentiellement une substance A et une substance B, dont le point d'ébullition est significativement plus élevé que celui de la substance A. Dans le procédé selon l'invention, le taux de reflux est modifié selon le flux d'alimentation et, en même temps, l'entrée d'énergie au moyen du milieu de transfert thermique est modifiée de manière proactive (dite commande d'action directe) en tenant compte du flux d'alimentation au moyen d'une commande d'action directe. En même temps, la température de fond est observée et la structure de commande est modifiée si la température de fond tombe trop loin lorsque le milieu de transfert thermique est réduit au moyen du flux d'alimentation.
EP20819765.7A 2019-12-12 2020-12-09 Procédé pour faire fonctionner une colonne de distillation Pending EP4072697A1 (fr)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
EP19215603 2019-12-12
EP20210976 2020-12-01
PCT/EP2020/085198 WO2021116146A1 (fr) 2019-12-12 2020-12-09 Procédé pour faire fonctionner une colonne de distillation

Publications (1)

Publication Number Publication Date
EP4072697A1 true EP4072697A1 (fr) 2022-10-19

Family

ID=73698872

Family Applications (1)

Application Number Title Priority Date Filing Date
EP20819765.7A Pending EP4072697A1 (fr) 2019-12-12 2020-12-09 Procédé pour faire fonctionner une colonne de distillation

Country Status (5)

Country Link
US (1) US12076670B2 (fr)
EP (1) EP4072697A1 (fr)
JP (1) JP2023505683A (fr)
CN (1) CN114728211B (fr)
WO (1) WO2021116146A1 (fr)

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US11702381B1 (en) 2022-02-23 2023-07-18 Covestro Deutschland Ag Method for operating a rectification column
CN117180784B (zh) * 2023-11-06 2024-02-02 万华化学集团股份有限公司 进料分馏塔控制系统

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Also Published As

Publication number Publication date
CN114728211A (zh) 2022-07-08
WO2021116146A1 (fr) 2021-06-17
CN114728211B (zh) 2024-09-27
US12076670B2 (en) 2024-09-03
JP2023505683A (ja) 2023-02-10
US20230008804A1 (en) 2023-01-12

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