EP2173447A2 - Procédé de réglage et de refroidissement d'une colonne de distillation - Google Patents

Procédé de réglage et de refroidissement d'une colonne de distillation

Info

Publication number
EP2173447A2
EP2173447A2 EP08784744A EP08784744A EP2173447A2 EP 2173447 A2 EP2173447 A2 EP 2173447A2 EP 08784744 A EP08784744 A EP 08784744A EP 08784744 A EP08784744 A EP 08784744A EP 2173447 A2 EP2173447 A2 EP 2173447A2
Authority
EP
European Patent Office
Prior art keywords
column
pressure
temperature
product
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.)
Ceased
Application number
EP08784744A
Other languages
German (de)
English (en)
Inventor
Frank Bahr
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.)
Individual
Original Assignee
Individual
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
Priority claimed from DE102007033540A external-priority patent/DE102007033540A1/de
Priority claimed from DE102007038918A external-priority patent/DE102007038918A1/de
Priority claimed from DE200710038919 external-priority patent/DE102007038919A1/de
Application filed by Individual filed Critical Individual
Publication of EP2173447A2 publication Critical patent/EP2173447A2/fr
Ceased 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
    • B01D3/4238—Head-, side- and bottom stream

Definitions

  • the invention relates to a method for manual or automatic control of the composition or quality of one or more of the head, the bottom or a side draw of a distillation column with built-in heat exchanger removed products.
  • the process is used for heat recovery through surface heat exchange.
  • the negative pressure at the top of the distillation column may in the short term change in practice for various reasons, for. B. due to a fault in the top condenser, because of fluctuations in the performance of the vacuum pump or as a result of the change in the raw material composition in a change of Rohstoffliefe- tion, etc. In this case, the concentrations change at the top and on the optional side draw and the specified specifications of these products are no longer met.
  • the prior art is a rigid distillate mass control and a variable return control (setpoint here is the distillate decrease amount) or rigid return and variable distillate mass control (setpoint here is the return amount).
  • This control reacts only to the distillate attack at the top of the column and distributes the mass flows. Responding to the thermodynamically induced mass shifts is insufficient. Vacuum shifts resulting from vacuum changes lead to mass flow changes within the distillation columns. Without manual intervention, changes in concentration occur, which are represented by process analytics. The target concentration is reached again by manual driving parameter changes.
  • the prior art is also a sump temperature control.
  • control is thus carried out here as a function of the temperature difference of two at the top of the column at a distance from each other arranged thermometer, but not as a function of the pressure at the top of the column.
  • the reflux ratio is adjusted only in two coarse steps and not continuously.
  • Heat exchangers within the head of distillation columns for cooling are known in the art, e.g. German Offenlegungsschriften DE 34 16 519 A1, DE 34 36 021 A1, DE 35 05 590 A1 and DE 35 10 097 A1 (Linde AG 1984 to 1986).
  • the number of separation stages and the pressure loss per column height are usually dependent on the liquid and more of the steam load of the columns.
  • the "comparable air velocity” was introduced, taking into account the influence of vapor density on the pressure loss, as required by the Bernoulli equation, and is also more illustrative than the F-factor used in Anglo-Saxon literature.
  • the invention has for its object to achieve in the process of the type mentioned in a short-term change in the pressure in the top of a very fast settling of the column state of a stationary state to the new stationary state with a good quality of the top product as in the previous state ,
  • This object is achieved according to the invention in the method of the type mentioned in that the new boiling temperature of the product is determined at a pressure change in the column in the product removal at this pressure from the vapor pressure curve of the product and the temperature of the cooling medium flowing through the heat exchanger to adjust to this new boiling temperature.
  • the method is based on the fact that the components of the compositions to be distilled have certain boiling or condensation temperatures at given pressures corresponding to the vapor pressure curves. If the pressure in the column changes, the boiling point of the components of the mixture also changes.
  • steam / liquid heat exchangers are installed in the distillation column, in which the distillation vapors are cooled in the buoyancy phase and / or only in the condensation region and before the vapor tube by means of a cooling medium.
  • the condensation or boiling temperatures are calculated by a distillation control device based on the vapor pressure curve of the components and the cooling medium is adjusted to the condensation / boiling temperature at the predetermined pressure ratios.
  • the return takes place at this Method via a return manifold on the Kopikondensatoren and / or is injected into the vapor tubes of the buoyancy part.
  • the cooling medium falls below the condensation temperature of the distillate in the column inlet, this ensures the effective vapor condensation.
  • the temperature measurement for the distillation loop is at the first distillate decrease above the buoyancy part.
  • the measuring point regulates the coolant flow and thus adjusts the condensation point of the distillate.
  • the cooling medium flows through the buoyancy part in countercurrent, this ensures a temperature increase in the sump direction and thus for a thermal return.
  • the inventive method for manual or automatic control of the composition or quality of one or more of the head, the bottom or a side draw a distillation column with built-in heat exchanger removed products (s) is characterized in that in a change in pressure in the column in the range In the case of product removal, the new boiling temperature of the product at this pressure is determined from the vapor pressure curve of the product and the temperature is determined by changing the cooling medium flow rate to the new one
  • control is carried out by changing the withdrawal amount or the return in response to a thermodynamic state variable that is determined in a change in pressure in the column in the product removal the resulting temperature change from the vapor pressure curve of the product, the return and / or the distillate decrease temporarily changes until the temperature in the column in the region of the product removal has reached the new desired value determined by the vapor pressure curve, and then sets the return or the distillate decrease back to the original value.
  • the method is characterized in that when changing the raw material composition of the control loop adjusts the distillate decrease due to the resulting temperature shifts.
  • the temperature is additionally recorded at a location other than the product removal, and the measured values obtained are also used for regulation.
  • the distillation control can be better damped, since there concentration changes make earlier noticeable.
  • yield improvements can be achieved by setting the temperature value to a determined distillate concentration (calculated from the energy content of the mixture due to the different boiling points). However, it is not about the temperature difference of the two measuring points as in DE 1 059 410.
  • an overshoot or undershoot of the setpoint temperature determined by the vapor pressure curve of the product be detected by means of limit value detectors and an optical and / or acoustic signal emitted.
  • the distillate decrease is now throttled and the return increased. This lowers the temperature at the top of the column. If the temperature has then reached the new determined by the vapor pressure curve boiling point at the corresponding negative pressure, in particular the distillate decrease and the return are restored to the old value.
  • the product concentration at the top of the column and thus the purity of the product again have the same value or similar value as before the pressure change.
  • the newly set temperature is maintained despite the same reflux ratio and the same distillate decrease.
  • the reflux ratio changes significantly with vacuum changes and the subsequent interventions. However, it fits in stationary operation again approximately. An exact adaptation is possible only by changing the energy supply.
  • the pressure in a limited space area above the sump is thus substantially higher than in the remaining area of the column, so that significantly less high-boiling components evaporate out of the sump.
  • the desired amount of middle and low boilers only a slight increase in the bottom temperature is required, which does not affect the quality of the thermally sensitive oleochemicals.
  • the reduced height of the column reduces the investment required for the construction. In operating experiments it could be demonstrated that the energy requirement decreases by more than 20% when using the method according to the invention.
  • the pressure loss at the throttle element is greater than the total pressure loss of the other internals.
  • the pressure loss in the region of the throttle element is greater than the total pressure loss in the other regions of the column.
  • the feed is fed laterally between the throttle element and the head or the sump and that the feed temperature is higher than the boiling temperature of the heaviest component of the desired overhead product at a pressure corresponding to the pressure in the feed inlet of the column and lower than the boiling temperature of is the lightest boiling component of the desired bottoms product at a pressure corresponding to the pressure in the sump region.
  • the bottom temperature be lower than the boiling point of the lightest boiling component of the desired bottom product, measured above the throttle element taking into account the pressure prevailing there, and higher than the boiling temperature of the heaviest component of the desired top product, each at a pressure corresponding to Pressure in the sump area is.
  • the intended bottom temperature is selected so that the components of the desired bottom product only to a very small part or not at all flow through the throttle element and the liquid accumulated thereon gas upwards and thus overcome.
  • the height of the column is chosen or reduced so that the top product within the column remains gaseous / vaporous and does not condense within the column.
  • the inventive method is applicable to all distillable homogeneous liquid mixtures whose boiling points spread by> 10 ° C, applicable.
  • Examples of such mixtures are z.
  • fatty acids methyl esters, hydrocarbons, vegetable oils, benzenes, alcohols, glycerol, petrochemical raw materials and the derivatives of the aforementioned substance groups, but also inorganic chemicals and seawater and other aqueous solutions.
  • Figure 1 is a schematic representation of a first embodiment of a
  • FIG. 2 shows a flow diagram of a distillation plant with the inventive control circuit with return according to a second exemplary embodiment
  • FIG. 3 is a flow chart corresponding to FIG. 2, but with a control loop according to the invention without return,
  • Figure 4 is a flow diagram of a system for carrying out the inventive
  • Figure 5 is a flow diagram of a system with which the inventive experiment described below has been moved to the third embodiment
  • Figure 6 shows the structure of columns Kl and K2 in Figure 5 in a schematic
  • a distillation column 1 with a heat exchanger 2 in this case, a jacket heat exchanger (sheathed pipes), filled with fine tissue packings in the vapor tubes.
  • a jacket heat exchanger sheathed pipes
  • shell and tube heat exchangers can be used in flat design, the vapors flow past the cooling coils.
  • a post-condenser 3 connected to a vacuum unit 4 and the cooling medium inlet 5 and thedemedium- outlet 6 for the heat exchanger 2 are also shown the inlet 7 for the raw material, the steam inlet 8 for the sump heater and the Condensate outlet 9 for this sump heater and the distillate return 10, the distillate is returned to the bottom, and the distillate 11.
  • the steam supply for the sump heater is locked against bottom overheating, wherein the control device 12 of the invention calculates the bottom temperature, which a Destillatgehaltinate in the sump guaranteed.
  • a further control device 13 for the head region of the column is likewise shown in FIG. 1, which regulates the coolant flow rate via the calculated boiling temperature of the distillate and thus sets the condensation point of the distillate.
  • the bottom Via the line 16, the bottom can be passed to a subsequent distillation column, which is not shown here.
  • the copy capacitors 17 and 18 are shown. Of the Return is applied via the return line 19 via the return cooler 20 to the return manifold 21 and 22.
  • the column works as follows: The distillate condenses on the head of the buoyant cooler 2 and on the top condensers 17 and 18 and flows off. At a temperature deviation, the distillate z. B. are returned to the column via a three-way valve 14 or passed into the raw material tank not shown. The feedstock is controlled by the bottom of this column. The bottom transfer of this column to a subsequent column is in turn controlled by the control device 12, which also works on the basis of the vapor pressure curves to ensure that no low boilers are in the bottom medium, which must be distilled off in the present column. To prevent overheating of the sump medium, the supply of the heating medium, in this case steam, should also have a temperature control. Alternatively, of course, the conventional procedure with constant feed quantity and level-controlled bottom discharge of the column is possible.
  • the last distillation column may be conventionally constructed with a low differential pressure, since this column serves to achieve the highest possible yield, but this would not be useful for the distillation of propanediol for energetic reasons.
  • cooling medium for the heat exchangers 18, 17 and 2 can serve a variety of liquids, gases or molten salts.
  • the feedstock and / or feedwater is used as the cooling medium.
  • Molten salts molten salt
  • shell and tube heat exchangers As a heat exchanger, shell and tube heat exchangers, shell heat exchangers and mesh heat exchangers, etc. can be used.
  • spiral heat exchangers or tube bundle heat exchangers in which the distillate vapors flow past and condense on the cooling tubes in countercurrent, can be used for the top condensation.
  • FIG. 2 shows a distillation column 101, in which the overhead product is withdrawn via a line 102 and, after condensation in the condenser 103, is passed via a line 104 to the distillate receiver 105.
  • a distillate pump 106 delivers the distillate via a valve 107 and a flow measurement 122 to the product outlet.
  • the distillate which has not been removed flows back into the column 101 via a reflux line 108 and a valve 109 controlled by the liquid level in the distillate receiver 105 at its head.
  • a vacuum unit 110 which is connected via a valve 111 to the top condenser 103, provides for the negative pressure in the condenser 103 and in the top of the column 101.
  • the valve 111 is controlled by the pressure at the top of the column.
  • a ratio control is now carried out with a control device 112 which controls or regulates temperature and pressure in accordance with the boiling point specifications from the vapor pressure curves.
  • This is a so-called ratio regulation.
  • the control is based on the ratio of boiling point shifts analogous to the pressure change.
  • the control device 112. calculates a control value for the valve 107 based on the vapor pressure curves, which controls the amount of distillate removal and thus indirectly also the return and thus the reflux ratio.
  • the valve 109 which is controlled by the liquid level in the distillate receiver 105, serves only to maintain a certain level of liquid in the distillate receiver which must never be pumped empty.
  • a condenser 116 is additionally provided at the top of the column 101.
  • the column is designed for a liquid distillate decrease.
  • the vapor vapors precipitate on the condenser 116 and flow directly back into the column.
  • the vapor which has not yet condensed there passes via the line 117 to the further condenser 118, which is connected to the vacuum unit 110.
  • the condensate from the condenser 118 is returned to the feed tank or a collection tank. This means the feed tank from which the raw material is fed into the column.
  • the measured values of a temperature measuring point 119 and a pressure measuring point 120 at the top of the column 101 are offset by the control device 112 taking into account the vapor pressure curves of the components of the mixture to be processed to a manipulated variable with which the valve 121 is controlled.
  • the valve 121 determines the size of the distillate decrease.
  • the flow meter 122 detects the instantaneous distillate stream.
  • test results are presented on the basis of tables, wherein the tests have been carried out with a system according to FIG. 2.
  • the negative pressure was evenly increased from 30 mbar to 50 mbar for testing the process according to the invention, ie the vacuum worsened.
  • the distillate decrease was increased by up to 750 kg / h.
  • the temperature increased by about 0.5 degrees Celsius per 1 mbar pressure change.
  • the distillate decrease was reduced again by 1800 kg / h. This was necessary because the distillate decrease had been increased a little too much, so that the regulation was overdriven.
  • the distillate removal was returned to the old value of 4400 kg / h, and the desired concentration of C8 fatty alcohol at the top was again about 99%.
  • the temperature then remained at the elevated level of 114 ° C.
  • the negative pressure was reduced from 65 mbar to 30 mbar, thus significantly improving the vacuum.
  • the distillate decrease was set to zero, so the reflux ratio increased to 100%.
  • the distillate decrease was again gradually increased to the desired value of 4600 kg / h and it was again the desired target concentration of about 99% C8 fatty alcohol on the head and a desired desired concentration of about 95% C10 fatty alcohol on the side offtake.
  • the temperature had settled after this transitional time to 105 ° C. The entire transition took only about half an hour.
  • control according to the invention is also applicable for controlling the sump temperature or the reflux ratio resulting from the power supply changes.
  • control concept according to the invention has the following advantages: A self-controlling distillation plant is possible. A quality improvement of the head distillate by a direct reaction of the control to pressure and temperature changes in the
  • the rule principle has a balancing effect on changes in the raw material composition.
  • An online analysis can then be dispensed with.
  • Visual or acoustic monitoring can be carried out via limit detectors when the calculated boiling or condensation temperatures are exceeded or fallen short of.
  • FIG. 4 shows the flow chart of a possible installation for carrying out the method according to the invention in accordance with a third exemplary embodiment.
  • the column Kl contains packages 201, 202, 203 which, in the usual mode of operation of the column, cause a pressure drop of 8 mbar for all three packages.
  • a fatty alcohol mixture with C chain lengths C6-Cl 8 is worked up by distillation.
  • the feed is fed via a feeder heater 204 laterally into the column Kl ( Figure 4).
  • the top product consisting of a fatty alcohol mixture with chain lengths of C6 - ClO, is withdrawn via a cooler 205 and a distillate template 206 by means of a pump 207.
  • a sump heater 208 and a pump 209 are also shown, with which the sump is pumped off and either returned via the sump heater 208 or fed via the line 210 into the bottom region of the column K2 (see FIG. 5).
  • a throttle element 212 is now arranged between the sump 211 and the lowermost packing 203, which causes a greater pressure loss than the total pressure loss of the packs 201, 202, 203.
  • This throttle element may be designed differently in terms of apparatus. It may, for example, be a bubble tray, sieve bottom or a packing according to the prior art, but which is modified according to the invention so that this bottom or this packing causes the desired pressure loss. Due to the throttle element 212, the pressure above the sump 211 is 220 mbar, although directly above the throttle element 212, a pressure of only 105 mbar is observed.
  • the installation position of the throttle element is dependent on the distillate load of the column, in Figure 4, the mounting position is selected for a low distillate content.
  • FIG. 6 shows details of the columns K1 and K2 in FIG. 5.
  • Columns Kl and K2 contain 14 trays numbered from top to bottom.
  • the 1st to 4th floor is a sieve bottom.
  • the 5th to 14th floor is designed as a bubble tray.
  • the quality of the fatty alcohol products obtained was about the same as before the installation of the throttle element, the term "quality" to understand the purity and the absence of unwanted components.

Landscapes

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

Abstract

L'invention concerne un procédé de réglage manuel ou automatique de la composition ou de la qualité d'un ou de plusieurs produits soutirés en tête, en queue ou en un point de soutirage latéral d'une colonne de distillation (1) à échangeur thermique (2, 17, 18) intégré. Le procédé se caractérise en ce que, lorsque la pression régnant à l'intérieur de la colonne (1) dans la zone de soutirage du (des) produit(s) varie, la nouvelle température d'ébullition du produit à cette pression est déterminée à partir de la courbe de pression de vapeur du produit et la température du distillat soutiré est réglée sur cette nouvelle température d'ébullition par modification du débit du fluide de refroidissement s'écoulant à travers l'échangeur thermique (2, 17, 18), de préférence à contre-courant.
EP08784744A 2007-07-19 2008-07-12 Procédé de réglage et de refroidissement d'une colonne de distillation Ceased EP2173447A2 (fr)

Applications Claiming Priority (4)

Application Number Priority Date Filing Date Title
DE102007033540A DE102007033540A1 (de) 2007-07-19 2007-07-19 Verfahren zum Regeln einer Destillationskolonne
DE102007038918A DE102007038918A1 (de) 2007-08-17 2007-08-17 Verfahren zum Regeln und Kühlen einer Destillationskolonne (II)
DE200710038919 DE102007038919A1 (de) 2007-08-17 2007-08-17 Verfahren zum Destillieren/Rektifizieren von oleochemischen Stoffgemischen
PCT/EP2008/005713 WO2009010250A2 (fr) 2007-07-19 2008-07-12 Procédé de réglage et de refroidissement d'une colonne de distillation

Publications (1)

Publication Number Publication Date
EP2173447A2 true EP2173447A2 (fr) 2010-04-14

Family

ID=40260124

Family Applications (1)

Application Number Title Priority Date Filing Date
EP08784744A Ceased EP2173447A2 (fr) 2007-07-19 2008-07-12 Procédé de réglage et de refroidissement d'une colonne de distillation

Country Status (5)

Country Link
US (1) US8419903B2 (fr)
EP (1) EP2173447A2 (fr)
JP (1) JP2010533578A (fr)
CN (1) CN101754788A (fr)
WO (1) WO2009010250A2 (fr)

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Also Published As

Publication number Publication date
WO2009010250A3 (fr) 2009-04-23
CN101754788A (zh) 2010-06-23
US8419903B2 (en) 2013-04-16
WO2009010250A2 (fr) 2009-01-22
JP2010533578A (ja) 2010-10-28
WO2009010250A4 (fr) 2009-06-11
US20100181184A1 (en) 2010-07-22

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