CN107365242A - A kind of dynamic control scheme of heterogeneous separation of extractive distillation methanol toluene water - Google Patents

A kind of dynamic control scheme of heterogeneous separation of extractive distillation methanol toluene water Download PDF

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Publication number
CN107365242A
CN107365242A CN201710683265.XA CN201710683265A CN107365242A CN 107365242 A CN107365242 A CN 107365242A CN 201710683265 A CN201710683265 A CN 201710683265A CN 107365242 A CN107365242 A CN 107365242A
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China
Prior art keywords
tower
rectifying column
toluene
methanol
controller
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Pending
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CN201710683265.XA
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Chinese (zh)
Inventor
朱兆友
张霞
亓鹏超
戴姚
王英龙
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Qingdao University of Science and Technology
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Qingdao University of Science and Technology
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Priority to CN201710683265.XA priority Critical patent/CN107365242A/en
Publication of CN107365242A publication Critical patent/CN107365242A/en
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    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C7/00Purification; Separation; Use of additives
    • C07C7/04Purification; Separation; Use of additives by distillation
    • C07C7/05Purification; Separation; Use of additives by distillation with the aid of auxiliary compounds
    • C07C7/08Purification; Separation; Use of additives by distillation with the aid of auxiliary compounds by extractive distillation
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D3/00Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
    • B01D3/34Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping with one or more auxiliary substances
    • B01D3/40Extractive distillation
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D3/00Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
    • B01D3/42Regulation; Control
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D3/00Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
    • B01D3/42Regulation; Control
    • B01D3/4211Regulation; Control of columns
    • B01D3/4294Feed stream
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C29/00Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
    • C07C29/74Separation; Purification; Use of additives, e.g. for stabilisation
    • C07C29/76Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
    • C07C29/80Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by distillation
    • C07C29/84Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by distillation by extractive distillation

Abstract

The present invention relates to a kind of dynamic control scheme of heterogeneous separation of extractive distillation methanol toluene water, including:Flow controller, for adjusting feed flow rates;Fluid level controller, it is respectively used to adjust the liquid level of return tank of top of the tower, the liquid level of tower reactor and the liquid level of phase-splitter;Pressure controller, it is respectively used to adjust rectifying tower pressure and the tower pressure of extractant recovery tower;Temperature controller, it is respectively used to adjust the tower temperature of extractant recovery tower and the temperature of heat exchanger;Reflux ratio adjustment structure, it is respectively used to adjust the capacity of returns of rectifying column and the capacity of returns of extractant recovery tower.The present invention realizes to be automatically controlled to rectifying column temperature, pressure and flow, it is ensured that the high-purity quiet run of three kinds of product methanol, toluene and water, and there is good dynamic control effect.The equipment requirement that the present invention uses is low, easily realizes, and the present invention has low cost, and low energy consumption, product purity is high, the advantages that high income.

Description

A kind of dynamic control scheme of heterogeneous separation of extractive distillation methanol-toluene-water
【Technical field】
The present invention relates to the automation control area of chemical field, more particularly to Chemical Manufacture.
【Background technology】
It is dynamically control on exploitation and performance evaluation, the simulation of driving and parking process, the process working condition calibration of process control system Etc. be used widely.For rectifying separation process, common is exactly the purity for controlling product, therefore for distillation process The research of control technique have great importance.
Two towers circulation logistics is connected in distillation process, during by rectifying to be constrained, and height is produced in distillation process Coupling, there is disturbance in a tower and be transmitted as readily to another tower, cause to be formed between Liang Ta certain mutual Effect, this interaction inevitably cause control problem.At present for ternary system separation dynamic control research very It is few, the introducing as the 4th component extracting agent so that the control difficulty for flow greatly increases, therefore present invention is generally directed to The steady-state flow of heterogeneous separation of extractive distillation methanol-toluene-water proposes a kind of effective control program, ensures three kinds of product first The high-purity quiet run of alcohol, toluene and water.
Patent (CN106431812A) discloses a kind of method and dress of separation of extractive distillation toluene-methanol-water azeotropic mixture Put, this method by Liang Ta and phase-splitter separation of tertiary system methanol-toluene-water, obtain high purity methanol, toluene and Water, but this patent is not carried out dynamic control.
Patent (CN106110700A) discloses a kind of Rectification Tower Control System, by introducing pressure regulating mechanism, heating Mechanism, backflow mechanism automatically control to realize to rectifying column temperature and pressure.But this patent is to realize the control to single column System, the INTERACTION PROBLEMS not being related between two towers, also being probed into without progress multicomponent for what control influenceed.
Patent (CN106916050A) discloses a kind of piece-rate system and its application method for low carbon mixed alcohol, is applicable In the dehydration of low carbon mixed alcohol, the patent gives the single column Dynamic Control Strategy of single tower distillation separation, compared to this patent Double column pressure swing controls, and the variable that single column control needs control is few and simple, and control difficulty is less than this patent.
Patent (CN201006332Y) and patent (CN106110700A) disclose a kind of Rectification Tower Control System, the control System is only capable of realizing single column control, and does not provide the specific separate substance classification of rectifying column, the double column pressure swing rectifying with the application Dynamic control difficulty is wanted to go to very remote.
【The content of the invention】
【Technical problems to be solved】
Solve the problems, such as it is overcome the deficiencies in the prior art, a kind of heterogeneous separation of extractive distillation methanol-toluene of proposition- The dynamic control scheme of water, the patent of the present invention problem in science to be solved are as follows:
It is an object of the invention to provide a kind of dynamic control suitable for heterogeneous separation of extractive distillation ternary mixture technique Scheme processed.
It is a further object of the present invention to provide the control program to separate the application of methanol-toluene-aqueous systems.
【Technical scheme】
The present invention ensures three kinds using a kind of dynamic control scheme of heterogeneous separation of extractive distillation methanol-toluene-water The high-purity quiet run of product methanol, toluene and water, is mainly included the following steps that:
(1) steady state process:Methanol-toluene-aqueous mixtures are sent into rectifying column T1, the condensed device C1 of overhead vapours is condensed, Partial material passes back into rectifying column T1, and partial material produces as methanol product, and bottom of towe partial material enters reboiler R1, then boils Enter rectifying column T1 afterwards, another part material enters extractant recovery tower T2;Extractant recovery tower T2 bottom of towe partial material enters Tower bottom reboiler R2, then enter extractant recovery tower T2 after boiling, another part material returns to rectifying column T1 and recycled, and tower top steams Vapour condensed device C2 condensations, partial material pass back into extractant recovery tower T2, partial material after heat exchanger H coolings, into point Phase device DEC, upper strata directly produce product toluene, and lower floor directly produces product water.
(2) dynamic control scheme:Rectifying column T1 inlet amounies are controlled by flow controller FC, extractant recovery tower T2 circulations Circulation logistics flux to rectifying column T1 is based on proportional controller S/F by circulating logistics flow controller FC2 controls, the stream Amount controller FC and FC2 are Reverse Turning Control;Rectifying column T1 and extractant recovery tower T2 tower top pressure are cold by corresponding tower top The removal speed control of condenser thermic load, pressure controller PC1, PC2 are Reverse Turning Control;Rectifying column T1 and extractant recovery tower T2 The liquid level of return tank controlled by adjusting the produced quantity of tower top, return tank fluid level controller LC11, LC21 control to be positive;Essence The tower reactor liquid level for evaporating tower T1 is controlled by adjusting bottom of towe produced quantity, and extractant recovery tower T2 tower reactor liquid level is by adjusting extractant Recovery tower T2 is recycled to rectifying column T1 circulation logistics flux control, and tower reactor fluid level controller LC12, LC22 control to be positive;It is logical Cross proportional controller RR1, RR2 control rectifying column T1 capacity of returns and extractant recovery tower T2 capacity of returns;Pass through temperature control Device TC1, TC2 are respectively used to adjust extractant recovery tower T2 tower temperature and heat exchanger H temperature.
In accordance with another preferred embodiment of the present invention, it is characterised in that:Rectifying column (T1) tower reactor adoption rate controller B1/QR1, based on rectifying column T1 bottom of towe flow rates B1 adjust reboiler R1 thermic load output quantity QR1 so as to ensureing rectifying column (T1) The purity of overhead extraction product.
In accordance with another preferred embodiment of the present invention, it is characterised in that:The purity of methanol maintains more than 99.9%, toluene Purity maintain more than 99.8%, the purity of water maintains more than 99.9%.
【Beneficial effect】
The present invention compared with prior art, mainly there is following beneficial effect:
(1) the high-purity quiet run of three kinds of product methanol, toluene and water is ensured using simple control structure.
(2) this control technique can solve the disturbance of feed flow rates and feed composition well.
(3) equipment requirement used is low, easily realizes.
(4) present invention has low cost, and low energy consumption, product purity is high, the advantages that high income.
【Brief description of the drawings】
Accompanying drawing 1 is a kind of structural representation of the dynamic control scheme of heterogeneous separation of extractive distillation methanol-toluene-water. In figure, rectifying column T1, extractant recovery tower T2, phase-splitter DEC, return tank D1, return tank D2, reboiler R1, reboiler R2, change Hot device H, condenser C1, condenser C2, valve V1-V11, pump P1-P4;Feed flow controller FC is used to adjust entering for rectifying column T1 Stream rate Feed;Fluid level controller LC is respectively used to adjust the liquid level of return tank of top of the tower, the liquid level of tower reactor and the liquid of phase-splitter Position;Pressure controller PC is respectively used to adjust rectifying column T1 towers pressure and extractant recovery tower T2 tower pressure;Temperature controller TC Being respectively used to adjust extractant recovery tower T2 tower temperature, (temperature sensitive plate is that the 31st block of column plate is used to represent extractant recovery tower T2 Tower temperature) and heat exchanger H temperature;Composition control device CC, for adjusting the purity of product methanol;Proportional controller RR distinguishes For adjusting rectifying column T1 overhead reflux amount and the capacity of returns of extractant recovery tower T2 tower tops;Proportional controller QR1/B1 is based on Rectifying column T1 bottom of towe flow rates B1 adjustment reboilers R1 thermic load output quantity QR1;Proportional controller S/F is entered based on rectifying column T1's Stream rate F regulation extractant 1-METHYLPYRROLIDONEs NMP flow rate S;△ T are the dead time;Solid line with the arrow represents each logistics Pipeline, dotted line with the arrow represent input or the output signal of controller.
Accompanying drawing 2 is that (feed flow rates are changed into 120kmol/h or feed flow rates from 100kmol/h for feed flow rates change ± 20% 80kmol/h is changed into from 100kmol/h) dynamic response figure.
Accompanying drawing 3 be feed composition change ± 20% (methanol from 49% be changed into 58.8% or methanol be changed into 39.2% from 49%) Dynamic response figure.
【Embodiment】
Further illustrated below in conjunction with accompanying drawing 1, not limit scope involved in the present invention.
Steady state process flow:Feed flow rates 100kmol/h, 25 DEG C, pressure 1atm of temperature, molal weight composition:Methanol 49%, toluene 37%, water 14%;Extractant 90kmol/h;51 pieces of rectifying column (T1) number of theoretical plate, material liquid are drawn by the 26th block of plate Enter, recycle feed position is the 4th block of plate, operating pressure 1atm;Extractant recovery tower (T2) number of theoretical plate is 31 pieces, rectifying column (T1) bottom of towe Produced Liquid is introduced by the 7th block of plate, operating pressure 1atm, and under this process conditions, the purity of methanol can reach More than 99.9%, the purity of toluene can reach more than 99.8%, and the purity of water reaches more than 99.9%.
Embodiment 1:
Each controller automatically enters setting value, and determine scope by median of setting value after initialization is run, with closing Loop back path does method of testing.Feed flow rates are changed into 120kmol/h from 100kmol/h, and its dynamic response figure such as Fig. 2 (solid line) is aobvious Show, methanol returns to Reinheitszahl 99.9% after 6h fluctuation;The purity of water has almost no change, and maintains 99.9% always; Toluene returns to Reinheitszahl 99.8% after 2.5h fluctuation;The tower temperature of extractant recovery tower (T2) returns to after 3h is fluctuated Initial value, illustrate that the control technique can handle the disturbance of+20% feed flow rates well.
Embodiment 2:
Each controller automatically enters setting value, and determine scope by median of setting value after initialization is run, with closing Loop back path does method of testing.Feed flow rates are changed into 80kmol/h from 100kmol/h, its dynamic response figure such as Fig. 2 (dotted line) displays, Methanol returns to Reinheitszahl 99.9% after 6h fluctuation;The purity of water has almost no change, and maintains 99.9% always;First Benzene returns to Reinheitszahl 99.8% after 2.5h fluctuation;The tower temperature of extractant recovery tower (T2) returns to most after 3h is fluctuated First value, illustrate that the control technique can handle the disturbance of -20% feed flow rates well.
Embodiment 3:
Each controller automatically enters setting value, and determine scope by median of setting value after initialization is run, with closing Loop back path does method of testing.Feed composition is by methanol 49%, toluene 37%, and water 14% is changed into methanol 58.8%, toluene 29.9%, Water 11.3%, its dynamic response figure such as Fig. 3 (solid line) displays, methanol return to Reinheitszahl 99.9% after 2h fluctuation;Water Purity has almost no change, and maintains 1 or so always;Toluene returns to Reinheitszahl 99.8% after 2h fluctuation;Extractant returns The tower temperature for receiving tower (T2) returns to initial value after 3h is fluctuated, and illustrates that the control technique can handle+20% charging well The disturbance of composition.
Embodiment 4:
Each controller automatically enters setting value, and determine scope by median of setting value after initialization is run, with closing Loop back path does method of testing.Feed composition is by methanol 49%, toluene 37%, and water 14% is changed into methanol 39.2%, toluene 44.1%, Water 16.7%, its dynamic response figure such as Fig. 3 (dotted line) displays, methanol return to Reinheitszahl 99.9% after 8h fluctuation;Water Purity has almost no change, and maintains 1 or so always;Toluene returns to Reinheitszahl 99.8% after 3h fluctuation;Extractant returns The tower temperature for receiving tower (T2) returns to initial value after 3h is fluctuated, and illustrates that the control technique can handle -20% charging well The disturbance of composition.

Claims (5)

  1. A kind of 1. dynamic control scheme of heterogeneous separation of extractive distillation methanol-toluene-water, it is characterised in that the separation first The technique that the steady state process of alcohol-toluene-water ternary mixture is separated for two-tower rectification combination phase-splitter, the separation first The dynamic control scheme of alcohol-toluene-water ternary mixture is the dynamic control of two-tower rectification combination phase-splitter separating technology design Scheme.
  2. It is 2. as claimed in claim 1, it is characterised in that the steady state process of separation methanol-toluene-water ternary mixture is as follows:
    Methanol-toluene-aqueous mixtures are sent into rectifying column T1, the condensed device C1 condensations of overhead vapours, partial material passes back into essence Tower T1 is evaporated, partial material produces as methanol product, and bottom of towe partial material enters reboiler R1, then enters rectifying column T1 after boiling, Another part material enters extractant recovery tower T2;Extractant recovery tower T2 bottom of towe partial material enters tower bottom reboiler R2, then Enter extractant recovery tower T2 after boiling, another part material returns to rectifying column T1 and recycled, and the condensed device C2 of overhead vapours is cold Solidifying, partial material passes back into extractant recovery tower T2, and partial material is straight into phase-splitter DEC, upper strata after heat exchanger H coolings Extraction product toluene is connect, lower floor directly produces product water.
  3. It is 3. as claimed in claim 1, it is characterised in that the dynamic control of control separation methanol-toluene-water ternary mixture flow Scheme is as follows:
    Feed flow controller FC is used for the feed flow rates for adjusting rectifying column T1;Fluid level controller LC is respectively used to adjust tower top time Flow the liquid level of tank, the liquid level of tower reactor and the liquid level of phase-splitter;Pressure controller PC be respectively used to adjust rectifying column T1 towers pressure with And extractant recovery tower T2 tower pressure;Temperature controller TC is respectively used to adjust extractant recovery tower T2 tower temperature and heat exchanger H temperature;Composition control device CC, for adjusting the purity of product methanol;Proportional controller RR is respectively used to adjust rectifying column T1 Overhead reflux amount and extractant recovery tower T2 tower tops capacity of returns;Proportional controller QR1/B1 is based on rectifying column T1 bottom of towe flow rates B1 adjustment reboilers R1 thermic load output quantity QR1;Feed flow rates F regulation extractions of the proportional controller S/F based on rectifying column T1 Agent 1-METHYLPYRROLIDONE NMP flow rate S.
  4. 4. according to claim 1-3, it is characterised in that:Rectifying column (T1) tower reactor adoption rate controller B1/QR1, is based on Rectifying column T1 bottom of towe flow rates B1 regulation reboilers R1 thermic load output quantity QR1;Rectifying column T1 tower tops use composition control device CC Control the purity of product methanol;Adoption rate controller S/F, the feed flow rates F regulation extractant N- methyl based on rectifying column T1 Pyrrolidones NMP flow rate S.
  5. 5. according to claim 1-3, it is characterised in that:The control technique can be sane control 20% within enter stream Feed composition disturbance within amount disturbance and 20%, the purity of methanol, toluene and water is more than 99.80% after separation.
CN201710683265.XA 2017-08-11 2017-08-11 A kind of dynamic control scheme of heterogeneous separation of extractive distillation methanol toluene water Pending CN107365242A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109678677A (en) * 2019-01-03 2019-04-26 青岛科技大学 A kind of liquid-liquid extraction-rectifying separating propylene glycol methyl ether and water dynamic control scheme
CN109704928A (en) * 2019-01-03 2019-05-03 青岛科技大学 A kind of heterogeneous liquid-liquid extraction-rectifying separating propylene glycol methyl ether and water dynamic control scheme
CN109745723A (en) * 2018-12-29 2019-05-14 恒天纤维集团有限公司 A kind of double tower continuous feeding distillation system and control method
CN109776285A (en) * 2019-01-03 2019-05-21 青岛科技大学 A kind of dynamic control scheme of mixed extractant separating propylene glycol methyl ether-water

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CN106431812A (en) * 2016-09-21 2017-02-22 青岛科技大学 Method and device for separating methylbenzene-methanol-water azeotrope using extractive distillation
CN106916050A (en) * 2017-04-27 2017-07-04 太原理工大学 For the piece-rate system and its application method of MAS

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109745723A (en) * 2018-12-29 2019-05-14 恒天纤维集团有限公司 A kind of double tower continuous feeding distillation system and control method
CN109745723B (en) * 2018-12-29 2021-07-06 恒天纤维集团有限公司 Double-tower continuous feed rectification system and control method
CN109678677A (en) * 2019-01-03 2019-04-26 青岛科技大学 A kind of liquid-liquid extraction-rectifying separating propylene glycol methyl ether and water dynamic control scheme
CN109704928A (en) * 2019-01-03 2019-05-03 青岛科技大学 A kind of heterogeneous liquid-liquid extraction-rectifying separating propylene glycol methyl ether and water dynamic control scheme
CN109776285A (en) * 2019-01-03 2019-05-21 青岛科技大学 A kind of dynamic control scheme of mixed extractant separating propylene glycol methyl ether-water

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