CN104151137A - High pressure and normal pressure double-tower rectification method used for separating n-butanol and MIBK azeotrope - Google Patents

High pressure and normal pressure double-tower rectification method used for separating n-butanol and MIBK azeotrope Download PDF

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Publication number
CN104151137A
CN104151137A CN201410388310.5A CN201410388310A CN104151137A CN 104151137 A CN104151137 A CN 104151137A CN 201410388310 A CN201410388310 A CN 201410388310A CN 104151137 A CN104151137 A CN 104151137A
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tower
mibk
propyl carbinol
pressurizing
atmospheric
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CN201410388310.5A
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CN104151137B (en
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朱兆友
王万玲
马艺心
朱峰
王丽丽
彭涛
张�焕
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HONGZE COUNTY HENGTAIKE INDUSTRY AND TRADE Co Ltd
Qingdao University of Science and Technology
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HONGZE COUNTY HENGTAIKE INDUSTRY AND TRADE Co Ltd
Qingdao University of Science and Technology
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    • 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
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C45/00Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds
    • C07C45/78Separation; Purification; Stabilisation; Use of additives
    • C07C45/81Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation
    • C07C45/82Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation by distillation

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

Abstract

The invention relates to a high pressure and normal pressure double-tower rectification device used for separating n-butanol and MIBK azeotrope. The device mainly comprises a high pressure tower HT, a normal pressure tower LT, a pressure pump P1, a pressure pump P2, a return tank A1, a return tank A2, a heat exchanger and the like; a rectification separation method comprises the following steps: a material is conveyed to the high pressure tower HT through the P1; part of the material at the bottom of the HT tower enters the HT after entering a reboiler R1, and the other part of the material at the bottom of the HT tower is recovered as an MIBK product; part of vapor at the top of the HT tower flows back to the HT, and the other part of the vapor at the top of the HT tower is conveyed to the LT, after being condensed through a condenser C1 and collected through the return tank A1; part of the vapor at the top of the LT tower flows back to the LT, and the other part of the vapor at the top of the LT tower is conveyed to the HT through the P2, after being condensed through a condenser C2 and collected through the return tank A2; part of the material at the bottom of the LT tower enters a reboiler R2 and then enters the LT, and the other part of the material at the bottom of the LT tower is recovered as an n-butanol product. Through the adoption of the method, the cost of separating the n-butanol and the MIBK is reduced, the purity and the yield of the product are improved, the technology is simple and the device is reasonable.

Description

The method of the separated propyl carbinol of high pressure normal pressure two-tower rectification and MIBK azeotropic system
Technical field
The invention belongs to chemical separating purifying field, relate to the separated of a kind of propyl carbinol and mibk (MIBK) azeotrope system, particularly the double tower tripping device of a kind of first high-pressure tower rectifying, atmospheric tower rectifying again and use this to install the method for separated propyl carbinol and MIBK azeotropic system.
Background technology
Propyl carbinol, MIBK are important Chemicals.The two all has outstanding application at chemical industry and pharmaceutical industries, is important organic synthesis auxiliary agent and organic solvent.In industrial production, recycle propyl carbinol and MIBK, this extremely has economic implications for enterprise.
Owing to there is azeotropic point in propyl carbinol and MIBK two-component system, therefore be difficult to obtain by conventional distillation method propyl carbinol and the MIBK of higher degree.Conventional separation method is mainly azeotropic distillation and extracting rectifying at present.
Document (research of methyl isobutyl ketone synthetic fluid heterogeneous azeotropic rectification separating technology. modern chemical industry, 2007.11, the 27th the 2nd phase of volume) provide a kind of heterogeneous azeotropic rectification separation method, adopt the method for heterogeneous azeotropic rectification to carry out propyl carbinol and mibk binary azeotropic system separated, the mibk that to have obtained purity be 99.5%.
Document (research of Virahol One-step production methyl iso-butyl ketone (MIBK) sepn process. chemical industry progress, 2005.12, the 24th the 5th phase of volume) reported that it is feasible that spent glycol carrys out the method for separation of extractive distillation propyl carbinol and mibk binary azeotropic system as extraction agent, gained mibk product purity is 99.5%, and yield is 91.7%.
The defect and the deficiency that in above-mentioned existing isolation technique, exist are: the cost compare of sepn process is high; In system, introducing other materials has increased separation costs, and has affected quality product to a certain extent; Technical process is complicated, and has brought this problem of new extractant regeneration.
The present invention adopts first high-pressure tower rectifying, the method for atmospheric tower rectification and purification again, specifically, the present invention utilizes the azeotropic composition of propyl carbinol and MIBK to occur this characteristic of larger variation with pressure change, first adopt compression rectification tower, adopt again atmospheric distillation tower, separated propyl carbinol and MIBK azeotropic system, method of the present invention is especially applicable to MIBK composition and accounts for more than 50% propyl carbinol and MIBK azeotropic system.In system of the present invention, do not introduce other components, in the time of cost-saving, guaranteed again the quality of product; Technique is simple, and device rationally; Can make highly purified propyl carbinol, MIBK product simultaneously.
Summary of the invention
[technical problem that will solve]
The object of this invention is to provide a kind of by the propyl carbinol high pressure normal pressure two-tower rectification tripping device separated with mibk (MIBK) azeotrope system.
Another object of the present invention is to provide the method for using the separated propyl carbinol of described device and MIBK azeotrope system.
Another object of the present invention is to provide the purposes of described device in separated propyl carbinol and MIBK azeotrope system.
[technical scheme]
The present invention overcomes shortcoming in prior art, has proposed a kind of first high-pressure tower rectifying, the method for atmospheric tower rectifying separation propyl carbinol and MIBK azeotropic system again.There is this characteristic of larger variation in the change that the present invention utilizes the azeotropic of propyl carbinol and MIBK to form with pressure, adopts the method for two tower pressure reduction rectifying, realizes the effective separation of the two.The method has solved the problems that current employing extracting rectifying or the separated propyl carbinol of azeotropic distillation and MIBK exist, and avoids introducing impurity, reduces separation costs, has improved product purity.
The invention provides a kind of technique simple, be easy to the high pressure normal pressure double tower tripping device realized, and use this to fill separated MIBK to account for more than 50% propyl carbinol and the method for MIBK azeotropic system.
The present invention is achieved through the following technical solutions: the device of the separated propyl carbinol of a kind of high pressure normal pressure two-tower rectification and MIBK azeotropic system, is characterized in that this device comprises following integral part:
Pressurizing tower (HT), reboiler (R1), condenser (C1), return tank (A1), atmospheric tower (LT), reboiler (R2), condenser (C2), return tank (A2), force (forcing) pump (P1), force (forcing) pump (P2); Wherein force (forcing) pump (P1) connects pressurizing tower (HT) opening for feed, at the bottom of reboiler (R1) is connected in pressurizing tower (HT) tower, pressurizing tower (HT) tower top, condenser (C1), return tank (A1), atmospheric tower (LT) opening for feed connect with pipeline successively, at the bottom of reboiler (R2) is connected in atmospheric tower (LT) tower, atmospheric tower (LT) tower top, condenser (C2), return tank (A2), force (forcing) pump (P2), pressurizing tower (HT) circulation fluid opening for feed connect with pipeline successively.
According to another preferred implementation of the present invention, it is characterized in that the method comprises the steps:
(1) propyl carbinol and MIBK raw material mixed solution are delivered to a rectifying of pressurizing tower (HT) through force (forcing) pump (P1), part pressurizing tower (HT) materials at bottom of tower enters tower bottom reboiler (R1), after boiling, enter pressurizing tower (HT), partial material is as the extraction of MIBK product again;
(2) pressurizing tower (HT) overhead vapor stream is after condenser (C1) condensation, return tank (A1) are collected, and partial material passes back into pressurizing tower (HT), and partial material is delivered to atmospheric tower (LT) and carries out secondary rectifying;
(3) atmospheric tower (LT) overhead vapor stream is after condenser (C2) condensation, return tank (A2) are collected, and partial material passes back into atmospheric tower (LT), and partial material is delivered to pressurizing tower (HT) through force (forcing) pump (P2);
(4) part atmospheric tower (LT) materials at bottom of tower enters tower bottom reboiler (R2), then after boiling, enters atmospheric tower (LT), and partial material is as the extraction of propyl carbinol product.
According to another preferred implementation of the present invention, it is characterized in that: pressurizing tower (HT) working pressure is 3~10atm, and reflux ratio is 1.5~3.5; Atmospheric tower (LT) working pressure is 1atm, and reflux ratio is 1.5~3.0.
According to another preferred implementation of the present invention, it is characterized in that: 29 of pressurizing tower (HT) number of theoretical plates, feed plate position 15~18, recycle stream feed plate position 18~22; 30 of atmospheric tower (LT) number of theoretical plates, feed plate position 15~17.
According to another preferred implementation of the present invention, it is characterized in that: 151.2~203.1 ℃ of pressurizing tower (HT) tower top temperatures, 160~224.2 ℃ of column bottom temperatures; 113.6 ℃ of atmospheric tower (LT) tower top temperatures, 117.7 ℃ of column bottom temperatures.
According to another preferred implementation of the present invention, it is characterized in that: the purity of the propyl carbinol product that the separation of use the method obtains is 99.85%~99.95%, and yield is 99.85%~99.95%; The purity range of MIBK product is 99.90%~99.99%, and yield is 99.90%~99.99%.
The device of the separated propyl carbinol of described high pressure normal pressure two-tower rectification and MIBK azeotropic system accounts for more than 50% propyl carbinol and the application in MIBK azeotrope system at rectifying separation MIBK.
According to another preferred implementation of the present invention, it is characterized in that: the purity of the propyl carbinol product that the separation of use the method obtains is 99.85%~99.95%, and yield is 99.85%~99.95%; The purity range of MIBK product is 99.90%~99.99%, and yield is 99.90%~99.99%.
The method of the separated propyl carbinol of high pressure normal pressure two-tower rectification of the present invention and MIBK azeotropic system specifically describes as follows:
Under normal temperature, propyl carbinol and MIBK mixed solution 1 is first delivered to pressurizing tower HT via force (forcing) pump P1, carries out rectifying separation propyl carbinol and MIBK mixture.At the bottom of in tower, liquid flow to tower, partial material 5 is as the extraction of MIBK product, and partial material enters tower bottom reboiler R1, produces rising steam 4 and enter in HT after water vapour heating.Overhead vapours in overhead condenser C1 with water coolant heat exchange, all condensations, the liquid collecting that condensation is got off is in return tank A1, partial condensation liquid 2 refluxes and returns in tower HT, 3 of partial condensation liquid utilize pressure reduction to deliver to atmospheric tower LT.
Logistics 3 is delivered to pressurizing tower LT and carries out secondary rectifying.At the bottom of part tower, liquid 9 is as the extraction of propyl carbinol product, and another part enters tower bottom reboiler R2, produces rising steam 8 and enter in LT after water vapour heating.Overhead vapours in overhead condenser C2 with water coolant heat exchange, all condensations, the liquid collecting that condensation is got off is in return tank A2, partial condensation liquid 6 refluxes and returns in tower LT, 7 of partial condensation liquid are delivered to HT via force (forcing) pump P2.
In the present invention, HT tower working pressure is 3~10atm, HT tower diameter 500~670mm, 151.2~203.1 ℃ of HT tower top temperatures, 160~224.2 ℃ of HT column bottom temperatures, 29 of number of theoretical plates, feed plate position 15~18, recycle stream feed plate position 18~22, reflux ratio 1.5~3.5; LT tower working pressure is 1atm, LT tower diameter 400~600mm, 113.6 ℃ of LT tower top temperatures, 117.7 ℃ of LT column bottom temperatures, 30 of number of theoretical plates, feed plate position 15~17, reflux ratio 1.5~3.0.Above pressure value all represents absolute pressure.
Using the purity of the propyl carbinol product after the method separation is 99.85%~99.95%; The purity range of MIBK product is 99.90%~99.99%.
Use the method can obtain propyl carbinol and MIBK product, the scope 99.85%~99.95% that the yield of propyl carbinol reaches simultaneously; The scope 99.90%~99.99% that the yield of MIBK reaches.
[beneficial effect]
The present invention compared with prior art, mainly contains following beneficial effect:
(1) reduced the cost of sepn process;
(2) product is not introduced impurity, and purity is improved;
(3) without the solvent recovery process of extracting rectifying, technique is simple, and device rationally;
(4) propyl carbinol, MIBK product yield improve.
Accompanying drawing explanation
Fig. 1 is the high pressure normal pressure two-tower rectification schematic diagram of separated propyl carbinol and MIBK azeotropic system, wherein:
HT-pressurizing tower; LT-atmospheric tower; A1, A2-return tank; C1, C2-overhead condenser; R1, R2-tower bottom reboiler;
P1, P2-force (forcing) pump; Each logistics of numeral.
Embodiment
Embodiment 1:
Feed rate is 1000kg/h, 25 ℃ of temperature, pressure 1atm(absolute pressure), quality forms: propyl carbinol 30%, MIBK70%.Pressurizing tower HT tower diameter 650mm, 29 of number of theoretical plates, the 18th charging, cycling stream is in the 21st plate charging of tower HT.Atmospheric tower LT tower diameter 550mm, 30 of number of theoretical plates, the 15th charging.
Distillation system Operating parameters is in Table 1, and system feeding and product stream situation are in Table 2.Data in table, after separation: propyl carbinol product purity reaches 99.85%; MIBK product purity reaches 99.95%; The yield of propyl carbinol reaches 99.85%; The yield of MIBK reaches 99.95%.
Table 1. distillation system process operation parameter
The charging of table 2. distillation system and product stream table
Embodiment 2:
Feed rate is 1000kg/h, 25 ℃ of temperature, pressure 1atm(absolute pressure), quality forms: propyl carbinol 40%, MIBK60%.Pressurizing tower HT tower diameter 580mm, 29 of number of theoretical plates, the 17th charging, cycling stream is in the 20th plate charging of tower HT.Atmospheric tower LT tower diameter 550mm, 30 of number of theoretical plates, the 17th charging.Distillation system Operating parameters is in Table 3, and system feeding and product stream situation are in Table 4.Data in table, after separation: propyl carbinol product purity reaches 99.95%; MIBK product purity reaches 99.97%; The yield of propyl carbinol reaches 99.95%; The yield of MIBK reaches 99.97%.
Table 3. distillation system process operation parameter
The charging of table 4. distillation system and product stream table
Embodiment 3:
Feed rate is 1000kg/h, 25 ℃ of temperature, pressure 1atm(absolute pressure), quality forms: propyl carbinol 20%, MIBK80%.Pressurizing tower HT tower diameter 550mm, 29 of number of theoretical plates, the 16th charging, cycling stream is in the 19th plate charging of tower HT.Atmospheric tower LT tower diameter 400mm, 30 of number of theoretical plates, the 15th charging.Distillation system Operating parameters is in Table 5, and system feeding and product stream situation are in Table 6.Data in table, after separation: propyl carbinol product purity reaches 99.95%; MIBK product purity reaches 99.99%; The yield of propyl carbinol reaches 99.95%; The yield of MIBK reaches 99.99%.
Table 5. distillation system process operation parameter
The charging of table 6. distillation system and product stream table
Embodiment 4:
Feed rate is 1000kg/h, 25 ℃ of temperature, pressure 1atm(absolute pressure), quality forms: propyl carbinol 15%, MIBK85%.Pressurizing tower HT tower diameter 670mm, 29 of number of theoretical plates, the 16th charging, cycling stream is in the 18th plate charging of tower HT.Atmospheric tower LT tower diameter 600mm, 30 of number of theoretical plates, the 16th charging.Distillation system Operating parameters is in Table 7, and system feeding and product stream situation are in Table 8.Data in table, after separation: propyl carbinol product purity reaches 99.88%; MIBK product purity reaches 99.99%; The yield of propyl carbinol reaches 99.88%; The yield of MIBK reaches 99.99%.
Table 7. distillation system process operation parameter
The charging of table 8. distillation system and product stream table

Claims (8)

1. a device for the separated propyl carbinol of high pressure normal pressure two-tower rectification and MIBK azeotropic system, is characterized in that this device comprises following integral part:
Pressurizing tower (HT), reboiler (R1), condenser (C1), return tank (A1), atmospheric tower (LT), reboiler (R2), condenser (C2), return tank (A2), force (forcing) pump (P1), force (forcing) pump (P2); Wherein force (forcing) pump (P1) connects pressurizing tower (HT) opening for feed, at the bottom of reboiler (R1) is connected in pressurizing tower (HT) tower, pressurizing tower (HT) tower top, condenser (C1), return tank (A1), atmospheric tower (LT) opening for feed connect with pipeline successively, at the bottom of reboiler (R2) is connected in atmospheric tower (LT) tower, atmospheric tower (LT) tower top, condenser (C2), return tank (A2), force (forcing) pump (P2), pressurizing tower (HT) circulation fluid opening for feed connect with pipeline successively.
2. right to use requires the separated propyl carbinol of high pressure normal pressure two-tower rectification and the device rectifying separation propyl carbinol of MIBK azeotropic system and the method for mibk (MIBK) azeotropic system described in 1, it is characterized in that the method comprises the steps:
(1) propyl carbinol and MIBK raw material mixed solution are delivered to a rectifying of pressurizing tower (HT) through force (forcing) pump (P1), part pressurizing tower (HT) materials at bottom of tower enters tower bottom reboiler (R1), after boiling, enter pressurizing tower (HT), partial material is as the extraction of MIBK product again;
(2) pressurizing tower (HT) overhead vapor stream is after condenser (C1) condensation, return tank (A1) are collected, and partial material passes back into pressurizing tower (HT), and partial material is delivered to atmospheric tower (LT) and carries out secondary rectifying;
(3) atmospheric tower (LT) overhead vapor stream is after condenser (C2) condensation, return tank (A2) are collected, and partial material passes back into atmospheric tower (LT), and partial material is delivered to pressurizing tower (HT) through force (forcing) pump (P2);
(4) part atmospheric tower (LT) materials at bottom of tower enters tower bottom reboiler (R2), then after boiling, enters atmospheric tower (LT), and partial material is as the extraction of propyl carbinol product.
3. as method according to claim 2, it is characterized in that: pressurizing tower (HT) working pressure is 3~10atm, and reflux ratio is 1.5~3.5; Atmospheric tower (LT) working pressure is 1atm, and reflux ratio is 1.5~3.0.
4. as method according to claim 3, it is characterized in that: 29 of pressurizing tower (HT) number of theoretical plates, feed plate position 15~18, recycle stream feed plate position 18~22; 30 of atmospheric tower (LT) number of theoretical plates, feed plate position 15~17.
5. as method according to claim 3, it is characterized in that: 151.2~203.1 ℃ of pressurizing tower (HT) tower top temperatures, 160~224.2 ℃ of column bottom temperatures; 113.6 ℃ of atmospheric tower (LT) tower top temperatures, 117.7 ℃ of column bottom temperatures.
6. as method according to claim 3, it is characterized in that: the purity of the propyl carbinol product that the separation of use the method obtains is 99.85%~99.95%, and yield is 99.85%~99.95%; The purity range of MIBK product is 99.90%~99.99%, and yield is 99.90%~99.99%.
7. first pressurizing tower rectifying claimed in claim 1, the device of atmospheric tower rectifying separation propyl carbinol and the MIBK azeotropic system application in rectifying separation propyl carbinol and MIBK azeotrope system again.
8. purposes according to claim 7, is characterized in that: the purity of the propyl carbinol product that the separation of use the method obtains is 99.85%~99.95%, and yield is 99.85%~99.95%; The purity range of MIBK product is 99.90%~99.99%, and yield is 99.90%~99.99%.
CN201410388310.5A 2014-08-08 2014-08-08 High pressure normal pressure two-tower rectification is separated the method for propyl carbinol and MIBK azeotropic system Active CN104151137B (en)

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CN105130742A (en) * 2015-07-26 2015-12-09 青岛科技大学 Method for separating mixture of tert-butyl alcohol and benzene through pressure swing distillation
CN106431880A (en) * 2016-09-12 2017-02-22 青岛科技大学 Novel method for rectifying and separating acetone and isopropyl ether systems under variable pressures

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CN105130742A (en) * 2015-07-26 2015-12-09 青岛科技大学 Method for separating mixture of tert-butyl alcohol and benzene through pressure swing distillation
CN105001056A (en) * 2015-09-06 2015-10-28 青岛科技大学 Method for separating isobutyl alcohol and normal heptanes azeotropic system by using pressure swing distillation
CN105001056B (en) * 2015-09-06 2016-06-08 青岛科技大学 A kind of method of variable-pressure rectification separation isobutanol and normal heptane azeotropic system
CN106431880A (en) * 2016-09-12 2017-02-22 青岛科技大学 Novel method for rectifying and separating acetone and isopropyl ether systems under variable pressures
CN106431880B (en) * 2016-09-12 2019-07-26 青岛科技大学 Novel variable-pressure rectification acetone, isopropyl ether object system method

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