CN104151137B - High pressure normal pressure two-tower rectification is separated the method for propyl carbinol and MIBK azeotropic system - Google Patents
High pressure normal pressure two-tower rectification is separated the method for propyl carbinol and MIBK azeotropic system Download PDFInfo
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- CN104151137B CN104151137B CN201410388310.5A CN201410388310A CN104151137B CN 104151137 B CN104151137 B CN 104151137B CN 201410388310 A CN201410388310 A CN 201410388310A CN 104151137 B CN104151137 B CN 104151137B
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- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
- C07C29/76—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
- C07C29/80—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by distillation
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C45/00—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds
- C07C45/78—Separation; Purification; Stabilisation; Use of additives
- C07C45/81—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation
- C07C45/82—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation by distillation
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- Crystallography & Structural Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
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Abstract
The present invention relates to the rectifier unit that a kind of high pressure normal pressure two-tower rectification is separated propyl carbinol and MIBK azeotropic system.This device is primarily of compositions such as pressurizing tower HT, atmospheric tower LT, force (forcing) pump, return tank and interchanger.Distillation and separation method comprises: raw material is delivered to pressurizing tower HT through P1, and part HT materials at bottom of tower enters HT after entering reboiler R1, and part is then as the extraction of MIBK product; HT overhead vapours is after condenser C1 condensation, return tank A1 collect, and partial reflux enters HT, and part is then delivered to atmospheric tower LT; LT overhead vapours is after condenser C2 condensation, return tank A2 collect, and partial reflux enters LT, and part is then delivered to HT through P2, and part LT materials at bottom of tower enters LT after entering reboiler R2, and part is then as the extraction of propyl carbinol product.Use method of the present invention to reduce the cost being separated propyl carbinol and MIBK, improve product purity and yield, technique is simple, and device is reasonable.
Description
Technical field
The invention belongs to chemical separating purification art, relate to being separated of a kind of propyl carbinol and mibk (MIBK) azeotrope system, double tower tripping device and the method using this device to be separated propyl carbinol and MIBK azeotropic system of particularly a kind of first high-pressure tower rectifying, again atmospheric tower rectifying.
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.Recycle propyl carbinol and MIBK in the industrial production, this extremely has economic implications for enterprise.
Because propyl carbinol and MIBK two-component system exist azeotropic point, therefore be difficult to the propyl carbinol and the MIBK that obtain higher degree by conventional distillation method.Separation method mainly azeotropic distillation and extracting rectifying conventional at present.
Document (methyl isobutyl ketone synthetic fluid heterogeneous azeotropic rectification separating technology is studied. modern chemical industry, 2007.11,27th volume the 2nd phase) provide a kind of heterogeneous azeotropic rectification separation method, adopt the method for heterogeneous azeotropic rectification to be separated with mibk binary azeotropic system propyl carbinol, obtain the mibk that purity is 99.5%.
Document (research of Virahol One-step production methyl iso-butyl ketone (MIBK) sepn process. chemical industry is in progress, 2005.12,24th volume the 5th phase) to report the method that spent glycol comes separation of extractive distillation propyl carbinol and mibk binary azeotropic system as extraction agent be feasible, gained mibk product purity is 99.5%, and yield is 91.7%.
The defect existed in above-mentioned existing isolation technique and deficiency are: the cost compare of sepn process is high; Introduce other materials in system and add separation costs, and have impact on quality product to a certain extent; Technical process is complicated, and brings this problem of new extractant regeneration.
The present invention adopts the method for first high-pressure tower rectifying, again atmospheric tower rectification and purification, specifically, the present invention utilizes the azeotropic of propyl carbinol and MIBK composition to occur this characteristic of larger change with pressure change, first adopt compression rectification tower, adopt atmospheric distillation tower again, be separated propyl carbinol and MIBK azeotropic system, method of the present invention is especially applicable to propyl carbinol and the MIBK azeotropic system that MIBK composition accounts for more than 50%.Do not introduce other components in system of the present invention, while cost-saving, in turn ensure that the quality of product; Technique is simple, and device is reasonable; Highly purified propyl carbinol, MIBK product can be obtained simultaneously.
Summary of the invention
[technical problem that will solve]
The object of this invention is to provide a kind of high pressure normal pressure two-tower rectification tripping device be separated with mibk (MIBK) azeotrope system by propyl carbinol.
Another object of the present invention is to provide the method using described device to be separated propyl carbinol and MIBK azeotrope system.
Another object of the present invention is to provide described device and is being separated the purposes in propyl carbinol and MIBK azeotrope system.
[technical scheme]
The present invention overcomes shortcoming in prior art, proposes the method for a kind of first high-pressure tower rectifying, again atmospheric tower rectifying separation propyl carbinol and MIBK azeotropic system.The present invention utilizes the azeotropic of propyl carbinol and MIBK composition to occur this characteristic of larger change with the change of pressure, adopts the method for two tower pressure reduction rectifying, effective separation of both realizations.This method solve the problems adopting extracting rectifying or azeotropic distillation to be separated propyl carbinol and MIBK existence at present, avoid introducing impurity, reduce separation costs, improve product purity.
The invention provides the high pressure normal pressure double tower tripping device that a kind of technique is simple, be easy to realization, and use this dress separation MIBK to account for the propyl carbinol of more than 50% and the method for MIBK azeotropic system.
The present invention is achieved through the following technical solutions: a kind of high pressure normal pressure two-tower rectification is separated the device of propyl carbinol and MIBK azeotropic system, it 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, reboiler (R1) is connected at the bottom of pressurizing tower (HT) tower, pressurizing tower (HT) tower top, condenser (C1), return tank (A1), atmospheric tower (LT) opening for feed connect with pipeline successively, reboiler (R2) is connected at the bottom of atmospheric tower (LT) tower, and 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 pressurizing tower (HT) rectifying through force (forcing) pump (P1), part pressurizing tower (HT) materials at bottom of tower enters tower bottom reboiler (R1), enter pressurizing tower (HT) after boiling, partial material is then 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 then 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 then 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 enters atmospheric tower (LT) after boiling, and partial material is then 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, 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: pressurizing tower (HT) number of theoretical plate 29 pieces, feed plate position 15 ~ 18, recycle stream feed plate position 18 ~ 22; Atmospheric tower (LT) number of theoretical plate 30 pieces, feed plate position 15 ~ 17.
According to another preferred implementation of the present invention, it is characterized in that: pressurizing tower (HT) tower top temperature 151.2 ~ 203.1 DEG C, column bottom temperature 160 ~ 224.2 DEG C; Atmospheric tower (LT) tower top temperature 113.6 DEG C, column bottom temperature 117.7 DEG C.
According to another preferred implementation of the present invention, it is characterized in that: the purity using the method to be separated the propyl carbinol product obtained 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 that described high pressure normal pressure two-tower rectification is separated propyl carbinol and MIBK azeotropic system rectifying separation MIBK account for more than 50% propyl carbinol and MIBK azeotrope system in application.
According to another preferred implementation of the present invention, it is characterized in that: the purity using the method to be separated the propyl carbinol product obtained 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 that high pressure normal pressure two-tower rectification of the present invention is separated propyl carbinol and MIBK azeotropic system specifically describes as follows:
Under normal temperature, propyl carbinol and MIBK mixed solution 1 are first delivered to pressurizing tower HT via force (forcing) pump P1, carry out a rectifying separation propyl carbinol and MIBK mixture.In tower at the bottom of liquid stream to tower, partial material 5 is as the extraction of MIBK product, and partial material then enters tower bottom reboiler R1, produces upflowing vapor 4 and enter in HT after water vapour heating.Overhead vapours in overhead condenser C1 with water coolant heat exchange, whole condensation, the liquid collecting that condensation is got off in return tank A1, partial condensation liquid 2 backflow return in tower HT, partial condensation liquid 3 utilizes 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 then enters tower bottom reboiler R2, produces upflowing vapor 8 and enter in LT after water vapour heating.Overhead vapours in overhead condenser C2 with water coolant heat exchange, whole condensation, the liquid collecting that condensation is got off in return tank A2, partial condensation liquid 6 backflow return in tower LT, partial condensation liquid 7 is delivered to HT via force (forcing) pump P2.
In the present invention, HT tower working pressure is 3 ~ 10atm, HT tower diameter, 500 ~ 670mm, HT tower top temperature 151.2 ~ 203.1 DEG C, HT column bottom temperature 160 ~ 224.2 DEG C, number of theoretical plate 29 pieces, 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, LT tower top temperature 113.6 DEG C, LT column bottom temperature 117.7 DEG C, number of theoretical plate 30 pieces, feed plate position 15 ~ 17, reflux ratio 1.5 ~ 3.0.Above pressure value all represents absolute pressure.
The purity of the propyl carbinol product after using the method to be separated 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) cost of sepn process is reduced;
(2) product does not introduce impurity, and purity is improved;
(3) without the need to the solvent recovery process of extracting rectifying, technique is simple, and device is reasonable;
(4) propyl carbinol, MIBK product yield improve.
Accompanying drawing explanation
Fig. 1 is the high pressure normal pressure two-tower rectification schematic diagram being 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; The each logistics of numeral.
Embodiment
Embodiment 1:
Feed rate is 1000kg/h, temperature 25 DEG C, pressure 1atm(absolute pressure), quality forms: propyl carbinol 30%, MIBK70%.Pressurizing tower HT tower diameter 650mm, number of theoretical plate 29 pieces, the 18th piece of charging, cycling stream is in tower HT the 21st piece of plate charging.Atmospheric tower LT tower diameter 550mm, number of theoretical plate 30 pieces, the 15th piece of charging.
Distillation system Operating parameters is in table 1, and system feeding and product stream situation are in table 2.From 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, temperature 25 DEG C, pressure 1atm(absolute pressure), quality forms: propyl carbinol 40%, MIBK60%.Pressurizing tower HT tower diameter 580mm, number of theoretical plate 29 pieces, the 17th piece of charging, cycling stream is in tower HT the 20th piece of plate charging.Atmospheric tower LT tower diameter 550mm, number of theoretical plate 30 pieces, the 17th piece of charging.Distillation system Operating parameters is in table 3, and system feeding and product stream situation are in table 4.From 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, temperature 25 DEG C, pressure 1atm(absolute pressure), quality forms: propyl carbinol 20%, MIBK80%.Pressurizing tower HT tower diameter 550mm, number of theoretical plate 29 pieces, the 16th piece of charging, cycling stream is in tower HT the 19th piece of plate charging.Atmospheric tower LT tower diameter 400mm, number of theoretical plate 30 pieces, the 15th piece of charging.Distillation system Operating parameters is in table 5, and system feeding and product stream situation are in table 6.From 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, temperature 25 DEG C, pressure 1atm(absolute pressure), quality forms: propyl carbinol 15%, MIBK85%.Pressurizing tower HT tower diameter 670mm, number of theoretical plate 29 pieces, the 16th piece of charging, cycling stream is in tower HT the 18th piece of plate charging.Atmospheric tower LT tower diameter 600mm, number of theoretical plate 30 pieces, the 16th piece of charging.Distillation system Operating parameters is in table 7, and system feeding and product stream situation are in table 8.From 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 (2)
1. use a method for first pressurizing tower rectifying, again atmospheric tower rectifying separation propyl carbinol and MIBK azeotropic system device rectifying separation propyl carbinol and MIBK azeotropic system, it 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; reboiler R1 is connected at the bottom of pressurizing tower (HT) tower; pressurizing tower (HT) tower top, condenser C1, return tank A1, atmospheric tower (LT) opening for feed connect with pipeline successively; reboiler R2 is connected at the bottom of atmospheric tower (LT) tower, and 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;
The method of this rectifying separation propyl carbinol and MIBK azeotropic system comprises the steps:
(1) propyl carbinol and MIBK raw material mixed solution are delivered to pressurizing tower (HT) rectifying through force (forcing) pump P1, and part pressurizing tower (HT) materials at bottom of tower enters tower bottom reboiler R1, then enters pressurizing tower (HT) after boiling, and partial material is then as the extraction of MIBK product;
(2) pressurizing tower (HT) overhead vapor stream is after condenser C1 condensation, return tank A1 collect, and partial material passes back into pressurizing tower (HT), and partial material is then 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 collect, and partial material passes back into atmospheric tower (LT), and partial material is then 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 enters atmospheric tower (LT) after boiling, and partial material is then as the extraction of propyl carbinol product;
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;
Pressurizing tower (HT) number of theoretical plate 29 pieces, feed plate position 15 ~ 18, recycle stream feed plate position 18 ~ 22; Atmospheric tower (LT) number of theoretical plate 30 pieces, feed plate position 15 ~ 17;
Pressurizing tower (HT) tower top temperature 151.2 ~ 203.1 DEG C, column bottom temperature 160 ~ 224.2 DEG C; Atmospheric tower (LT) tower top temperature 113.6 DEG C, column bottom temperature 117.7 DEG C.
2. method as defined in claim 1, is characterized in that: the purity using the method to be separated the propyl carbinol product obtained 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%.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105130742B (en) * | 2015-07-26 | 2017-02-15 | 青岛科技大学 | Method for separating mixture of tert-butyl alcohol and benzene through 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 |
| 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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| US4656037A (en) * | 1983-08-01 | 1987-04-07 | Shigezo Udaka | SPF-100 and process for the preparation thereof |
| CN202951270U (en) * | 2012-12-14 | 2013-05-29 | 天津大学 | Variable-pressure heat integrated rectifying device for separating ethanol and methylbenzene |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4656037A (en) * | 1983-08-01 | 1987-04-07 | Shigezo Udaka | SPF-100 and process for the preparation thereof |
| CN202951270U (en) * | 2012-12-14 | 2013-05-29 | 天津大学 | Variable-pressure heat integrated rectifying device for separating ethanol and methylbenzene |
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| Comparison of extractive distillation and pressure-swing distillation for acetone-methanol separation;William L.Luyben et al.;《Ind.Eng.Chem.Res.》;20080320;第47卷(第8期);第2696-2707页 * |
| 异丙醇一步法生产甲基异丁基酮分离过程的研究;张成中等;《化工进展》;20051231;第24卷(第5期);第541-544页 * |
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