CN105175280A - Acetonitrile-tert-butanol azeotropic mixture continuous extraction rectification separation method - Google Patents

Acetonitrile-tert-butanol azeotropic mixture continuous extraction rectification separation method Download PDF

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Publication number
CN105175280A
CN105175280A CN201510335523.6A CN201510335523A CN105175280A CN 105175280 A CN105175280 A CN 105175280A CN 201510335523 A CN201510335523 A CN 201510335523A CN 105175280 A CN105175280 A CN 105175280A
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acetonitrile
extraction
tower
trimethyl carbinol
extraction agent
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CN105175280B (en
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马守涛
崔玉
姜占坤
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University of Jinan
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University of Jinan
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    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00—Technologies relating to chemical industry
    • Y02P20/50—Improvements relating to the production of bulk chemicals
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
    • Y02P70/10—Greenhouse gas [GHG] capture, material saving, heat recovery or other energy efficient measures, e.g. motor control, characterised by manufacturing processes, e.g. for rolling metal or metal working

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Abstract

The present invention discloses an acetonitrile-tert-butanol azeotropic mixture continuous extraction rectification separation method. According to the method, propanediol and butanediol form a mixture according to any ratios, the operation conditions of an extraction rectification tower are used, a mass ratio of the extractant to the fed material is 0.5:1-10:1, different temperature ratios and different reflux ratios of the continuous extraction rectification tower top and the solvent recovery tower top are controlled, the acetonitrile is extracted from the extraction rectification tower top, the tert-butanol is extracted from the solvent recovery tower top, and the extractant at the tower bottom enters the extraction rectification tower so as to be recycled. According to the present invention, the extractant is used to damage the acetonitrile-tert-butanol azeotropic system to separate the high purity acetonitrile product and the high purity tert-butanol product; and the continuous rectification efficiency is high, the yield is large, and the solvent recovery is simple.

Description

Acetonitrile-trimethyl carbinol azeotropic mixture continuous extraction distillation and separation method
Technical field
The present invention relates to the continuous extraction distillation and separation method of a kind of acetonitrile-trimethyl carbinol azeotropic mixture, belong to the isolation technique of acetonitrile-trimethyl carbinol azeotropic mixture.
Background technology
Extracting rectifying is a kind of special extract rectification isolation technique, is applicable to the separation of azeotropic system.To reach the object of separation with the relative volatility changing stock blend by adding extraction agent continuously toward the top of rectifying tower.The advantage of continuous rectification and extracting rectifying is merged in continuous extraction rectifying, has flexible operation, and separating power is large, efficiency high, is applicable to being separated of azeotropic system in enormous quantities and system of closely boiling.The chemical structural formula of acetonitrile is: C 2h 3n, acetonitrile is a kind of important industrial chemicals, is also that a kind of important organic-solvent industrial is widely used simultaneously.The trimethyl carbinol (TBA), has another name called trimethyl carbinol, 2-methyl-2-propanol, is colourless crystallization or transparent liquid, has camphor smell under normal temperature.Boiling point 82.8 DEG C, tool water absorbability, can be dissolved in multiple organic solvent.Volatile, inflammable, poisonous.And the trimethyl carbinol and acetonitrile form azeotropic system, azeotropic temperature is 74.83 DEG C, has certain difficulty so be industrially separated.This patent discloses a kind of novel extraction agent, adopts the method for extracting rectifying to be separated.About the article of extracting rectifying aspect and patent a lot, not yet publish the data of acetonitrile-trimethyl carbinol azeotropic system separation of extractive distillation aspect.
Summary of the invention
The object of the present invention is to provide a kind of acetonitrile-trimethyl carbinol azeotropic mixture continuous extraction distillation and separation method, the isolated acetonitrile of the method, trimethyl carbinol product purity are high.
The present invention is realized by following technical proposals.Employing comprises extractive distillation column, solvent recovery tower, heating kettle, condenser, the continuous extraction rectifier unit that products pot and pump are formed, continuous extraction rectifying separation acetonitrile-trimethyl carbinol azeotropic mixture, its feature comprises following process: with propylene glycol, butyleneglycol or the two with arbitrary proportion composition mixture for extraction agent, extractive distillation column and solvent recovery tower operate under the following conditions, the extraction agent of extractive distillation column is entered and charge proportion is 0.5:1-10:1 at normal pressure or decompression, raw material enters from the bottom of extractive distillation column, extraction agent enters from the top of extractive distillation column, the temperature of charging is 20-60 DEG C, the temperature of extraction agent is 50-80 DEG C, when tower top temperature is 70-80 DEG C, overhead product is acetonitrile, and reflux ratio is 3:1-10:1, and overhead product enters products pot V-0101, when column bottom temperature is 90-120 DEG C, the trimethyl carbinol-extraction agent overhead product is entered solvent recovery tower, and feeding temperature is 20-60 DEG C, from the middle part charging of tower, when solvent recuperation column overhead temperatures is 80-90 DEG C, control reflux ratio is 3:1-10:1, by the overhead extraction trimethyl carbinol, enters products pot V-0102, when the temperature at the bottom of tower be higher than tower when 100 DEG C at the bottom of the higher extraction agent of extraction purity, reboil ratio is 5:1-10:1, and the extraction agent pump distillated enters extractive distillation column and recycles.Thus can continuous extraction rectifying separation be carried out.
Idiographic flow (see photo): acetonitrile-t-butanol mixture is joined in heating kettle, open thermal source and the water of condensation of heating kettle, rectifying tower top to be extracted have backflow and tower top temperature stable after, extraction agent enters extractive distillation column from the top of tower, when the purity of overhead product reaches requirement, the acetonitrile of overhead extraction enters products pot, the trimethyl carbinol-the extraction agent distillated at the bottom of tower enters the middle part of solvent recovery tower, in the tower reactor of solvent recovery tower liquid level reach two/for the moment, open thermal source and the water of condensation of the heating kettle of solvent recovery tower.After the tower top temperature of solvent recovery tower is stable, the trimethyl carbinol product introduction products pot that tower top distillates, the extraction agent distillated at the bottom of tower and fresh extraction agent enter the top of extractive distillation column, and raw material constantly enters extractive distillation column always.Thus reach the optimal operational condition of continuous rectification separation.
The invention has the advantages that and use rationally effective extraction agent to destroy acetonitrile-trimethyl carbinol azeotropic system, isolate highly purified acetonitrile, the trimethyl carbinol, adopt continuous extraction rectifying, good separating effect, productive rate is large.
Accompanying drawing explanation
Fig. 1 continuous extraction rectifier unit: T-0101 extractive distillation column T-0102 solvent recovery tower E-0101 extractive distillation column overhead condenser, E-0102 extractive distillation column tower bottom reboiler, E-0103 solvent recuperation tower top condenser, E-0104 solvent recovery tower tower bottom reboiler, V-0101 extracting rectifying column overhead storage tank, V-0102 solvent recuperation column overhead Tank, P-0101 solvent recovery tower reflux pump.
Embodiment
Embodiment 1: adopt continuous rectification apparatus, drop in the heating kettle of extractive distillation column azeotropic mixture acetonitrile-trimethyl carbinol 500L(wherein acetonitrile be 54%, the trimethyl carbinol is 46%, be molecular fraction), extraction agent selected by test is propylene glycol, open the thermal source of extractive distillation column and the water of condensation of condenser, after rectifying tower tower top temperature-stable to be extracted, backflow for some time, extraction agent propylene glycol is added on the top of extractive distillation column, the ratio of extraction agent and charging is 2:5, when the temperature of extractive distillation column is 70-80 DEG C, acetonitrile product will be distillated in extracting rectifying column overhead, reflux ratio is 3:1.When the column bottom temperature of extractive distillation column is 90-120 DEG C, the trimethyl carbinol-the extraction agent distillated at the bottom of tower is incorporated into the top of solvent recovery tower, reboil ratio is 1:5, and now in extractive distillation column, add raw material and extraction agent continuously, input speed is respectively 100L/h, 40L/h.Solvent recuperation column overhead have backflow and temperature remain on 80-90 DEG C substantially constant time, the overhead extraction trimethyl carbinol.The reflux ratio of extraction is 2:1; When solvent recovery tower column bottom temperature is higher than 100 DEG C, be driven into extractive distillation column by the extraction agent pump distillating purity at the bottom of tower higher, from the object reaching continuous rectification separation.
Embodiment 2: experimental installation and working method are with embodiment 1, and extraction agent adopts butyleneglycol
Embodiment 3: experimental installation and working method are with embodiment 1, and extraction agent adopts the equal-volume mixture of propylene glycol and butyleneglycol.

Claims (3)

1. the continuous extraction distillation and separation method of acetonitrile-trimethyl carbinol azeotropic mixture, the method adopts the extracting rectifying device comprising extractive distillation column, solvent recovery tower, heating kettle, condenser and products pot and form, continuous extraction rectifying separation acetonitrile-trimethyl carbinol azeotropic mixture.
2. the continuous extraction distillation and separation method of a kind of acetonitrile-trimethyl carbinol azeotropic mixture as claimed in claim 1, it is characterized in that with propylene glycol, butyleneglycol or the two with arbitrary proportion mixture for extraction agent.
3. a kind of acetonitrile as claimed in claim 2-trimethyl carbinol azeotropic mixture continuous extraction distillation and separation method, its feature comprises following process: extractive distillation column and solvent recovery tower operate under the following conditions: enter the extraction agent of extractive distillation column and charge proportion is 0.5:1-10:1 at normal pressure or decompression, raw material enters from the bottom of extractive distillation column, extraction agent enters from the top of extractive distillation column, the temperature of charging is 20-60 DEG C, and the temperature of extraction agent is 50-80 DEG C; When tower top temperature is 70-80 DEG C, overhead product is acetonitrile, and reflux ratio is 3:1-10:1, and overhead product enters products pot V-0101, when column bottom temperature is 90-120 DEG C, the trimethyl carbinol-extraction agent overhead product is entered solvent recovery tower, and feeding temperature is 20-60 DEG C, from the middle part charging of tower, when solvent recuperation column overhead temperatures is 80-90 DEG C, control reflux ratio is 3:1-10:1, by the overhead extraction trimethyl carbinol, enters products pot V-0102; The extraction agent that extraction purity is higher at the bottom of the temperature at the bottom of tower is higher than tower when 100 DEG C, reboil ratio is 5:1-10:1, and the extraction agent pump distillated enters extractive distillation column and recycles, thus can carry out continuous extraction rectifying separation.
CN201510335523.6A 2015-06-17 2015-06-17 Acetonitrile-tert-butyl alcohol azeotropic mixture continuous extraction distillation and separation method Expired - Fee Related CN105175280B (en)

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Cited By (6)

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CN105906479A (en) * 2016-05-24 2016-08-31 济南大学 Method for separating butanol-butyronitrile mixture
CN105949036A (en) * 2016-05-24 2016-09-21 济南大学 Separation method of propyl alcohol-allyl alcohol mixture
CN106008159A (en) * 2016-05-24 2016-10-12 济南大学 Method for separating isopropyl alcohol-propionitrile mixture
CN106220532A (en) * 2016-07-21 2016-12-14 青岛科技大学 A kind of separation of extractive distillation acetonitrile and the method for triethylamine
CN106492497A (en) * 2016-09-27 2017-03-15 大庆中蓝石化有限公司 High boiling mixture between extractive distillation column and tower bottom reboiler stablizes heat riser
CN110681173A (en) * 2019-10-23 2020-01-14 广州首联环境工程有限公司 Multifunctional waste organic solvent recovery device and application thereof

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Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105906479A (en) * 2016-05-24 2016-08-31 济南大学 Method for separating butanol-butyronitrile mixture
CN105949036A (en) * 2016-05-24 2016-09-21 济南大学 Separation method of propyl alcohol-allyl alcohol mixture
CN106008159A (en) * 2016-05-24 2016-10-12 济南大学 Method for separating isopropyl alcohol-propionitrile mixture
CN105949036B (en) * 2016-05-24 2019-01-22 济南大学 A kind of separation method of propyl alcohol-allyl alcohol mixture
CN106008159B (en) * 2016-05-24 2019-01-22 济南大学 A kind of separation method of isopropanol-propionitrile mixture
CN105906479B (en) * 2016-05-24 2019-01-22 济南大学 A kind of separation method of butanol-butyronitrile mixture
CN106220532A (en) * 2016-07-21 2016-12-14 青岛科技大学 A kind of separation of extractive distillation acetonitrile and the method for triethylamine
CN106220532B (en) * 2016-07-21 2018-06-22 青岛科技大学 A kind of method of separation of extractive distillation acetonitrile and triethylamine
CN106492497A (en) * 2016-09-27 2017-03-15 大庆中蓝石化有限公司 High boiling mixture between extractive distillation column and tower bottom reboiler stablizes heat riser
CN110681173A (en) * 2019-10-23 2020-01-14 广州首联环境工程有限公司 Multifunctional waste organic solvent recovery device and application thereof

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