CN105906479B - A kind of separation method of butanol-butyronitrile mixture - Google Patents
A kind of separation method of butanol-butyronitrile mixture Download PDFInfo
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- CN105906479B CN105906479B CN201610346565.4A CN201610346565A CN105906479B CN 105906479 B CN105906479 B CN 105906479B CN 201610346565 A CN201610346565 A CN 201610346565A CN 105906479 B CN105906479 B CN 105906479B
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- butyronitrile
- butanol
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- C—CHEMISTRY; METALLURGY
- 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
- C07C29/84—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by distillation by extractive distillation
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C253/00—Preparation of carboxylic acid nitriles
- C07C253/32—Separation; Purification; Stabilisation; Use of additives
- C07C253/34—Separation; Purification
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- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The present invention provides a kind of separation method of butanol-butyronitrile mixture, belongs to butanol-butyronitrile azeotropic mixture separation field.The present invention uses continuous operation mode and intermittent operation mode, by optimizing operating parameter, while improving product quality, reduces energy consumption, investment.In the biggish situation of production scale, continuous operation mode can be selected, it being capable of stabilized product quality, raising income, reduction cost of labor；Conversely, andnon-continuous operation manner, flexible operation can be selected.
Description
Technical field
The present invention relates to butanol-butyronitrile mixture separation fields, more particularly, to a kind of butanol-butyronitrile mixture
Extraction and rectification separation method, wherein comprising interval and continuous two kinds of modes of operation.
Background technique
Butanol and the butyronitrile all common solvent of chemical industry and pharmaceutical field or raw material, and dosage is all very huge.Butanol is more
The solvent of kind coating and the raw material of plasticizer phthalic acid dibutyl ester processed, are also used for manufacture butyl acrylate, butyl acetate, second
Glycol butyl ether and extractant as organic synthesis intermediate and biochemical medicine, are also used to manufacture surfactant；Butyronitrile
It is close with acetonitrile property, it is mainly used to do the raw material of organic synthesis.
It is divided into azeotropic distillation and extracting rectifying substantially for azeotropic system separation means at present, and extracting rectifying is come
It says, is mainly two kinds of modes of operation of continuous and intermittent in mode of operation.Continuous operation under extraction rectification technique mainly for
The operating condition that yield is big, automatic control level is high, stable product quality is high, intermittently operated mainly use it is not high with output demand, to from
Control degree requires low operation operating condition.
Chinese patent CN103159586A proposes a kind of dimethyl carbonate-methanol azeotropic mixture continuous extraction rectifying separation
Method.This method uses atmospheric distillation using the model under conventional extracting rectifying continuous operation, entire technical process.Due to whole
The presence of tower pressure drop causes temperature in tower higher, decomposes or polymerize so that the dimethyl carbonate containing unsaturated bond be promoted to generate
Reaction, so that product purity is affected, and relate only to continuous extracting rectifying mode in the patent, to small-scale yield
Working condition requirement is unable to satisfy.
Currently, delivering or reporting there is no relevant document about the separation of butanol-butyronitrile azeotropic mixture.
Summary of the invention
The purpose of the invention is to overcome deficiency present in prior art, and it is directed to butanol-butyronitrile mixture, proposed
It is a kind of to be suitable for the technique that most of operating condition, product purity are high, production stability is strong.
In order to solve the above technical problems, the technical solution adopted by the present invention is a kind of butanol-butyronitrile mixture extracting rectifying
Method, this method is operated using continuity or intermittent operation；Meanwhile in the innovation of extractant, the present invention uses imidazoles
Auxiliary additive of the ionic liquid as extractant ethylene glycol can be improved butanol-butyronitrile relative volatility.Ionic liquid adds
Dosage and Solvent quantity ratio are 0.03:1 ~ 0.10:1.
A kind of separation method of butanol-butyronitrile mixture as described in the above technical scheme, wherein continuity operates: main
Comprising extraction tower and recovery tower, the extraction tower number of plates is 35 ~ 60, and extractant feed position is 3 ~ 10 blocks of column plates, extractant and original
Material charge ratio is 4:1 ~ 7:1, and feedstock position is 24 ~ 28 blocks of column plates, and according to nearly azeotropic ratio into tower, tower top returns feedstock
Stream is than being 0.3:1 ~ 1:1, extraction tower overhead extraction butanol；The recovery tower number of plates is 25 ~ 40, and feed entrance point is 16 ~ 24 blocks of column plates,
Reflux ratio 3:1 ~ 5:1, overhead extraction butyronitrile, tower reactor recycle extractant ethylene glycol；Two column overhead operating pressures are 20KPa(exhausted
Pressure).
Raw material is delivered to preheater by head tank or feed pump, by preheater by the continuous operation process
Into in tower；After being heated to overhead reflux stabilization in tower reactor, extractant is delivered to preheating by head tank or feed pump
Device simultaneously enters in tower；After gas-liquid composition is stablized in tower, tower top starts to produce butanol；Kettle material is delivered to recycling through delivery pump
Tower, after recycling column overhead is stablized, overhead extraction butyronitrile, extractant returns extraction tower and applies.
The intermittent operation, mainly rectifying tower plates number are 30 ~ 45 blocks of column plates, and process is divided into the extracting rectifying stage
With recovery stage and changeover portion, extracting rectifying stage reflux ratio is 0.5:1 ~ 1.5:1, and extractant and feedstock ratio are 4:1 ~ 9:
1；Solvent recovery stage reflux ratio is 3:1 ~ 6:1；Changeover portion reflux ratio is 3:1 ~ 5:1.
The batch process procedures: raw material is added at one time tower reactor, begins to warm up, after band overhead reflux is stablized, extraction
Agent is entered in tower by head tank or feed pump, reaches 99.5% or more to tower top butanol content, starts to produce with reflux ratio；
After tower top butanol content starts reduction, stops extractant and be added；Changeover portion 1 is adopted by reflux ratio to storage tank, until tower top fourth
Nitrile content reaches 99.5% or more；After tower top butyronitrile content starts reduction, changeover portion 2 is produced by reflux ratio to storage tank, to tower reactor
Extraction agent content reaches 99.5% or more, stops heating.
Preferably, in the continuous operation mode: the extraction tower number of plates is 35 ~ 40, and extractant and raw material dosage ratio are 5:1
~ 6:1, extractant feed position are 7 ~ 9 blocks of column plates, and reflux ratio is 0.7:1 ~ 1:1；The recovery tower number of plates is 25 ~ 30, and reflux ratio is
3.5:1~4:1.Under the optimum condition, continuous operation mode is capable of the butanol of steady production content >=99.9%, butyronitrile product,
It and in energy consumption, stability is best.
Preferably, in the andnon-continuous operation manner, rectifying tower plates number be 30 ~ 35, extractant combined feed as far as possible with original
Doses ratio is 4:1 ~ 5:1, and extracting rectifying stage reflux ratio is 0.5:1 ~ 0.8:1, and recovery stage reflux ratio is 3.5:1 ~ 3.8:1,
Changeover portion reflux ratio is 3:1 ~ 5:1.Under the optimum condition, butanol and butyronitrile product that content is higher than 99.5% can be obtained, and extract
Take the content of agent also above 99.8%.
It is a further object of the present invention to provide a kind of rectifier units for the continuous operation mode, and wherein main body is set
Standby is extraction tower, recovery tower, reboiler, condenser, trap, mixer, preheater etc..Make raw material and extraction by preheater
Agent preheating, raw material preheating heat source are the extractants applied from recovery tower tower reactor, and the heat source that extractant preheating uses is public heat
Source.The mixture of extraction tower tower reactor extraction butyronitrile and extractant enters recovery tower, and the extractant of recovery tower tower reactor extraction passes through original
Enter mixer, the supplement as extractant after the preheater of material.
Novelty of the invention is with advantage:
1) separation of butanol and butyronitrile azeotropic system there is no separating technology to report or deliver at present；
2) various operating conditions and simple process be can adapt to, using double tower continuous rectification mode or single column batch fractionating mode,
It can require to be selected according to product yield, flexible operation.
Detailed description of the invention
Fig. 1 is continuous operation flow diagram, Fig. 2 intermittently operated flow diagram.
Specific embodiment
The following are specific implementation case is combined, the invention will be further described, but does not limit the scope of protection of the invention.
Embodiment one
The implementation case is continuous extraction distillation operation mode, Solvent quantity 500kg/h；Feed throughput is
100kg/h, raw material group becomes butanol and the azeotropic of butyronitrile forms.The extraction tower number of plates is 40, and extractant feed position is at the 5th piece
Column plate, feedstock position is in 25 blocks of column plates.Reflux ratio is set as 1:1, and the butanol purity that tower top obtains is 99.8%.Recovery tower
The number of plates is 40, and feed entrance point is the 20th block of column plate, and reflux ratio 4:1, the butyronitrile purity that tower top obtains is 99.5%, tower bottom extraction
It takes agent purity to be higher than 99.9%, and is back to mixer, the supplement as solvent.
Embodiment two
The implementation case is batch extracting rectified mode of operation, raw material (butanol azeotropic close with butyronitrile forms total 100kg)
It is added at one time tower reactor, is begun to warm up, after band overhead reflux is stablized, extractant is added in tower with the speed of 80 ~ 100kg/hr, to
Tower top butanol content reaches 99.5% with reflux ratio 0.8:1 extraction；After tower top butanol content starts to be reduced to 90% or less, stop
Extractant is added；Changeover portion 1 is adopted by reflux ratio 3:1 to storage tank, until tower top butyronitrile content reaches 99.5% or more, start with
Reflux ratio 3:1 produces butyronitrile product；After tower top butyronitrile content is reduced to 90% or less, changeover portion 2 by reflux ratio 3:1 produce to
Storage tank reaches 99.5% or more to tower reactor extraction agent content, stops heating.
Embodiment three
On the basis of example 1, the implementation case is all made of the parameter being related under optimum condition, final butanol content
>=99.99%, butyronitrile content >=99.9% extracts agent content >=99.9%.
Example IV
On the basis of example 1, the implementation case is all made of the parameter being related under optimum condition, final butanol content
>=99.9%, butyronitrile content >=99.8%.
Claims (1)
1. a kind of butanol-butyronitrile mixture separation method, it is characterised in that: the method includes continuity mode of operation or
Having a rest property mode of operation；The continuity mode of operation mainly includes extraction tower and recovery tower, and the extraction tower number of plates is 35~60, extraction
Taking agent feed entrance point is 3~10 blocks of column plates, and the recovery tower number of plates is 25~40, and feed entrance point is 16~24 blocks of column plates；Described
The operation of having a rest property mainly includes rectifying column, and the number of plates is 30~45 blocks of column plates, and operating process is divided into extracting rectifying stage, transition stage
1, recovery stage, transition stage 2；
In continuity operating process, the mass ratio of extractant and raw material dosage is 5:1~6:1, and extractant feed position is 7~9
Block column plate, reflux ratio are 0.7:1~1:1；Recovery tower reflux ratio is 3.5:1~4:1；Two tower operating pressures are absolute pressure 20KPa；
During intermittent operation, the mass ratio of extractant total feed and material quantity is 4~5:1, the reflux of extracting rectifying stage
Than for 0.5:1~0.8:1, recovery stage reflux ratio is 3.5:1~3.8:1, and changeover portion reflux ratio is 3:1~5:1；Operation pressure
Power is absolute pressure 20KPa；
Wherein extractant is the mixed solution of glyoxaline ion liquid and ethylene glycol, the additive amount of glyoxaline ion liquid and extraction
Agent amount ratio is 0.03:1-0.10:1；
Continuity operation mainly include non-standard equipment have: extraction tower, recovery tower, reboiler, condenser, trap, mixer,
Preheater；
Non-standard equipment connection type is to preheat raw material and extractant by preheater, and raw material preheating heat source is from recovery tower tower
The extractant that kettle is applied, the heat source that extractant preheating uses is public heat source；Extraction tower tower reactor produces the mixed of butyronitrile and extractant
It closes object and enters recovery tower, enter mixer after the preheater that the extractant of recovery tower tower reactor extraction passes through raw material, as extractant
Supplement；
The butanol-butyronitrile mixture is the mixture that butanol and butyronitrile azeotropic form.
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Citations (6)
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| CN101134736A (en) * | 2007-09-28 | 2008-03-05 | 天津大学 | Method for separating carbinol acetonitrile azeotrope |
| CN103242120A (en) * | 2013-04-27 | 2013-08-14 | 天津大学 | Circulating device and refining method of extractant in normal hexane, isohexane and benzene separation process |
| CN105001055A (en) * | 2015-07-17 | 2015-10-28 | 济南大学 | Isopropanol-acetonitrile azeotrope rectification separation method based on mixed solvent as extracting agent |
| CN105175280A (en) * | 2015-06-17 | 2015-12-23 | 济南大学 | Acetonitrile-tert-butanol azeotropic mixture continuous extraction rectification separation method |
| CN105503501A (en) * | 2016-01-17 | 2016-04-20 | 济南大学 | Butanol-cyclohexane azeotropic mixture extractive distillation method |
| CN105523889A (en) * | 2016-01-17 | 2016-04-27 | 济南大学 | Extractive distillation method for azeotropic mixture of tert-butyl alcohol and triethylamine |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS62223300A (en) * | 1986-03-25 | 1987-10-01 | 旭化成株式会社 | Fron type solvent mixture |
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Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101134736A (en) * | 2007-09-28 | 2008-03-05 | 天津大学 | Method for separating carbinol acetonitrile azeotrope |
| CN103242120A (en) * | 2013-04-27 | 2013-08-14 | 天津大学 | Circulating device and refining method of extractant in normal hexane, isohexane and benzene separation process |
| CN105175280A (en) * | 2015-06-17 | 2015-12-23 | 济南大学 | Acetonitrile-tert-butanol azeotropic mixture continuous extraction rectification separation method |
| CN105001055A (en) * | 2015-07-17 | 2015-10-28 | 济南大学 | Isopropanol-acetonitrile azeotrope rectification separation method based on mixed solvent as extracting agent |
| CN105503501A (en) * | 2016-01-17 | 2016-04-20 | 济南大学 | Butanol-cyclohexane azeotropic mixture extractive distillation method |
| CN105523889A (en) * | 2016-01-17 | 2016-04-27 | 济南大学 | Extractive distillation method for azeotropic mixture of tert-butyl alcohol and triethylamine |
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