CN106008159B - A kind of separation method of isopropanol-propionitrile mixture - Google Patents
A kind of separation method of isopropanol-propionitrile mixture Download PDFInfo
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- CN106008159B CN106008159B CN201610346561.6A CN201610346561A CN106008159B CN 106008159 B CN106008159 B CN 106008159B CN 201610346561 A CN201610346561 A CN 201610346561A CN 106008159 B CN106008159 B CN 106008159B
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- propionitrile
- isopropanol
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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
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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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- 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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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The present invention provides a kind of separation method of isopropanol-propionitrile mixture, belongs to isopropanol-propionitrile 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 isopropanol-propionitrile mixture separation fields, mixed more particularly, to a kind of isopropanol-propionitrile
The extraction and rectification separation method of object is closed, wherein including interval and continuous two kinds of modes of operation.
Background technique
Isopropanol and the propionitrile all common solvent of chemical industry and pharmaceutical field or raw material, and dosage is all very huge.Isopropanol
As industrial chemicals, it is mainly used to produce ketone and the relevant product of esters, but main still as industrial less expensive rubber
In addition to this solvent of glue etc. also acts as antifreezing agent, detergent, the additive of blended gasoline, the dispersing agent of pigment production, print
Fixative, glass and antifoggant of transparent plastic of dyer's industry etc..Propionitrile is mainly used as organic synthesis raw material, solvent and resin and adds
Add agent, a small amount of intermediate for being used as medicine or pesticide.
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 is using the model under conventional extracting rectifying continuous operation, and entire technical process uses atmospheric distillation, 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, makes product purity be affected.And continuous extracting rectifying mode is related only in the patent, to small-scale yield
It is required that being unable to satisfy.
Currently, delivering or reporting there is no relevant document about the separation of isopropanol-propionitrile azeotropic mixture.
Summary of the invention
The purpose of the invention is to overcome deficiency present in prior art, and it is directed to isopropanol-propionitrile mixture, mentioned
It is a kind of out 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, a kind of isopropanol of the technical solution adopted by the present invention-propionitrile 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 isopropanol-propionitrile relative volatility.Ionic liquid
Additive amount and Solvent quantity ratio are 0.03:1 ~ 0.10:1.
A kind of separation method of isopropanol-propionitrile mixture as described in the above technical scheme, wherein continuity operates: main
It to include extraction tower and recovery tower, the extraction tower number of plates is 30 ~ 45, and extractant feed position is 3 ~ 8 blocks of column plates, extractant and original
Material charge ratio is 1:1 ~ 4:1, and feedstock position is 20 ~ 28 blocks of column plates, and according to nearly azeotropic ratio into tower, tower top returns feedstock
Stream is than being 0.8:1 ~ 2.1:1, extraction tower overhead extraction isopropanol；The recovery tower number of plates is 30 ~ 50, and feed entrance point is 16 ~ 24 pieces
Column plate, reflux ratio 1.5:1 ~ 3:1, overhead extraction propionitrile, tower reactor recycle extractant ethylene glycol.
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 isopropanol, and kettle material is delivered to through high temperature delivery pump
Recovery tower；After recovery tower is heated to tower top stabilization, overhead extraction propionitrile, extractant returns extraction tower and applies.
The intermittent operation, mainly rectifying tower plates number are 20 ~ 35 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 1:1 ~ 3:1, and extractant and feedstock ratio are 2.2:1 ~ 4:1；
Solvent recovery stage reflux ratio is 1.5:1 ~ 2.8:1；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 isopropanol content, starts to adopt with reflux ratio
Out；After tower top isopropanol content starts reduction, stops extractant and be added；Changeover portion 1 is adopted by reflux ratio to storage tank, until tower
Top propionitrile content reaches 99.5% or more；After tower top propionitrile 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 is with raw material dosage ratio
1.5:1 ~ 2:1, extractant feed position are 5 ~ 6 blocks of column plates, and reflux ratio is 1.1:1 ~ 1.3:1；The recovery tower number of plates is 35 ~ 40,
Reflux ratio is 1.9:1 ~ 2.1:1.Under the optimum condition, continuous operation mode is capable of the isopropyl of steady production content >=99.9%
Alcohol, propionitrile product, and be best in energy consumption, stability.
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 3:1 ~ 6:1, and extracting rectifying stage reflux ratio is 1.8:1 ~ 2.0:1, and recovery stage reflux ratio is 2.4:1 ~ 2.8:1,
2 reflux ratio of changeover portion is 3.5:1 ~ 3.8:1.Under the optimum condition, isopropanol of the content higher than 99.5% can be obtained and propionitrile produces
Product, and the content of extractant is 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 propionitrile 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 isopropanol and propionitrile 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 200kg/h；Feed throughput is
100kg/h, raw material group becomes isopropanol and the azeotropic of propionitrile forms.The extraction tower number of plates is 40, and extractant feed position is the 5th
Block column plate, feedstock position is in 25 blocks of column plates.Reflux ratio is set as 1.2:1, and the isopropanol purity that tower top obtains is 99.8%.
The recovery tower number of plates is 40, and feed entrance point is the 20th block of column plate, and reflux ratio 2:1, the propionitrile purity that tower top obtains is 99.5%,
Tower bottom extractant purity is 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, and (isopropanol azeotropic composition close with propionitrile is total for raw material
It 100kg) is added at one time tower reactor, is begun to warm up, after band overhead reflux is stablized, extractant is added with the speed of 80 ~ 100kg/hr
In tower, reach 99.5% to tower top isopropanol content with reflux ratio 1.8:1 extraction；Start to be reduced to 90% to tower top isopropanol content
After below, stops extractant and be added；Changeover portion 1 is adopted by reflux ratio 3:1 to storage tank, until tower top propionitrile content reaches 99.5%
More than, start to produce propionitrile product with reflux ratio 2:1；After tower top propionitrile content is reduced to 90% or less, changeover portion 2 passes through reflux
It produces than 3:1 to storage tank, reaches 99.5% or more to tower reactor extraction agent content, stop heating.
Embodiment three
On the basis of example 1, the implementation case is all made of the parameter being related under optimum condition, and final isopropanol contains
Amount >=99.99%, propionitrile content >=99.9% extract 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, and final isopropanol contains
Amount >=99.9%, propionitrile content >=99.8%.
Claims (1)
1. a kind of isopropanol-propionitrile mixture separation method, it is characterised in that: the method includes continuity mode of operation or
Intermittent operation mode；The continuity mode of operation mainly includes extraction tower and recovery tower, and the extraction tower number of plates is 30~45,
Extractant feed position is 3~8 blocks of column plates, and feedstock position is 20~28 blocks of column plates, and the recovery tower number of plates is 30~50, into
Material position is set to 16~24 blocks of column plates；The intermittent operation mainly includes rectifying column, and the number of plates is 20~35 blocks of column plates, is operated
Journey is divided into extracting rectifying stage, transition stage 1, recovery stage, transition stage 2；
In continuity operating process, operating parameter are as follows: extractant and the mass ratio of raw material dosage are 1.5:1~2:1, extractant into
Material position is set to 5~6 blocks of column plates, and reflux ratio is 1.1:1~1.3:1；Recovery tower reflux ratio is 1.9:1~2.1:1；
During intermittent operation, operating parameter are as follows: the mass ratio of extractant total feed and material quantity is 3:1~6:1, extraction
Stage of rectification reflux ratio is 1.8:1~2.0:1, and recovery stage reflux ratio is 2.4:1~2.8:1, and changeover portion reflux ratio is
3.5:1~3.8:1；
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 propionitrile 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 isopropanol-propionitrile mixture is the mixture of isopropanol and propionitrile azeotropic composition.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106588862A (en) * | 2016-12-05 | 2017-04-26 | 东营市海科新源化工有限责任公司 | Ethylene carbonate purification process and purification system |
| CN107488103B (en) * | 2017-08-24 | 2020-06-05 | 王婵 | Extraction and rectification method for water-isopropanol azeotropic mixture |
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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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