CN101225012B - Method for ultrasonic extraction and distillation separation of benzene-cyclohexane and benzene-n-heptane - Google Patents
Method for ultrasonic extraction and distillation separation of benzene-cyclohexane and benzene-n-heptane Download PDFInfo
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- CN101225012B CN101225012B CN2008100639382A CN200810063938A CN101225012B CN 101225012 B CN101225012 B CN 101225012B CN 2008100639382 A CN2008100639382 A CN 2008100639382A CN 200810063938 A CN200810063938 A CN 200810063938A CN 101225012 B CN101225012 B CN 101225012B
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Abstract
The invention provides a method in separating benzene from cyclohexane and from heptane by ultrasonic extractive distillation, comprising steps as ultrasonic processing and extractive distillation. The ultrasonic extractive distillation method adopts the conditions for the extractive distillation in that: under atmospheric pressure, a volume ratio between the raw material solution and solvent is between 0.2 and 2; constant temperature for the distilled materials is kept between 70 and 80 centigrade; the bottom temperature is constantly kept between 90 and 120 centigrade; the ultrasonic processing is characterized in that ultrasonic fields, with ultrasonic output frequencies from 20 to 24 KHz, powers from 200 to 308W and ultrasonic time from 10 to 40 minutes, are added at the pre-processingphase, or intermittently or continuously added in the process of extractive distillation. Aiming at the benzene and cyclohexane azeotropic system and the benzene and heptane systems with close boiling points, the ultrasonic techniques coupled with the extractive distillation is put forward to improve the separation efficiency of the extractive distillation through the acoustic cavitation of the ultrasonic wave.
Description
One, technical field
The present invention relates to a kind of novel combination isolation technique, specifically is ultrasonic and the extractive distillation coupling technique.
Two, background technology
Sepn process at present is towards efficient fine separation trend development, and the research focus has certain extreme colors, concentrates on the extraction of high purity substance preparation, minor component and relative volatility and levels off on the difficult problems such as separation of 1 system.
Level off to the separation of 1 system for relative volatility, as remove alkane impurity hexanaphthene in the crude benzol, (benzene and hexanaphthene form azeotrope for normal heptane and methylcyclohexane etc., and only be 0.962) for the benzene that contains benzene 93% (molar mass mark) and its relative volatility of normal heptane mixture, the normal extraction and distillation technology that adopts, classical extraction and distillation technology is to increase relative volatility between the pre-separation component by adding a large amount of solvents, though obtained gratifying effect, but solvent load has brought a series of problem demanding prompt solutions greatly, restricted the development of this technology in a sense, thereby the research of reduction solvent load becomes the hot subject of academia.It is reported that extractive distillation with salt can be successfully applied to the separation of polarity system, the salt of selection also locate initial stage just and to(for) the separation of nonpolar system all also rests on the experimental phase, and the salt component is separated out the problem solution of still needing easily; The double solvents extraction and distillation technology is that to select two kinds of single solvents to carry out composite, and it is added rectifying then in the stock liquid of pre-separation, and this method relates to that solvent is selected and compositely waits work, needs spend great effort and predicts and experimental study.Under this background, this patent proposes technology ultrasonic and extractive distillation coupling separation of benzol-cyclohexane azeotrope and the nearly boiling point system of benzene-normal heptane, it is simple that it has technology, energy-conservation and separation efficiency advantages of higher is for separation of benzol-cyclohexane azeotrope and the nearly boiling point system of benzene-normal heptane provide another novel method.
Three, summary of the invention
The object of the present invention is to provide a kind of method that can improve the ultrasonic extraction fractionation by distillation benzol-cyclohexane azeotrope and the nearly boiling point system of benzene-normal heptane of separation efficiency.
The object of the present invention is achieved like this: it comprises supersound process and extractive distillation two portions, the condition of described extractive distillation is: the volume ratio of normal pressure, stock liquid and solvent is 0.2～2, steam the thing homo(io)thermism at 70～80 ℃, the still temperature is constant at 90～120 ℃; Described supersound process is to add ultrasonic field in the extractive distillation process, the adding mode be add at the pretreatment stage of extractive distillation, extractive distillation process discontinuous adds or the extractive distillation process in add continuously, ultrasonic output frequency is 20～24KHz, power is 200～308W, and ultrasonic time is 10～40min.
The present invention can also comprise:
1, described solvent is N, dinethylformamide (DMF) or furfural.
2, described stock liquid is the benzol-cyclohexane azeotrope, and benzene mole content is 45%～58%.
3, described stock liquid is the nearly boiling point system of benzene-normal heptane, benzene mole content 93.3%.
4, described extractive distillation technology is periodical operation.
The present invention is directed to the nearly boiling point system of benzol-cyclohexane azeotrope and benzene-normal heptane, propose ultrasonic technique and extractive distillation coupled technology, utilize hyperacoustic sound cavitation effect to improve the separating effect of extractive distillation.Thereby hyperacoustic sound cavitation effect has greatly strengthened organic solvent and has strengthened solvent molecule and the intermolecular effect of stock liquid mixing of stock liquid, has improved the relative volatility between separated component.Promptly consume less solvent load and can obtain separating effect preferably.
Four, description of drawings
Fig. 1 is the influence figure of ultrasonic field to benzene-normal heptane-furfural system distillation relative volatility;
Fig. 2 is the influence figure of ultrasonic field to benzol-cyclohexane-DMF system distillation relative volatility.
Five, embodiment
Illustrate the specific embodiment of the present invention below:
Embodiment one: the nearly boiling point system of ultrasonic extraction fractionation by distillation benzene-normal heptane
Benzene and normal heptane mixture (the normal heptane molar content is 6.74%) place ultrasonic field 30min, (the ultrasonic field condition is output frequency 22KHz, and power is 240W) with after a certain amount of furfural solvent (solvent ratio 0.5: 1～2: 1) mixes.Material poured in the extractive distillation still distill.The extractive distillation working pressure is a normal pressure, and the still temperature is constant to be 90～120 ℃, and steaming thing is normal heptane and benzol mixture.Analyze every the 15min sample thief.Do not add ultrasonic field with similarity condition and distill sampling analysis.Add ultrasonic system and do not add ultrasonic system relative volatility result as shown in Figure 1.
Under same solvent ratio, the relative volatility of the system of adding ultrasonic field is than not adding the big of ultrasonic field as seen from Figure 1.
Embodiment two: ultrasonic extraction fractionation by distillation benzol-cyclohexane azeotrope
Get approach benzene that azeotrope forms and hexanaphthene mixture (benzene mole content is 45%～58%) and a certain amount of DMF solvent (solvent ratio 0.2) mix after, material poured in the extractive distillation still distills.The extractive distillation working pressure is a normal pressure, and the still temperature is 90～120 ℃, intermittently adds ultrasonic field (the ultrasonic field condition is: output frequency 22KHz, power are 308W) 10min every 10min.When vapour-liquid phase temperature equates, when being constant at 80～85 ℃, getting and steam thing and carry out check and analysis with chromatogram.Do not add ultrasonic field with similarity condition and distill sampling analysis.Add ultrasonic system and do not add ultrasonic system relative volatility result as shown in Figure 2:
As seen from Figure 2 under same solvent ratio, the relative volatility that the nearly azeotropic point of benzol-cyclohexane is formed the system that adds ultrasonic field down than do not add ultrasonic field greatly, so the adding of ultrasonic field can improve separating effect.We it can also be seen that solvent ratio is that ultrasonic field effect in 0.2 o'clock can make relative volatility bring up to 1.48 by 1.17 from figure.
Claims (4)
1. one kind is used for benzol-cyclohexane or the isolating ultrasonic extraction distillating method of benzene-normal heptane system, it comprises supersound process and extractive distillation two portions, it is characterized in that: the condition of described extractive distillation is: the volume ratio of normal pressure, stock liquid and solvent is 0.2～2, steam the thing homo(io)thermism at 70～80 ℃, the still temperature is constant at 90～120 ℃; Described supersound process is to add ultrasonic field in the extractive distillation process, the adding mode is to add continuously in adding of extractive distillation process discontinuous or extractive distillation process, ultrasonic output frequency is 20～24KHz, power is 200～308W, ultrasonic time is 10～40min, described solvent is N, dinethylformamide or furfural.
2. benzol-cyclohexane or the isolating ultrasonic extraction distillating method of benzene-normal heptane system of being used for according to claim 1, it is characterized in that: described stock liquid is the benzol-cyclohexane azeotrope, benzene mole content is 45%～58%.
3. benzol-cyclohexane or the isolating ultrasonic extraction distillating method of benzene-normal heptane system of being used for according to claim 1, it is characterized in that: described stock liquid is the nearly boiling point system of benzene-normal heptane, benzene mole content 93.3%.
4. according to claim 1,2 or 3 described benzol-cyclohexane or the isolating ultrasonic extraction distillating methods of benzene-normal heptane system of being used for, it is characterized in that: described extractive distillation technology is periodical operation.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2008100639382A CN101225012B (en) | 2008-01-30 | 2008-01-30 | Method for ultrasonic extraction and distillation separation of benzene-cyclohexane and benzene-n-heptane |
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| CN2008100639382A CN101225012B (en) | 2008-01-30 | 2008-01-30 | Method for ultrasonic extraction and distillation separation of benzene-cyclohexane and benzene-n-heptane |
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| CN101225012A CN101225012A (en) | 2008-07-23 |
| CN101225012B true CN101225012B (en) | 2010-06-02 |
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| CN103073383B (en) * | 2013-02-07 | 2015-07-01 | 天津大学 | Method and device for separating isohexane, n-hexane and benzene |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6392115B1 (en) * | 2000-09-18 | 2002-05-21 | Phillips Petroleum Company | Separation of hydrocarbons by extractive distillation |
| CN1430660A (en) * | 2000-04-28 | 2003-07-16 | Gtc技术公司 | Aromatic separation from petroleum streams |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1430660A (en) * | 2000-04-28 | 2003-07-16 | Gtc技术公司 | Aromatic separation from petroleum streams |
| US6392115B1 (en) * | 2000-09-18 | 2002-05-21 | Phillips Petroleum Company | Separation of hydrocarbons by extractive distillation |
Non-Patent Citations (4)
| Title |
|---|
| 张志刚 等.常规间歇萃取精馏分离苯-环己烷的研究.化学工程34 (4).2006,34((4)),5-8. |
| 张志刚 等.常规间歇萃取精馏分离苯-环己烷的研究.化学工程34 (4).2006,34((4)),5-8. * |
| 秦炜 等.超声场对化工分离过程的强化.化工进展 (1).1995,((1)),1-5. |
| 秦炜 等.超声场对化工分离过程的强化.化工进展 (1).1995,((1)),1-5. * |
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