CN104844404B - The method that continuous lateral line rectification couples separation of extractive distillation hendecane, dodecane and positive ten alcohol - Google Patents
The method that continuous lateral line rectification couples separation of extractive distillation hendecane, dodecane and positive ten alcohol Download PDFInfo
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- CN104844404B CN104844404B CN201510137644.XA CN201510137644A CN104844404B CN 104844404 B CN104844404 B CN 104844404B CN 201510137644 A CN201510137644 A CN 201510137644A CN 104844404 B CN104844404 B CN 104844404B
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- dodecane
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
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Abstract
The method that continuous lateral line rectification couples separation of extractive distillation hendecane, dodecane and positive ten alcohol：(1) raw material adds continuous lateral line rectifying column, through rectification pretreatment, obtain simultaneously overhead fraction that boiling range is 102.1～103.4 DEG C 2., the tower bottom distillate of 146.7～147.9 DEG C of 3. with 186.2～187.5 DEG C of side run-off 4., wherein side run-off 3. dodecane more than 94.8%；(2) 3. side run-off enters extractive distillation column, is extractant using glycerol, and 5. tower top obtains overhead fraction that boiling range is 121.0～122.1 DEG C, dodecane content more than 99.2%, and 6. tower bottom distillate mainly contains extractant；(3) 6. tower bottom distillate is processed through solvent recovery tower, and tower reactor recycles for extractant.The present invention adopts continuous lateral line rectification to couple separation of extractive distillation technique, and not only process is simple, separation efficiency are high, improves content and the yield of dodecane simultaneously, the having a high potential of industrialized production.
Description
Technical field
The present invention relates to a kind of chemical separating method, more particularly to a kind of continuous lateral line rectification coupling separation of extractive distillation
The method of hendecane, dodecane and positive ten alcohol.
Background technology
Produce substantial amounts of front-end volatiles and mink cell focus in soybean oil produces, wherein front-end volatiles account for the 12% about of total amount,
In front-end volatiles containing 23% about hendecane, 56% about dodecane and 21% about positive ten alcohol, the monomer such as dodecane is weight
The chemical industry wanted and pharmaceutical raw material, for producing SL-AH, straight chain alcohol and alkyl halide, as daily chemical products primary raw material
Deng.Using front-end volatiles as industrial solvent or fuel oil processing in the conventional production in soybean oil, not only waste important raw material,
Environment is produced with certain impact simultaneously.
Dodecane is mainly derived from the heavy distillat (boiling point >=200 DEG C) after extracting No. 200 solvent naphthas, through isomerization and rectification
Prepared by associated methods, because the method difficulty is big, high cost, domestic at present only small-scale production, only about 35 tons of yield/
Year, the content of product reaches 98%.Dodecane not yet forms large-scale production, basic dependence on import at home.
In view of during domestic soybean oil produces at present front-end volatiles behaviour in service, the present invention provides a kind of continuous lateral line rectification coupling
The method closing hendecane, dodecane and positive ten alcohol in separation of extractive distillation soybean oil front-end volatiles.
Content of the invention
It is an object of the invention to provide a kind of continuous lateral line rectification coupling separation of extractive distillation hendecane, dodecane and just
The method of ten alcohol, initially with the method pretreatment hendecane of continuous lateral line rectification, dodecane and positive ten alcohol mixtures, just gets
Three fractions to different boiling ranges；Then the fraction mainly comprising dodecane is processed using extraction rectifying method, separate dodecane
With positive ten alcohol, obtain more than 99.2% dodecane, this process choosing glycerol is extractant, separating effect significantly improves；And adopt
Solvent recovery tower reclaims glycerol, and solvent recycles.This process is simple, separation efficiency are high, low production cost, industrialized production
Have a high potential.
For achieving the above object, the present invention adopts the following technical scheme that：
A kind of method that continuous lateral line rectification couples separation of extractive distillation hendecane, dodecane and positive ten alcohol, step is as follows：
(1) raw material hendecane, dodecane and positive ten alcohol mixed liquors add continuous lateral line rectifying column, and bottom of towe heats, control tower
Top, bottom of towe and side stream temperature, through rectification pretreatment, obtain simultaneously overhead fraction that boiling range is 102.1 DEG C～103.4 DEG C 2., boiling
Journey be 146.7 DEG C～147.9 DEG C of side run-off 3. with boiling range be 186.2 DEG C～187.5 DEG C tower bottom distillate 4.；Wherein, side
Line fraction 3. middle dodecane content be more than 94.8wt%；
(2) 3. side run-off enters extractive distillation column, is extractant using glycerol, controls tower top, column bottom temperature, extraction essence
Evaporate column overhead and obtain overhead fraction that boiling range is 121.0 DEG C～122.1 DEG C 5., dodecane content is more than 99.2wt%；Bottom of towe
Obtain tower bottom distillate that boiling range is 199.1 DEG C～201.7 DEG C 6., mainly contain extractant and a small amount of dodecane, positive ten alcohol；
(3) extractive distillation column tower bottom distillate is 6. through solvent recovery tower rectification process, solvent recovery tower overhead extraction dodecane
With positive ten alcohol fractions 7., 8. tower reactor produces extractant, then flows into extractive distillation column recycling.
In above scheme, the extractant in described (2nd) step is glycerol, extractant and extractive distillation column feedstock amount
Mass ratio be 1：0.8-1.2.
Described raw material hendecane, dodecane and positive ten alcohol mixed liquors by weight percentage, consisting of hendecane 22
～25%, dodecane 55～58% and positive ten alcohol 20～22%.
In described method, in (2nd) step, the Stress control of extractive distillation column is 0.05～1.0atm.
In described method, in (3rd) step, solvent recovery column overhead temperatures are 127.5～128.6 DEG C, and bottom temperature is
211.4～213.3 DEG C, reflux ratio is 2～3.
Said method initially with the method pretreatment hendecane of continuous lateral line rectification, dodecane and positive ten alcohol mixtures,
Different boiling ranges are controlled to obtain hendecane, dodecane and positive ten alcohol fractions, traditional handicraft needs two rectifying columns just can complete this
Business；Two is mainly to comprise dodecane, the fraction containing positive ten alcohol on a small quantity to just get, separates ten using extraction rectifying method
Dioxane and positive ten alcohol, this process choosing glycerol is extractant, and separating effect significantly improves, and can obtain more than 99.2% ten two
Alkane.Finally, glycerol is reclaimed using solvent recovery tower, solvent recycles.Methods described process is simple, separation efficiency are high.
More specific and more optimally say, taking front-end volatiles during soybean oil produces as a example, hendecane in its composition, dodecane and just
Ten alcohol are about hendecane 22～23%, dodecane 56～57% and positive ten alcohol 20～21%, couple extraction using continuous lateral line rectification
Rectification is taken to carry out separating, the concrete operation step of the present invention is：
(1) raw material hendecane, dodecane and positive ten alcohol mixed liquors add continuous lateral line rectifying column, and control inlet amount is
10Kg/h, tower top, side line and bottom of towe load D2、D3And D4It is respectively 2.5Kg/h, 4.5Kg/h and 3.0Kg/h, tower top temperature exists
102.1 DEG C～103.4 DEG C, bottom temperature at 186.2 DEG C～187.5 DEG C, side stream temperature at 146.7 DEG C～147.9 DEG C, reflux ratio
4～5, theoretical cam curve be 50, feedstock position at the 25th block of column plate, lateral line discharging position at the 30th block of column plate, warp
Continuous lateral line rectifying column pretreatment, can obtain simultaneously boiling range be 102.1 DEG C～103.4 DEG C evaporate tower top divide 2., boiling range be 146.7
DEG C～147.9 DEG C of side run-off 3. with boiling range be 186.2 DEG C～187.5 DEG C tower bottom distillate 4., overhead fraction 2. hendecane
The content of fraction be >=91.40%, side run-off 3. middle dodecane content be >=94.8%, tower bottom distillate 4. mainly contain ten
Dioxane and positive ten alcohol.
(2) 3. the side run-off of continuous lateral line rectifying column enters extractive distillation column, and feedstock amount is 4.0Kg/h, tower top
With bottom of towe load D5And D6It is respectively 3.8Kg/h and 4.2Kg/h, control tower top temperature at 121.0～122.1 DEG C, bottom temperature
At 199.1～201.7 DEG C, 2～3, theoretical cam curve is 30 to reflux ratio, and 3. side run-off enters extracting rectifying tower position the
15 blocks of plates, 5. extractant feed position obtains content >=99.20% of dodecane in the 3rd block of plate, extractive distillation column overhead fraction,
Tower reactor be the tower bottom distillate containing a large amount of extractants, a small amount of dodecane and positive ten alcohol 6..
Described extractant is glycerol, and extractant is 1: 1 with the optimum quality ratio of extractive distillation column feedstock amount.
(3) 6. above-mentioned extractive distillation column tower bottom distillate is processed through solvent recovery tower, and control inlet amount is 4.2Kg/h, tower top
With bottom of towe load D7And D8It is respectively 0.19Kg/h, 4.01Kg/h, at 127.5～128.6 DEG C, bottom temperature exists tower top temperature
211.4～213.3 DEG C, in the 12nd block of plate, 2～3, solvent recovery column overhead is dodecane and positive ten alcohol to reflux ratio to feed entrance point
Fraction 7., tower reactor be extractant 8., content more than 99.70%, then flow into extractive distillation column recycle.
Above-mentioned separation process conditions and result are as shown in Table 1 and Table 2.
The process conditions of table 1 separation process
The composition of table 2 each fraction of separation process and content
The method that the continuous lateral line rectification of the present invention couples separation of extractive distillation hendecane, dodecane and positive ten alcohol, adopts
Continuous lateral line rectification carries out pretreatment, and after mixed alkanes are preprocessed, the content rich in dodecane fraction brings up to 94.80%
More than, yield is more than 75%；Adopt extraction rectifying method separation dodecane and positive ten alcohol again, extracting rectifying adopts glycerol
As extractant, improve separation efficiency, the content of dodecane component brings up to more than 99.2%, yield is more than 94.5%.
The inventive method process is simple, separation efficiency are high, significantly reduce production cost, the having a high potential of industrialized production.
Describe the present invention with reference to specific embodiment.Protection scope of the present invention is not to be embodied as
Mode is limited, but is defined in the claims.
Brief description
Fig. 1 is the process chart of continuous lateral line rectification and extracting rectifying integrated purification hendecane, dodecane and positive ten alcohol；
In figure, 1, continuous lateral line rectifying column, 2, extractive distillation column, 3, solvent recovery tower.
Specific embodiment
Below by specific embodiment, technical solutions according to the invention are further described in detail, but are necessary
Point out that following examples are served only for the description to content of the invention, do not constitute limiting the scope of the invention.
Embodiment 1, continuous lateral line rectification couples the mixture of separation of extractive distillation hendecane, dodecane and positive ten alcohol, respectively
Tower internal diameter is 57cm, using φ 3 × 3 θ type stainless steel helices, through being measured with standards system, this height equivalent to one theoretical plate HETP=
27mm, tower reactor adopts pressure regulator to control electrical heating, is qualitatively and quantitatively analyzed by gas chromatography-mass spectrometry chromatogram instrument.Methods described
Comprise the following steps：
(1) 1. raw material hendecane, dodecane and positive ten alcohol mixed liquors add continuous lateral line rectifying column 1, and tower reactor passes through pressure regulation
Device controls electrical heating, feedstock amount and operating parameter and the results are shown in Table shown in 3, and 2. overhead fraction for hendecane content is
91.40%, side run-off 3. middle dodecane content be 94.8%, tower bottom distillate 4. contain dodecane and positive ten alcohol；
(2) 3. the side run-off of continuous lateral line rectifying column 1 enters extractive distillation column 2, feedstock amount and operating parameter and
The results are shown in Table shown in 4, the content that 5. extractive distillation column 2 overhead fraction obtains dodecane fraction is 99.60%, and tower reactor is containing big
The fraction of amount extractant, dodecane and positive ten alcohol is 6.；
(3) 6. the above-mentioned fraction containing a large amount of extractants, dodecane and positive ten alcohol is processed through solvent recovery tower 3, controls
Inlet amount is 4.2Kg/h, load D7And D8Be respectively 0.19Kg/h, 4.01Kg/h, tower top temperature at 128.1 DEG C, bottom temperature
At 212.3 DEG C, in the 12nd block of plate, 2～3, solvent recovery tower 3 tower top is dodecane and positive ten alcohol fractions to reflux ratio to feed entrance point
7., 8. tower reactor fraction is containing 99.7% extractant, then flows into extractive distillation column 2 and recycle.
Table 3 side line rectifying column operating condition and separating resulting
Table 4 extractive distillation column operating condition and separating resulting
Embodiment 2, substantially the same manner as Example 1, but in described (2nd) step, the Stress control of extractive distillation column 2 is
0.05atm, extracting rectifying experimental result is shown in Table 5.
Table 5 extractive distillation column operating condition and separating resulting
Embodiment 3, substantially the same manner as Example 1, but in described (2nd) step, the Stress control of extractive distillation column is
1.0atm, extracting rectifying experimental result is shown in Table 6.
Table 6 extractive distillation column operating condition and separating resulting
Claims (7)
1. a kind of method that continuous lateral line rectification couples separation of extractive distillation hendecane, dodecane and positive ten alcohol, step is as follows：
(1) raw material hendecane, dodecane and positive ten alcohol mixed liquors add continuous lateral line rectifying column, and bottom of towe heats, and controls tower top, tower
Bottom and side stream temperature, through rectification pretreatment, obtain simultaneously overhead fraction that boiling range is 102.1 DEG C～103.4 DEG C 2., boiling range be
146.7 DEG C～147.9 DEG C of side run-off 3. with boiling range be 186.2 DEG C～187.5 DEG C of tower bottom distillate 4.；Wherein, side line evaporates
The content dividing 3. middle dodecane is more than 94.8wt%；
(2) 3. side run-off enters extractive distillation column, is extractant using glycerol, controls tower top, column bottom temperature, extractive distillation column
5. tower top obtains overhead fraction that boiling range is 121.0 DEG C～122.1 DEG C, and wherein the content of dodecane is more than 99.2wt%, tower
6. bottom obtains tower bottom distillate that boiling range is 199.1 DEG C～201.7 DEG C, mainly contains extractant and a small amount of dodecane, positive ten alcohol；
(3) extractive distillation column tower bottom distillate is 6. through solvent recovery tower rectification process, solvent recovery tower overhead extraction dodecane and just
7., 8. tower reactor extraction extractant, then flows into extractive distillation column recycling to ten alcohol fractions.
2. continuous lateral line rectification according to claim 1 couples separation of extractive distillation hendecane, dodecane and positive ten alcohol
Method it is characterised in that：In described (2nd) step, extractant glycerol is 1 with the mass ratio of extractive distillation column feedstock amount:
0.8～1.2.
3. continuous lateral line rectification coupling separation of extractive distillation hendecane according to claim 1 and 2, dodecane and positive ten alcohol
Method it is characterised in that described raw material hendecane, dodecane and positive ten alcohol mixed liquors by weight percentage, its composition
For hendecane 22～25%, dodecane 55～58% and positive ten alcohol 20～22%.
4. continuous lateral line rectification according to claim 3 couples separation of extractive distillation hendecane, dodecane and positive ten alcohol
Method it is characterised in that described raw material hendecane, dodecane and positive ten alcohol mixed liquors by weight percentage, consisting of,
Hendecane 22～23%, dodecane 56～57% and positive ten alcohol 20～21%.
5. continuous lateral line rectification according to claim 4 couples separation of extractive distillation hendecane, dodecane and positive ten alcohol
It is characterised in that in methods described, (1st) step controls reflux ratio 4～5, side line theoretical number of plates of rectifying tower is 50 to method,
At the 25th block of column plate, lateral line discharging position is at the 30th block of column plate for feedstock position；(2nd) step controls reflux ratio 2
～3, extractive distillation column theoretical cam curve is 30, and 3. side run-off enters extracting rectifying tower position in the 15th block of plate, and extractant enters
Discharge position is in the 3rd block of plate.
6. continuous lateral line rectification coupling separation of extractive distillation hendecane according to claim 1 and 2, dodecane and positive ten alcohol
Method it is characterised in that in described method, in (2nd) step, the Stress control of extractive distillation column is 0.05～1.0atm.
7. continuous lateral line rectification coupling separation of extractive distillation hendecane according to claim 1 and 2, dodecane and positive ten alcohol
Method it is characterised in that in described method, in (3rd) step, solvent recovery column overhead temperatures are 127.5～128.6 DEG C,
Bottom temperature is 211.4～213.3 DEG C, and reflux ratio is 2～3.
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| CN105646126B (en) * | 2016-03-07 | 2018-10-23 | 南京师范大学 | The separation method of toluene, dimethylbenzene, trimethylbenzene in a kind of aromatic solvent naphtha |
| CN105777472B (en) * | 2016-04-15 | 2018-01-23 | 河北工业大学 | It is a kind of to separate pentane, hexane, heptane and the method for octane mixture system |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3506569A (en) * | 1966-12-24 | 1970-04-14 | Nippon Mining Co | Process for production of normal paraffins from middle distillate by urea adduction |
| CN101360699A (en) * | 2005-12-14 | 2009-02-04 | 考格尼斯知识产权管理有限责任公司 | Process for the production of hydrocarbons |
| WO2014159484A1 (en) * | 2013-03-14 | 2014-10-02 | E. I. Du Pont De Nemours And Company | Process for making linear long-chain alkanes from renewable feedstocks using catalysts comprising heteropolyacids |
| WO2014159490A1 (en) * | 2013-03-14 | 2014-10-02 | E. I. Du Pont De Nemours And Company | Process for making linear long-chain alkanes from renewable feedstocks using catalysts comprising heteropolyacids |
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| CN101538185A (en) * | 2009-04-14 | 2009-09-23 | 中国石化扬子石油化工有限公司 | Method for extracting mesitylene fraction rich in hydrocracking C 9 by combination of continuous lateral line distillation and extractive distillation |
| CN101851188A (en) * | 2010-05-14 | 2010-10-06 | 南京师范大学 | Method and device for extracting Alpha-pyrrolidone and N-vinyl pyrrolidine by integrating side rectification and extractive distillation |
| CN102219699A (en) * | 2011-04-28 | 2011-10-19 | 江苏沿江化工资源开发研究院有限公司 | Method for separating nitroethane and 2-nitropropane by combined process of continuous side distillation and extractive distillation |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3506569A (en) * | 1966-12-24 | 1970-04-14 | Nippon Mining Co | Process for production of normal paraffins from middle distillate by urea adduction |
| CN101360699A (en) * | 2005-12-14 | 2009-02-04 | 考格尼斯知识产权管理有限责任公司 | Process for the production of hydrocarbons |
| WO2014159484A1 (en) * | 2013-03-14 | 2014-10-02 | E. I. Du Pont De Nemours And Company | Process for making linear long-chain alkanes from renewable feedstocks using catalysts comprising heteropolyacids |
| WO2014159490A1 (en) * | 2013-03-14 | 2014-10-02 | E. I. Du Pont De Nemours And Company | Process for making linear long-chain alkanes from renewable feedstocks using catalysts comprising heteropolyacids |
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