前苏联专利SU1205755A3 Method of extracting pure benzol from hydrocarbon mixtures

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专利摘要:

公开号:SU1205755A3
申请号:SU823475641
申请日:1982-08-13
公开日:1986-01-15
发明作者:Пройссер Герхард；Шульце Мартин；Эммрих Герд；Шнайдер Ханс-Кристоф
申请人:Крупп-Копперс Гмбх (Фирма)；
IPC主号:

专利说明:

"
The invention relates to a process for the recovery of pure benzene from hydrocarbon mixtures containing, together with aromatic hydrocarbons, any large amount of non-aromatic hydrocarbons, by extractive distillation in the presence of N-formylmorpholine as a selective solvent. This invention may find application in the petrochemical industry.
The purpose of the invention is to reduce energy consumption by using the heat content of the distillate vapor obtained during the preliminary separation of the feedstock to heat the extractive distillation columns and the feedstock. one
The drawing shows a diagram of
according to which the proposed method is carried out.
The technological scheme presented in the drawing contains only those necessary for explaining the method of the device, while other additional devices, for example valves and pumps, are not present. In the presented technological scheme, the preliminary distillation column 1 operates at elevated pressure. The hydrocarbon mixture containing aromatic hydrocarbons serving as a feedstock is fed through conduit 2 and heat exchangers 3 and 4 and, if necessary, 5 in the middle part, equipped with plates of the column 1 for preliminary distillation. This column is equipped with a circulating boiler-heater 6, the tubular system of which can be heated with high-pressure steam or through (not shown). The vaporous head product of the preliminary distillation is removed from the head of the column 1 of the preliminary distillation . In this case, the steam flow in line 7 is divided into two partial flows. A larger partial flow is fed through line 8 to the tubular system of the circulation boiler of heater 9, in which the heat of the steam is used to heat the striker. 10. At the same time, the partial vapor flow from pipe 8 through pipe 11 goes to the tubular system of the circulation boiler of heater 12, which serves to
50
five
,R
5 0 5
0
552
heating the column 13 for extractive distillation.
At the same time, a smaller part of the partial vapor stream of the head product from pipeline 7 is fed through pipe 14 to the tubular system of the indirect heat exchanger 3, in which the heat of vapor is used to preheat the starting product. After the heat exchangers 3 and circulating boilers of heaters 9 and 12, the condensates form, as shown in the flow chart, into the main pipeline 15, which leads to the collector 16, which collects the condensed head product from the distillation column 1. . According to E5ODU 17, it is diverted from collection 16 to the head of column 1 for preliminary distillation as a flep. At the same time, the reflux number and the number of plates in the column 1 of the preliminary distillation are chosen on the basis that the amount of vapors of the main product is sufficient to heat the columns on the subsequent stand of the extractive distillation. The main amount of the obtained head product is fed via line 18 in the form of feed into the middle part, equipped with plates of extractive distillation column 13.
In the column 13 for the extractive distillation and the distillation column 10 belonging to it, the distillation is carried out under a pressure that is lower than the working pressure of the column 1 for the preliminary distillation. Otherwise, the extractive distillation step is carried out according to the principles of extractive distillation. This means that non-aromatic hydrocarbons from the starting product are withdrawn through conduit 19 through the head of the extractive distillation column 13 while the extract containing aromatic hydrocarbons is withdrawn from the bottom of this column through conduit 20 and fed to the stripper 10. The resulting the aromatic hydrocarbon extract is distilled in column 10 and separated from the selective solvent contained in the extract. This solvent is withdrawn from conduit 21 from the bottom of the stripping column 10 and is again fed to the head of the extractive distillation column 13, while the aromatic hydrocarbons simultaneously obtained are withdrawn from the stripping column 10 as a leading product through the conduit 22.
Pipeline 23 in column 13 can be fed fresh solvent in the circulating solvent.
The product leaving the bottom of the pre-distillation column 1 is passed through conduit 24 and fed through heat exchanger 4 to collector 25, from which this product is withdrawn through conduit 25 for further use. In the heat exchanger 4, the heat of the product leaving the distillation column 1 from the bottom of the column 1 is used to preheat the starting feed that comes through conduit 2.
The process scheme also provides heat exchangers 27 and 28 for using the bottom product heat of the distant column 10 (solvent) to heat the columns 13 and 10. The solvent, having passed heat exchangers 27 and 28, goes to the top of the extractive distillation column 1.3 via line 29.
Example 1. This example illustrates the production of pure benzene from refined coke benzene under pressure. The starting product according to the technological scheme shown in the drawing is subjected to preliminary distillation and the head product obtained is processed by extractive distillation using N-formylmorpholine as a selective solvent.
The original product has the following composition, wt.%:
Hydrocarbons With 0.04
Hydrocarbons, 0.78
Methylcyclopentane 0.20
Iso-hydrocarbons
Su0.12
0.35 cyclohexane
Normal hydrocarbons Cj +
+ dimethylcyclopentane 0.16
Methylcyclohexane 0.25
Benzene75.30
Paraffin
hydrocarbons Cg 0.07
Dimethylcyclohex-san0.48
Toluene
Aromatic hydrocarbons C
eight

In part A of the experiment, the initial product is subjected to preliminary distillation at normal pressure (pressure at the head of the column is at most 1.1 atm), and the resulting head product is introduced into a series (additionally) connected column 13 for extractive distillation, which operates under pressure 1, 98 atm. In this case, there is no heat connection between the pre-distillation and the extractive distillation stage. Pure benzene contained in the form of a head product by distilling off a column (1.98 atm) contains 100 ppm. (ppm) toluene and 350 ppm non-aromatic hydrocarbons as impurities. The yield of benzene is thus 99.8%. The total heat consumption of the method is in this case
Pre-distillation
Extraction step
Total heat consumption
1440 kJ / kg benzene
920 kJ / kg benzene
2360 kJ / kg
benzene In part In the experience in the case of such
same precursor, pre-distillation is carried out under the following conditions:
Pressure at the head of the column Temperature at the head of the column
Sludge temperature
16.8 atm
209 С
28GS 1: 3.2
The operating conditions in the extractive distillation stage compared with part of experiment A changed only slightly due to the fact that, due to the high content of methylcyclohexane in the head product of preliminary distillation, the proportion of solvent used in extractive distillation increased slightly. The purity and yield of the benzene obtained in this case correspond to the results.
5 1
According to the invention, the pairs of the head product of the preliminary distillation are used to heat the column 13 of the extractive distillate, and the distant column 10, and the heat balance of the process is as follows:
Pre-distillation is 1270 kJ / kg benzene, extractive distillation stage 982 kJ / kg benzene. Compared with the preliminary distillation at normal pressure (part A), the required amount of heat (heat consumption) during preliminary distillation at constant pressure (part B), despite the slightly increased reflux number, is lower, since at the used pressure the heat of evaporation is about 30% Below, in the case of the method of work proposed in accordance with the invention, it is not necessary to add the necessary amount of heat at the extractive distillation stage in the form of a separate energy (preferably steam). This necessary amount of heat, on the contrary, is completely covered by the heat content of the vapors of the pre-distillation head product. The vapor temperature of the head product is 209 ° C and is completely sufficient. In fact, typically, only 80-90% of the vapor of the overhead product is required to heat the extraction stage. The remaining amount can be used to preheat the starting product in heat exchanger 3.
The total heat consumption for part B is therefore generally only satisfied with 1270 kJ / kg benzene. Comparing part A with part B gives that for part B only
1270-100, „
- 54l of the required amount of heat of part A. Economy is achieved, the energy is thus 46%.
Example 2. This example illustrates the production of pure benzene from fully hydrogenated pyrolysis gasoline. The initial product has: t the following composition, wt.%:
Hydrocarbons Cj
Hydrocarbons
Methylcyclopentane Hydrocarbons
iso-design C /
55®
Cyclohexane 2.05 Normal hydrocarbons Dimethylcyclopentane 2.59 Methylcyclohexane 1.05 Benzene60.30
Paraffin hydrocarbons Cg 0,99 Dimethylcyclohex-san0,96
Toluene23,97
Aromatic hydrocarbons Cg 0,20
The experiment was carried out as in the example for Part A and the preliminary distillation was carried out at normal pressure. At the same time, heat consumption is as follows;

1290 kJ / kg benzene
1000 kJ / kg benzene
2290 kJ / kg benzene
10 15 --O 25 O
0
0
252 ° C
five
The resulting pure benzene thus contained another 100 m, d, toluene and 400 m, d, non-aromatic hydrocarbons as impurities. In Part B, preliminary distillation is carried out under the following conditions:
Head pressure
columns 16.8 atm
The temperature of the head of the column
The temperature of the sump Reflux 1: 3,6 at the same time the heat consumption has the following values: Pre-distillation 1420 kJ / kg
benzene
Extractive distillation stage 1290 kJ / kg
benzene
Here, too, the heat consumption in the extraction stage is completely covered by the heat content of the vapors of the pre-distillation head product, and then for the required amount of heating with Part A, the following calculation is obtained:
1420-100
229b
thus 38%. Data of material and heat balance to examples 1 and 2 are given in table.1 5 and 2.
it is yes Yes, it’s worth it and the heat balance to (Grnberg t, Ch1sg In
62%
Heat consumption, kg / h
; Temperatura,
Nonarononic "Hydrocarbons, Crystals
BEFORE
us 2
Benzene, ias. X
Highly more non-aromatic hydrocarbons, wt.X
Toluene, mas.X
SG
arctic
hydrocarbons,
ias.h
I-formshirifoliv,
wt.X
The remainder of the test is tvp-obob- Mcnmt- «. J / hg
toooo
fashion raw materials h
10,000 32424 26740 10161 5684 32424 2280 24704 7720 190 38510 31000 75) 0 2280 ZTHD
12 209 209 209 209 209 181 209 80 80 157 192 50 281 80
1.90 2.46 2.4 "2.46 2.46 2.46
75.30 97.54 97.54 97.54 97.54 97.54
2.46 2.46 94.0
0.03
97.54 97.54 6.0 15.81 1.0 99.96
1.0
0.55 20.05
2.4 88.0
2.4
Oh, 88.0
2.20
9.6
9.6
99.0
99.00
0.586
2.204
7.342
2.46 2.46 94.0
0.03
97.54 97.54 6.0 15.81 1.0 99.96
1.0
2.4 88.0
2.4
Oh, 88.0
9.6
9.6
99.0
99.00
0.586
2.204
7.342
IS

8,960 7,389 2,808 1,571 45691227

1,571 0,586 2,204 9,528 4,582 2,808 3,861 3,481
Data of material and thermal balance for example 2, part B
Heat consumption, kg / h 100000 32784 27887 17457 4897 25657 2883 25637 7127 1153 37974 32000 5974 2883 32000
Temperature ,
WITH
60 209 209 209 209 209 120 209 80 80 168 192 50 252 80

11.07 15,53 15,53 15.53 15.53 153
60.20 84.47 84.47 84.47 84.47 84.47
Continuation of table 1
17
18
nineteen
20
22
22
24
29
28
table 2
15.53 15.53 96,00,03
84.47 84.47 4.0 16.57 1.0 99.961.0
Obave aenne
flow
on tekhiologich “s-
which
pattern
Continuation of tARL.2
29
23.97
0.20
U.78 84.52
and, 7c
0.01 84.52
0.70
0.70
83.43 99.0
99.0

0.906
9,060 7,706 4,823, 354
12 .
27
28
, 354 0,906 2,035 6,483 2,883 4,823 3,000 4,503
0.906
2,035
7,503
27
28
./
eight
17
/four
; /
J.
3
19 .29. /
2
J 25
27
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:
/and
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Compiled by G.Gul eva Editor Yu, Sereda Tekhred 3.Paliy Proofreader 0.Lugov
Order 8548/61 Circulation 379.Subscription
VNSHSHI USSR State Committee
for inventions and discoveries 113035, Moscow, Zh-35, Raushsk nab., 4/5
Branch ShSh Patent, Uzhgorod, Proektna St., 4

权利要求:
Claims (1)
[1]
METHOD FOR PRODUCING PURE BENZENE FROM HYDROCARBON MIXTURES containing aromatic hydrocarbons and a high amount of non-aromatic hydrocarbons by extractive distillation in the presence of N-formylmorpholine as a selective solvent, carried out in an extractive distillation column and a distillation column at a pressure of 1.98 atm, characterized in that in order to reduce energy consumption, the initial hydrocarbon mixture is pre-separated by distillation at pressure
16.8 atm and a top temperature of the preliminary distillation column of 209 ⁹ C, pairs of the resulting overhead product before being fed to the extractive distillation stage in the amount of May 80-90.% Are used to heat the columns at the extractive distillation stage by indirect heat exchange with complete condensation of the head product , the remaining amount of vapors of the overhead product is used to preheat the feedstock by indirect heat exchange with complete condensation of the overhead product, with reflux and tare numbers approx preliminary distillation in a column selected from the calculation, the amount of overhead product vapor was sufficient to heat the columns to the extractive distillation step.
, 1205755

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US2400370A|1943-11-11|1946-05-14|Acme Coppersmithing & Machine|Process and apparatus for producing in the pure state, butyl alcohol, acetone, and ethyl alcohol from watery solutions|

US3639497A|1968-08-22|1972-02-01|Badger Co|Extraction and multi-stage fractional distillation with indirect heat exchange of liquid and vapor process and system for recovering aromatic products|

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US4081355A|1970-08-12|1978-03-28|Krupp-Koppers Gmbh|Process for recovering highly pure aromatics from a mixture of aromatics and non-aromatics|

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DE2745672A1|1977-10-11|1979-04-12|Metallgesellschaft Ag|METHOD FOR PRODUCING AROMATE-FREE N-HEXANE|

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US4256541A|1979-05-29|1981-03-17|National Distillers And Chemical Corp.|Production of anydrous alcohol|

US4306942A|1980-06-27|1981-12-22|Raphael Katzen Associates International, Inc.|Hydrous alcohol distillation method and apparatus|

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US5124004A|1983-08-22|1992-06-23|Trustees Of Dartmouth College|Distillation process for ethanol|

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US4824527A|1986-06-10|1989-04-25|Erickson Donald C|Nested enrichment cascade distillation of unequal mixtures|

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法律状态:

优先权:

申请号 | 申请日 | 专利标题

DE19813135319|DE3135319A1|1981-09-05|1981-09-05|"METHOD FOR OBTAINING PURE AROMATES"|

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