CN104844405A - Device and method for separating pseudocumene from pseudocumene-rich material of methanol synthetic oil - Google Patents
Device and method for separating pseudocumene from pseudocumene-rich material of methanol synthetic oil Download PDFInfo
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Abstract
The invention relates to a device and a method for separating pseudocumene from pseudocumene-rich material of methanol synthetic oil. The device comprises an extraction and rectification column, a solvent recycling column, a heavy removing tower, condensers, reboilers, a cooler, a pump, and related material feeding pipelines and connecting pipelines, wherein the condensers are respectively arranged at the top parts of the extraction and rectification column, the solvent recycling column and the heavy removing tower, and the reboilers are respectively arranged at the bottoms of the extraction and rectification column, the solvent recycling column and the heavy removing tower; the raw material is connected with a lower material inlet of the extraction and rectification column; a solvent is connected with an upper material inlet of the extraction and rectification column; the top part of the extraction and rectification column is provided with n-decane, and an outlet of the bottom part of the extraction and rectification column is connected with a material inlet of the solvent recycling column; an outlet at the top part of the solvent recycling column is connected with a material inlet of the heavy removing column, and the bottom part of the solvent recycling column is used for connecting the circulating solvent to the upper material inlet of the extraction and rectification column; the top part of the heavy removing tower is provided with a pseudocumene product, and the bottom part of the heavy removing tower is provided with heavy component. The device has the advantages that by adopting the extraction and distillation technique, the relative volatilizing degrees of the n-decane and the pseudocumene are increased, and then the n-decane and the pseudocumene can be separated; by utilizing the heavy removing column, the heavy component in the pseudocumene can be removed, so as to obtain the qualified pseudocumene product.
Description
Technical field
The present invention relates to purification unsym-trimethyl benzene technical field, particularly relate in a kind of methanol-fueled CLC oil being rich in the material of unsym-trimethyl benzene and be separated pseudocumene unit and method.
Background technology
Technique for preparing gasoline by methanol makes raw material production synthetic gas with coal or Sweet natural gas usually, then uses synthesising gas systeming carbinol, finally crude carbinol is converted into stop bracket gasoline.Brown coal are one of important in the world fossil energies, 40% is accounted in coal total reserves, there is the feature of clean, low volatilization and low-sulfur, simultaneously because brown coal hydrogen richness is relatively high, easilier than other coals to liquefy, have more magnetism from this feature preparing synthetic gas, methyl alcohol, finally obtained gasoline, potentiality to be exploited is huge.
Utilize after brown coal methanol-fueled CLC oil that wherein aromaticity content is higher usually, unsym-trimethyl benzene wherein occupies very large ratio, have impact on quality of gasoline.Unsym-trimethyl benzene is a kind of important Organic Chemicals, be widely used in the fields such as synthetic resins, painting, coating, vitamin-E, medicine and makeup, be a kind of fine chemistry industry material having high added value, extraction and isolation unsym-trimethyl benzene in methanol-fueled CLC oil is just seemed very important.For applying the material obtaining being rich in unsym-trimethyl benzene after distillation operation removes C8 and following component and is rich in durol component in methanol-fueled CLC oil, wherein the content of n-decane is higher, have impact on the purity of unsym-trimethyl benzene, makes it not reach unsym-trimethyl benzene product index.Because the boiling point of n-decane and unsym-trimethyl benzene only differs from 3.44 DEG C, and n-decane and unsym-trimethyl benzene may form low azeotrope, are therefore difficult to n-decane to be separated with unsym-trimethyl benzene with conventional distillation.
Summary of the invention
The object of this invention is to provide method and the device of the feed separation purification unsym-trimethyl benzene being rich in unsym-trimethyl benzene in a kind of methanol-fueled CLC oil.For aromatic hydrocarbons and non-aromatics separation system, solvent extraction distillation technique can be adopted to be separated.Solvent extraction distillation ratio juris is: after utilizing some polar solvent to mix with hydro carbons, can reduce hydrocarbon vapours pressure, also widens the boiling-point difference of various hydro carbons simultaneously, so just can make originally can not to become can be separated with the hydro carbons that distillating method is separated.
Solvent extraction distillation method is adopted to utilize extracting rectification tower to carry out being separated n-decane and unsym-trimethyl benzene with two tower combinations of solvent recuperation in the present invention.
Technical scheme of the present invention is as follows:
Be rich in the material of unsym-trimethyl benzene in methanol-fueled CLC oil of the present invention and be separated pseudocumene unit, comprise extracting rectification tower, solvent recovery tower, weight-removing column, condenser, reboiler, water cooler, pump and relevant feedstocks pipeline and the pipeline being connected above equipment; Extracting rectification tower, solvent recovery tower and weight-removing column tower top all arrange condenser, and tower reactor all arranges reboiler; Raw material is connected to the underfeed mouth of extracting rectification tower, and solvent is connected to the upper feed inlet of extracting rectification tower, and extracting rectification column overhead is n-decane, and tower reactor outlet is connected to solvent recovery tower opening for feed; Solvent recovery tower tower top outlet is connected to weight-removing column opening for feed, and tower reactor is the upper feed inlet that circulating solvent is connected to extracting rectification tower; Weight-removing column tower top is unsym-trimethyl benzene product, and tower reactor is heavy constituent.
Be rich in methanol-fueled CLC oil of the present invention in the material of unsym-trimethyl benzene and be separated unsym-trimethyl benzene method and be: raw material (S01) enters extracting rectification tower (T1) bottom, solvent (S02) enters the top of extracting rectification tower (T1), extracting rectification column overhead gas phase (S03) enters extracting rectification column overhead condenser (E1), condensed liquid phase is through the liquid phase of extracting rectification tower reflux-withdrawal pump (P1) extraction, a part is as extracting rectification tower backflow (S04), another part is as n-decane (S05) extraction, tower reactor liquid is through the charging of extracting rectification tower tower reactor extraction pump (P2) extraction liquid (S06) as solvent recovery tower (T2), solvent recovery tower (T2) top gaseous phase (S07) enters solvent recovery tower overhead condenser (E3), condensed liquid phase is through solvent recovery tower reflux-withdrawal pump (P3) extraction liquid phase, a part is as solvent recovery tower backflow (S08), another part is as the charging (S09) of weight-removing column (T3), tower reactor liquid through solvent recovery tower tower reactor extraction pump (P4) extraction, and returns extracting rectification tower (T1) top charging through supercooler (E5) cooled circulating solvent (S10), weight-removing column (T3) top gaseous phase (S11) enters weight-removing column overhead condenser (E6), condensed liquid phase is through weight-removing column reflux-withdrawal pump (P5) extraction liquid phase, a part is as weight-removing column backflow (S12), another part is as unsym-trimethyl benzene product (S13) extraction, and weight-removing column tower reactor liquid is through weight-removing column tower reactor extraction pump (P6) extraction heavy constituent (S14).
Be rich in methanol-fueled CLC oil in the material of unsym-trimethyl benzene and be separated in unsym-trimethyl benzene method: extracting rectification pressure tower 1-101.3KPa (a), solvent is tetramethylene sulfone, tetramethylene sulfone compares 1-2 with raw materials quality, reflux ratio 1-10, solvent recuperation pressure tower 1-101.3KPa (a), reflux ratio 0.1-1, weight-removing column pressure 101-300KPa (a), reflux ratio 10-20.
Be rich in the material of unsym-trimethyl benzene in methanol-fueled CLC oil of the present invention and be separated unsym-trimethyl benzene separating and purifying method and device, its advantage is to adopt extractive distillation technology, increases the relative volatility of n-decane and unsym-trimethyl benzene, makes both reach separation.Utilize weight-removing column, remove the heavy constituent in unsym-trimethyl benzene, obtain qualified unsym-trimethyl benzene product.
Accompanying drawing explanation
Fig. 1 is separated unsym-trimethyl benzene separating and purifying method and device schematic diagram in the material being rich in unsym-trimethyl benzene in methanol-fueled CLC oil.
Equipment: T1. extracting rectification tower, T2. solvent recovery tower, T3. weight-removing column, P1. extracting rectification tower reflux-withdrawal pump, P2. extracting rectification tower tower reactor extraction pump, P3. solvent recovery tower reflux-withdrawal pump, P4. solvent recovery tower tower reactor extraction pump, P5. weight-removing column reflux-withdrawal pump, P6. weight-removing column tower reactor extraction pump, E1. extracting rectification column overhead condenser, E2. extracting rectification tower reboiler, E3. solvent recovery tower overhead condenser, E4. solvent recovery tower reboiler, E5. water cooler, E6. weight-removing column overhead condenser, E7. weight-removing column reboiler.
Logistics: S01. raw material, S02. solvent, S03. extracting rectification column overhead gas phase, S04. extracting rectification tower backflow, S05. n-decane, S06. extracting rectification tower tower reactor Produced Liquid, S07. solvent recovery tower top gaseous phase, S08. solvent recovery tower backflow, the charging of S09. weight-removing column, S10. circulating solvent, S11. weight-removing column top gaseous phase, S12. weight-removing column backflow, S13. unsym-trimethyl benzene product, S14. heavy constituent.
Embodiment
Below in conjunction with accompanying drawing, method provided by the present invention and device are further detailed.
The present invention is achieved through the following technical solutions:
Be rich in methanol-fueled CLC oil in the material of unsym-trimethyl benzene and be separated pseudocumene unit, as shown in Figure 1, comprise extracting rectification tower, solvent recovery tower, weight-removing column, condenser, reboiler, water cooler, pump and relevant feedstocks pipeline and the pipeline being connected above equipment; Extracting rectification tower, solvent recovery tower and weight-removing column tower top all arrange condenser, and tower reactor all arranges reboiler; Raw material is connected to the underfeed mouth of extracting rectification tower, and solvent is connected to the upper feed inlet of extracting rectification tower, and extracting rectification column overhead is n-decane, and tower reactor outlet is connected to solvent recovery tower opening for feed; Solvent recovery tower tower top outlet is connected to weight-removing column opening for feed, and tower reactor is the upper feed inlet that circulating solvent is connected to extracting rectification tower; Weight-removing column tower top is unsym-trimethyl benzene product, and tower reactor is heavy constituent.
Be rich in methanol-fueled CLC oil of the present invention in the material of unsym-trimethyl benzene and be separated unsym-trimethyl benzene method and be: raw material (S01) enters extracting rectification tower (T1) bottom, solvent (S02) enters the top of extracting rectification tower (T1), extracting rectification column overhead gas phase (S03) enters extracting rectification column overhead condenser (E1), condensed liquid phase is through the liquid phase of extracting rectification tower reflux-withdrawal pump (P1) extraction, a part is as extracting rectification tower backflow (S04), another part is as n-decane (S05) extraction, tower reactor liquid is through the charging of extracting rectification tower tower reactor extraction pump (P2) extraction liquid (S06) as solvent recovery tower (T2), solvent recovery tower (T2) top gaseous phase (S07) enters solvent recovery tower overhead condenser (E3), condensed liquid phase is through solvent recovery tower reflux-withdrawal pump (P3) extraction liquid phase, a part is as solvent recovery tower backflow (S08), another part is as the charging (S09) of weight-removing column (T3), tower reactor liquid through solvent recovery tower tower reactor extraction pump (P4) extraction, and returns extracting rectification tower (T1) top charging through supercooler (E5) cooled circulating solvent (S10), weight-removing column (T3) top gaseous phase (S11) enters weight-removing column overhead condenser (E6), condensed liquid phase is through weight-removing column reflux-withdrawal pump (P5) extraction liquid phase, a part is as weight-removing column backflow (S12), another part is as unsym-trimethyl benzene product (S13) extraction, and weight-removing column tower reactor liquid is through weight-removing column tower reactor extraction pump (P6) extraction heavy constituent (S14).
Be rich in methanol-fueled CLC oil in the material of unsym-trimethyl benzene and be separated in unsym-trimethyl benzene method: extracting rectification pressure tower 1-101.3KPa (a), solvent is tetramethylene sulfone, tetramethylene sulfone compares 1-2 with raw materials quality, reflux ratio 1-10, solvent recuperation pressure tower 1-101.3KPa (a), reflux ratio 0.1-1, weight-removing column pressure 101-300KPa (a), reflux ratio 10-20.
Embodiment 1
What ammonia from coal synthetic oil obtained after removing C8 and following component and being rich in durol material is rich in unsym-trimethyl benzene material composition in table 1.
Table 1 is rich in the material composition of unsym-trimethyl benzene
Utilize the material in table 1 to form, separating-purifying is carried out to the unsym-trimethyl benzene be wherein rich in, the separation process of unsym-trimethyl benzene and device in this example, as shown in Figure 1.In this example, make solvent with tetramethylene sulfone, extracting rectification pressure tower 1KPa (a), tetramethylene sulfone and raw materials quality than 1, reflux ratio 10, solvent recuperation pressure tower 1KPa (a), reflux ratio 0.1, weight-removing column pressure 101KPa (a), reflux ratio 10; The unsym-trimethyl benzene rate of recovery finally obtained is 99.9%, and the quality purity of unsym-trimethyl benzene is 98.9%, solvent consumption 0.215g/h.
Embodiment 2
This example Raw component is identical with embodiment 1.The separation process of unsym-trimethyl benzene and device, as shown in Figure 1.In this example, make solvent with tetramethylene sulfone, extracting rectification pressure tower 101.3KPa (a), tetramethylene sulfone and raw materials quality than 2, reflux ratio 1, solvent recuperation pressure tower 101.3KPa (a), reflux ratio 1, weight-removing column pressure 300KPa (a), reflux ratio 20; The unsym-trimethyl benzene rate of recovery finally obtained is 99.8%, and the quality purity of unsym-trimethyl benzene is 99.0%, solvent consumption 0.64g/h.
Embodiment 3
This example Raw component is identical with embodiment 1.The separation process of unsym-trimethyl benzene and device, as shown in Figure 1.In this example, make solvent with tetramethylene sulfone, extracting rectification pressure tower 50KPa (a), tetramethylene sulfone and raw materials quality than 1.5, reflux ratio 5, solvent recuperation pressure tower 50KPa (a), reflux ratio 0.5, weight-removing column pressure 200KPa (a), reflux ratio 15; The unsym-trimethyl benzene rate of recovery finally obtained is 99.6%, and the quality purity of unsym-trimethyl benzene is 98.8%, solvent consumption 0.097g/h.
Claims (6)
1. be rich in the material of unsym-trimethyl benzene in methanol-fueled CLC oil and be separated a pseudocumene unit, comprise extracting rectification tower, solvent recovery tower, weight-removing column, condenser, reboiler, water cooler, pump and relevant feedstocks pipeline and the pipeline being connected above equipment; Extracting rectification tower, solvent recovery tower and weight-removing column tower top all arrange condenser, and tower reactor all arranges reboiler; Raw material is connected to the underfeed mouth of extracting rectification tower, and solvent is connected to the upper feed inlet of extracting rectification tower, and extracting rectification column overhead is n-decane, and tower reactor outlet is connected to solvent recovery tower opening for feed; Solvent recovery tower tower top outlet is connected to weight-removing column opening for feed, and tower reactor is the upper feed inlet that circulating solvent is connected to extracting rectification tower; Weight-removing column tower top is unsym-trimethyl benzene product, and tower reactor is heavy constituent.
2. adopt device according to claim 1 to carry out being rich in methanol-fueled CLC oil in the material of unsym-trimethyl benzene and be separated unsym-trimethyl benzene method, it is characterized in that: raw material (S01) enters extracting rectification tower (T1) bottom, solvent (S02) enters the top of extracting rectification tower (T1), extracting rectification column overhead gas phase (S03) enters extracting rectification column overhead condenser (E1), condensed liquid phase is through the liquid phase of extracting rectification tower reflux-withdrawal pump (P1) extraction, a part is as extracting rectification tower backflow (S04), another part is as n-decane (S05) extraction, tower reactor liquid is through the charging of extracting rectification tower tower reactor extraction pump (P2) extraction liquid (S06) as solvent recovery tower (T2), solvent recovery tower (T2) top gaseous phase (S07) enters solvent recovery tower overhead condenser (E3), condensed liquid phase is through solvent recovery tower reflux-withdrawal pump (P3) extraction liquid phase, a part is as solvent recovery tower backflow (S08), another part is as the charging (S09) of weight-removing column (T3), tower reactor liquid through solvent recovery tower tower reactor extraction pump (P4) extraction, and returns extracting rectification tower (T1) top charging through supercooler (E5) cooled circulating solvent (S10), weight-removing column (T3) top gaseous phase (S11) enters weight-removing column overhead condenser (E6), condensed liquid phase is through weight-removing column reflux-withdrawal pump (P5) extraction liquid phase, a part is as weight-removing column backflow (S12), another part is as unsym-trimethyl benzene product (S13) extraction, and weight-removing column tower reactor liquid is through weight-removing column tower reactor extraction pump (P6) extraction heavy constituent (S14).
3. method as claimed in claim 2, is characterized in that extracting rectification pressure tower 1-101.3KPa (a).
4. method as claimed in claim 2, is characterized in that solvent is tetramethylene sulfone, tetramethylene sulfone and raw materials quality than 1-2, reflux ratio 1-10.
5. method as claimed in claim 2, is characterized in that solvent recuperation pressure tower 1-101.3KPa (a), reflux ratio 0.1-1.
6. method as claimed in claim 2, is characterized in that weight-removing column pressure 101-300KPa (a), reflux ratio 10-20.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101445420A (en) * | 2008-12-25 | 2009-06-03 | 上海奥韦通工程技术有限公司 | Process for preparing benzene aromatic hydrocarbon by crude benzene |
| CN203960085U (en) * | 2014-06-26 | 2014-11-26 | 天津大学 | From methyl alcohol synthetic oil, extract the device of durol |
| CN104557457A (en) * | 2014-11-28 | 2015-04-29 | 天津大学 | Reactive distillation method and reactive distillation device for producing butanol by hydrogenating butyraldehyde |
| CN204714722U (en) * | 2015-05-14 | 2015-10-21 | 天津大学 | Be rich in methanol-fueled CLC oil in the material of unsym-trimethyl benzene and be separated pseudocumene unit |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101445420A (en) * | 2008-12-25 | 2009-06-03 | 上海奥韦通工程技术有限公司 | Process for preparing benzene aromatic hydrocarbon by crude benzene |
| CN203960085U (en) * | 2014-06-26 | 2014-11-26 | 天津大学 | From methyl alcohol synthetic oil, extract the device of durol |
| CN104557457A (en) * | 2014-11-28 | 2015-04-29 | 天津大学 | Reactive distillation method and reactive distillation device for producing butanol by hydrogenating butyraldehyde |
| CN204714722U (en) * | 2015-05-14 | 2015-10-21 | 天津大学 | Be rich in methanol-fueled CLC oil in the material of unsym-trimethyl benzene and be separated pseudocumene unit |
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