CN104058916A - Morpholine-class mixed solvent for isolating arene through extraction and rectification and method for isolating arene - Google Patents
Morpholine-class mixed solvent for isolating arene through extraction and rectification and method for isolating arene Download PDFInfo
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- CN104058916A CN104058916A CN201410309452.8A CN201410309452A CN104058916A CN 104058916 A CN104058916 A CN 104058916A CN 201410309452 A CN201410309452 A CN 201410309452A CN 104058916 A CN104058916 A CN 104058916A
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Abstract
The invention discloses a morpholine-class mixed solvent for isolating arene through extraction and rectification and a method for isolating the arene. The morpholine-class mixed solvent is formed by NFM and NAM in a mixed mode, wherein the weight percentage of one kind of the NFM and the NAM to the mixed solvent ranges from 5% to 95%. Devices used in the technology for isolating the arene through extraction and rectification include an extracting and rectifying tower comprising a reboiler and a condenser, a solvent recycling tower, a preheater, pipes, a pump, a storage tank, an instrument and the like. According to application research of the morpholine-class mixed solvent in the technology for isolating the arene through extraction and rectification, it is found that the solidifying point of a pure solvent can be reduced through the morpholine-class mixed solvent, and the requirement of the existing arene extraction technology can be met. Compared with the pure solvent, the mixed solvent is good in selectivity, low in solidifying point and particularly suitable for winter or cold regions; when feeding is carried out through the pump, a heat tracing device does not need to be additionally arranged on the pipes and the raw material tank, energy consumption is low, and the morpholine-class mixed solvent and the method are convenient to operate and use.
Description
Technical field
The invention belongs to solvent preparation field, be specially a kind of zero pour that reduces neat solvent, overcome because of weather reason, for the morpholine class mixed solvent of separation of extractive distillation aromatic hydrocarbons and utilize the method for this mixed solvent aromatics separation.
Background technology
From petroleum benzene or coking benzene, aromatics separation is that benzene,toluene,xylene mainly contains two class methods.One class is liquid-liquid extraction process, and this method is in fact the combined process of the extracting of liquid-liquid and solvent recuperation.Another kind of is extraction fractional distillation.Compared with liquid-liquid extraction process, extraction fractional distillation has that flow process is simple, simple to operate, facility investment is supported, low power consumption and other advantages, is particularly suitable for reclaiming aromatic hydrocarbons from the hydrocarbon mixture of high aromaticity content.This method is utilized the impact of solvent on the each component relative volatility of hydro carbons, is operated and is realized aromatic hydrocarbons and separate with non-aromatics by extracting rectifying.When operation, raw material adds from extractive distillation column middle part, and solvent adds from the top of tower, non-aromatics is from removed overhead, the rich solvent containing aromatic hydrocarbons obtaining at the bottom of tower enters solvent recovery tower again and carries out rectifying, separates and obtains aromatic hydrocarbons and lean solvent, and lean solvent returns to extractive distillation column and recycles after heat exchange.Solvent used is generally simple glycols, tetramethylene sulfone, N-Methyl pyrrolidone (NMP), NFM etc.
It is acid that glycols and tetramethylene sulfone kind solvent all show slightly, and for keeping the stable of circulating solvent potential of hydrogen, prevents equipment corrosion, needs regularly from backflow aromatic hydrocarbons tank, to add the monoethanolamine of some amount.Glycols and tetramethylene sulfone kind solvent boiling point are very high, and recovery and regeneration assisting workflows are long, and under high service temperature, energy and solvent consumption are larger.Glycols and tetramethylene sulfone kind solvent thermal stability are poor, need nitrogen protection in use.Tetramethylene sulfone is also easy to foaming in operational process, brings certain difficulty to operation.
NMP, in arene extracting process, degrades more serious, in product, can contain organonitrogen, and aromatic hydrocarbon product is had to impact, and in the time processing benzene cut, toluene fraction and dimethylbenzene cut, the consumption meeting of general facilities is with heavy the enlarging markedly of change of raw material.
Patent EP0329958 is the extractive distillation Morphylane technique of Krupp Koppers (K.K) company exploitation, adopt NFM solvent, can obtain high-quality benzene and toluene simultaneously, technical process is simple, solvent-oil ratio is few, reclaim easyly, its selectivity is obviously better than NMP, can reduce 20%-40% with tetramethylene sulfone technique phase specific energy consumption.In view of this, NFM solvent is a kind of good aromatic hydrocarbon extraction solvent of generally acknowledging so far.
Summary of the invention
The object of the present invention is to provide the zero pour that can reduce neat solvent NFM, and do not affect the morpholine class mixed solvent of its a kind of separation of extractive distillation aromatic hydrocarbons to aromatic hydrocarbons/non-aromatics separating effect in aromatics extraction process.
Another object of the present invention is for providing a kind of method of utilizing this morpholine class mixed solvent aromatics separation.
The object of the invention realizes by following technical proposals:
For a morpholine class mixed solvent for separation of extractive distillation aromatic hydrocarbons, this morpholine class mixed solvent comprises NFM and NAM, and in quality percentage composition, NAM shared quality percentage composition in mixed solvent is 5～95%; The shared quality percentage composition of NFM is 5～95%.
As preferably, comprise NFM and NAM for the morpholine class mixed solvent of separation of extractive distillation aromatic hydrocarbons, in quality percentage composition, NAM shared quality percentage composition in mixed solvent is 10～90%; The shared quality percentage composition of NFM is 10～90%.
Further preferred, comprise NFM and NAM for the morpholine class mixed solvent of separation of extractive distillation aromatic hydrocarbons, in quality percentage composition, NFM shared quality percentage composition in mixed solvent is 50%; The shared quality percentage composition of NAM is 50%.The mixed solvent that the quality percentage composition that preferably the quality percentage composition of NFM is 60%, NAM is 40%.The mixed solvent that the quality percentage composition that preferably the quality percentage composition of NFM is 70%, NAM is 30%.The mixed solvent that the quality percentage composition that preferably the quality percentage composition of NFM is 80%, NAM is 20%.
A method of utilizing morpholine class mixed extractant solvent rectifying and separating aromatic hydrocarbons, comprises the steps:
Hydrocarbon mixture is introduced from the middle part of extractive distillation column, solvent is introduced from the top of extractive distillation column, tower top obtains non-aromatics, the rich solvent that is rich in aromatic hydrocarbons of discharging at the bottom of tower is introduced solvent recovery tower and is carried out rectifying from middle part, separation obtains aromatic hydrocarbons and lean solvent, then the lean solvent introducing extractive distillation column obtaining after separating is recycled.The pressure of described extractive distillation column is 0.08MPa～0.18MPa, and it is 90 DEG C～120 DEG C that solvent enters tower temperature, and tower top temperature is 80 DEG C～120 DEG C, and column bottom temperature is 150 DEG C～180 DEG C, solvent ratio 4～6, reflux ratio 0.1～1.0.The tower top pressure of described solvent recovery tower is 0.04MPa～0.05MPa, and column bottom temperature is 180 DEG C～190 DEG C, and trim the top of column is than 0.5～1.0.
In extracting rectifying, solvent plays decisive role to the economy of product purity, yield and process.NFM as a kind of nontoxic, corrosion-free, chemical stability is good, low aromatic hydrocarbon extraction solvent consumes energy, subject matter is that its zero pour is higher, it is 23 DEG C, easily freeze during lower than 23 DEG C at temperature, when use, not only with steaming out head tank and pipeline, also to increase heating device, bring much more extremely inconvenience to operation, once and NFM in pipeline, solidify, can have a strong impact on normal production.The object of this patent is by adding other component to reduce the zero pour of NFM, overcome because solvent solidifies and bring operational inconvenience, and bring into play to greatest extent the effect of extracting rectifying section selective solvent aromatics separation and non-aromatics, improve selectivity and the operational stability of extraction distillation solvent.The morpholine class mixed solvent that the present invention uses is in NFM, to add the NAM close with NFM character.NAM with NFM is equally a kind of solvent of excellent property, corrosion-free, stable chemical performance, and decomposition temperature is to be also greater than 220 DEG C, and boiling point is 246 DEG C, and only high 3 DEG C than NFM, zero pour is 10 DEG C, lower 13 DEG C than NFM.
Find after deliberation, the morpholine class mixed solvent that NFM and NAM are mixed to form by a certain percentage, its zero pour can reach-23 DEG C, and have good aromatic hydrocarbons separation performance, in separation of extractive distillation aromatics process, reduce heating device, solidified the various inconvenience that bring thereby reduced because of neat solvent.
The raw material of separation of extractive distillation provided by the invention is petroleum benzene or coking benzene.
Compared with prior art, beneficial effect of the present invention is:
(1), the morpholine class mixed solvent of separation of extractive distillation aromatic hydrocarbons provided by the invention, zero pour scope is-23～23 DEG C.
(2), the advantage of morpholine class mixed solvent is that viscosity is little, in tower substantially without foamed phenomenon, zero pour is low, in winter or cold district, be difficult for crystallization freezing, pipeline, pump, storage tank are not needed to steam heating and extra heating device, isolated benzene content >=99.95% on extractive distillation column, process cost is low.
Brief description of the drawings
Fig. 1 is the freezing point curve figure of NFM/NAM mixed solvent;
Fig. 2 is the process flow sheet of separation of extractive distillation aromatic hydrocarbons.
Embodiment
For a morpholine class mixed solvent for separation of extractive distillation aromatic hydrocarbons, this morpholine class mixed solvent comprises NFM and NAM, and in quality percentage composition, NAM shared quality percentage composition in mixed solvent is 5～95%; The shared quality percentage composition of NFM is 5～95%.
As preferably, NAM shared quality percentage composition in mixed solvent is 10～90%; The shared quality percentage composition of NFM is 10～90%.Further preferred, NFM shared quality percentage composition in mixed solvent is 50%; The shared quality percentage composition of NAM is 50%.The mixed solvent that the quality percentage composition that preferably the quality percentage composition of NFM is 60%, NAM is 40%.The mixed solvent that the quality percentage composition that preferably the quality percentage composition of NFM is 70%, NAM is 30%.The mixed solvent that the quality percentage composition that preferably the quality percentage composition of NFM is 80%, NAM is 20%.
A method of utilizing morpholine class mixed extractant solvent rectifying and separating aromatic hydrocarbons, comprises the steps:
Hydrocarbon mixture is introduced from the middle part of extractive distillation column, solvent is introduced from the top of extractive distillation column, tower top obtains non-aromatics, the rich solvent that is rich in aromatic hydrocarbons of discharging at the bottom of tower is introduced solvent recovery tower and is carried out rectifying from middle part, separation obtains aromatic hydrocarbons and lean solvent, then the lean solvent introducing extractive distillation column obtaining after separating is recycled.The pressure of described extractive distillation column is 0.08MPa～0.18MPa, and it is 90 DEG C～120 DEG C that solvent enters tower temperature, and tower top temperature is 80 DEG C～120 DEG C, and column bottom temperature is 150 DEG C～180 DEG C, solvent ratio 4～6, reflux ratio 0.1～1.0.The tower top pressure of described solvent recovery tower is 0.04MPa～0.05MPa, and column bottom temperature is 180 DEG C～190 DEG C, and trim the top of column is than 0.5～1.0.
The method of separation of extractive distillation aromatic hydrocarbons, its process flow sheet is shown in accompanying drawing 2, aromatic hydrocarbons/non-aromatics 3 to be separated is added by extractive distillation column 1 middle part, morpholine class mixed solvent 4 is added by the top of 1 tower, non-aromatics 7 is from the top extraction of 1 tower, in the solvent recovery tower 2 connecing after the solvent (rich mixed solvent 8) that contains aromatic hydrocarbons causes from the bottom extraction of 1 tower, by distillation, aromatic hydrocarbons is separated with rich mixed solvent, aromatic hydrocarbons 5 is from 2 column overhead extraction, poor mixed solvent 6, from 2 tower tower reactor extraction, is reintroduced back to again 1 tower and is recycled.
Below in conjunction with embodiment, the present invention is described in further detail.
But this should be interpreted as to the scope of the above-mentioned theme of the present invention only limits to following embodiment.
Embodiment 1:
The raw material of separation of extractive distillation aromatic hydrocarbons is C in petroleum benzene
6～8hydrocarbon mixture, specifically form in table 1;
Morpholine class mixed solvent used is NFM and proportionally 6:4 (quality %) mixing of NAM, and the zero pour of this mixed solvent is-11 DEG C;
The method of separation of extractive distillation aromatic hydrocarbons, as shown in Figure 2, extractive distillation column used (1 tower) and solvent recovery tower (2 tower) they are all packing tower to its process flow sheet: material stainless steel, tower diameter Φ 20mm, filler is Stainless Steel Cloth filler; Two towers are adiabatic heat-insulation;
Carry out separation of extractive distillation aromatic hydrocarbons by the flow process shown in Fig. 2.In extractive distillation column, solvent ratio is 5, and reflux ratio is 0.5, and it is 110 DEG C that solvent enters tower temperature, and tower top temperature is 101 DEG C, tower top pressure 0.08MPa, and column bottom temperature is 170 DEG C; In solvent recovery tower, reflux ratio 0.8, tower top pressure 0.04MPa, 190 DEG C of column bottom temperatures.
Separation of extractive distillation aromatic hydrocarbons the results are shown in Table 2.
Embodiment 2:
Carry out the operation of separation of extractive distillation aromatic hydrocarbons by raw material composition and the identical processing condition of example 1, different is that morpholine class mixed solvent used is NFM and proportionally 9:1 (quality %) mixing of NAM, and the zero pour of this mixed solvent is 17 DEG C; Separation of extractive distillation aromatic hydrocarbons the results are shown in Table 2.
Embodiment 3:
Carry out the operation of separation of extractive distillation aromatic hydrocarbons by raw material composition and the identical processing condition of example 1, different is that morpholine class mixed solvent used is NFM and proportionally 1:9 (quality %) mixing of NAM, and the zero pour of this mixed solvent is-6 DEG C; Separation of extractive distillation aromatic hydrocarbons the results are shown in Table 2.
Comparative example:
Carry out the operation of separation of extractive distillation aromatic hydrocarbons by raw material composition and the identical processing condition of example 1, different is that solvent used is NFM neat solvent, and separation of extractive distillation aromatic hydrocarbons the results are shown in Table 2.
The feed composition of table 1 separation of extractive distillation aromatic hydrocarbons
As shown in Table 2, choose identical raw material composition, identical extraction rectification technique condition, just solvent difference, the isolated aromatic hydrocarbon product yield of NFM/NAM morpholine class mixed solvent (example 1) institute that the present invention uses and purity and the pure NFM solvent of use (comparative example) suitable, and the zero pour of morpholine class mixed solvent (11 DEG C) has also reduced by 34 DEG C than pure NFM solvent (23 DEG C), can adapt to better winter or cold district condition, without increasing heating device, process cost is lower.
The morpholine class mixed solvent of use-case 2 and example 3 isolated aromatic hydrocarbon product yield and purity also with use pure NFM solvent (comparative example) quite, under normal weather, use without any problem, just zero pour does not likely reach the requirement of cold district, therefore in use, according to field condition, can suitably adjust mixed solvent proportioning.
Claims (9)
1. a morpholine class mixed solvent for separation of extractive distillation aromatic hydrocarbons, is characterized in that: this morpholine class mixed solvent comprises NFM and NAM, and in quality percentage composition, NFM shared quality percentage composition in mixed solvent is 5～95%; The shared quality percentage composition of NAM is 5～95%.
2. the morpholine class mixed solvent of separation of extractive distillation aromatic hydrocarbons according to claim 1, is characterized in that: this morpholine class mixed solvent comprises NFM and NAM, and in quality percentage composition, NFM shared quality percentage composition in mixed solvent is 10～90%; The shared quality percentage composition of NAM is 10～90%.
3. the morpholine class mixed solvent of separation of extractive distillation aromatic hydrocarbons according to claim 1, is characterized in that: this morpholine class mixed solvent comprises NFM and NAM, and in quality percentage composition, NFM shared quality percentage composition in mixed solvent is 50%; The shared quality percentage composition of NAM is 50%.
4. the morpholine class mixed solvent of separation of extractive distillation aromatic hydrocarbons according to claim 1, is characterized in that: this morpholine class mixed solvent comprises NFM and NAM, and in quality percentage composition, NFM shared quality percentage composition in mixed solvent is 60%; The shared quality percentage composition of NAM is 40%.
5. the morpholine class mixed solvent of separation of extractive distillation aromatic hydrocarbons according to claim 1, is characterized in that: this morpholine class mixed solvent comprises NFM and NAM, and in quality percentage composition, NFM shared quality percentage composition in mixed solvent is 70%; The shared quality percentage composition of NAM is 30%.
6. the morpholine class mixed solvent of separation of extractive distillation aromatic hydrocarbons according to claim 1, is characterized in that: this morpholine class mixed solvent comprises NFM and NAM, and in quality percentage composition, NFM shared quality percentage composition in mixed solvent is 80%; The shared quality percentage composition of NAM is 20%.
7. utilize the method for claim 1 to the separation of extractive distillation aromatic hydrocarbons described in any one claim in claim 3, it is characterized in that comprising the steps:
Hydrocarbon mixture is introduced from the middle part of extractive distillation column, morpholine class mixed solvent is introduced from the top of extractive distillation column, tower top obtains non-aromatics, the rich solvent that is rich in aromatic hydrocarbons of discharging at the bottom of tower is introduced solvent recovery tower and is carried out rectifying from middle part, separation obtains aromatic hydrocarbons and lean solvent, then the lean solvent introducing extractive distillation column obtaining after separating is recycled.
8. the method for separation of extractive distillation aromatic hydrocarbons according to claim 4, it is characterized in that: the pressure of described extractive distillation column is 0.08MPa～0.18MPa, it is 90 DEG C～120 DEG C that solvent enters tower temperature, tower top temperature is 80 DEG C～120 DEG C, column bottom temperature is 150 DEG C～180 DEG C, solvent ratio 4～6, reflux ratio 0.1～1.0.
9. the method for separation of extractive distillation aromatic hydrocarbons according to claim 5, is characterized in that: the tower top pressure of described solvent recovery tower is 0.04 MPa～0.05 MPa, and column bottom temperature is 180 DEG C～190 DEG C, and trim the top of column is than 0.5～1.0.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110683934A (en) * | 2019-10-25 | 2020-01-14 | 许柏文 | Method and system for purifying vinyl chloride monomer |
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| US3755154A (en) * | 1969-12-10 | 1973-08-28 | Nissan Chemical Ind Ltd | Separation of hydrocarbons from mixture thereof |
| CN1218711A (en) * | 1997-12-05 | 1999-06-09 | 克鲁普犹德有限公司 | Process for removal of CO2 and sulphur compounds from industrial gases |
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Application publication date: 20140924 |