CN103232317A - Aromatic hydrocarbon purification apparatus and process used in hydrofining of coking crude benzene - Google Patents

Aromatic hydrocarbon purification apparatus and process used in hydrofining of coking crude benzene Download PDF

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Publication number
CN103232317A
CN103232317A CN2013101166546A CN201310116654A CN103232317A CN 103232317 A CN103232317 A CN 103232317A CN 2013101166546 A CN2013101166546 A CN 2013101166546A CN 201310116654 A CN201310116654 A CN 201310116654A CN 103232317 A CN103232317 A CN 103232317A
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tower
liquid
aromatic hydrocarbons
extractive distillation
aromatic hydrocarbon
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CN2013101166546A
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董宏光
胡定华
白滨
赵国强
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Dalian University of Technology
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Dalian University of Technology
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Abstract

The invention provides an aromatic hydrocarbon purification apparatus and process used in hydrofining of coking crude benzene. The apparatus comprises an extractive distillation tower, a liquid-liquid extraction tower, an aromatic hydrocarbon stripping tower, a crude benzene preheater, a hydrogenated oil preheater, a cooler, an air cooler, a raw material mixer, a discharging mixer and a distributor. The process comprises the following steps: allowing raw hydrogenated oil and a poor solvent N-formyl morpholine to enter into the extractive distillation tower, coupling a gas phase and a liquid phase in the extractive distillation tower and the liquid-liquid extraction tower, extracting a gas phase at a side line of a distillation section of the extractive distillation tower, mixing the gas phase with a tower top discharge, cooling an obtained mixture and allowing the mixture to enter into the liquid-liquid extraction tower for separation into two phases; re-introducing an aromatic hydrocarbon-rich heavy phase into the top of the extractive distillation tower as reflux, with an aromatic hydrocarbon-poor light phase mainly being non-aromatic hydrocarbons; and allowing a rich solvent at the bottom of the extractive distillation tower to enter into the aromatic hydrocarbon stripping tower for separation, wherein pure aromatic hydrocarbon is obtained at the top of the aromatic hydrocarbon stripping tower, and the poor solvent N-formyl morpholine is obtained at the bottom of the aromatic hydrocarbon stripping tower and is recycled. In the flow path of the process, process system engineering methodology is employed for realizing integration of mass and heat and optimization of a comprehensive heat exchange network, thereby realizing recovery of waste heat, improvement of a separation effect of aromatic hydrocarbon and reduction in operating cost.

Description

The aromatic hydrocarbons purifying plant and the technology that are used for hydrofining coking crude benzene
Technical field
The invention belongs to petrochemical industry, relate to a kind of aromatic hydrocarbons purifying plant and technology for hydrofining coking crude benzene, is solvent with the N-N-formyl morpholine N-, separates purification aromatic hydrocarbons from aromatic hydrocarbons and non-aromatics mixture.
Background technology
Industrial solvent for the aromatic hydrocarbons extracting has N-N-formyl morpholine N-, tetramethylene sulfone and N-Methyl pyrrolidone etc. at present.N-N-formyl morpholine N-selectivity and solvability are good, and many remarkable advantages such as its corresponding extraction process has that solvent consumption is few, energy consumption is low, product purity and yield height are so use comparatively extensive.According to the unit operation feature, the aromatic hydrocarbons extracting can be divided into liquid-liquid extraction and extracting rectifying.Liquid-liquid extraction is the unit operation that utilizes stock liquid component dissolubility difference and realizing in solvent to separate, and is applicable to the reformate raw material that non-aromatics content is higher; Extracting rectifying is to change the stock blend relative volatility and realize the unit operation that separates being applicable to the hydrogenated oil raw material that aromatic hydrocarbons purity is higher by adding solvent.Use the method for liquid-liquid extraction, separating effect and the rate of recovery of aromatic hydrocarbons are relatively poor; Use the method for extracting rectifying, the solvent usage quantity is big, and energy consumption is higher.Liquid liquid extraction plant generally includes extraction tower, stripping tower, non-aromatics water wash column, recovery tower, water separation column etc.
The existing processes technology mainly contains following several:
Aromatic hydrocarbons extractive distillation SED (the Sulfolane Extractive Distillation) technology of petrochemical complex academy of sciences exploitation, the patent No. is CN1393507, chooses the tetramethylene sulfone double solvents, can obtain the aromatic hydrocarbons of higher degree, but its aromatic recovery rate is lower.And then exploitation N-N-formyl morpholine N-is the solvent arene extracting process, improved separating effect, but solvent load and energy consumption is bigger.
Some extracting rectifying arene extracting process have been developed in UHDE's application.US Patent No. Patent Number 4081355 discloses a kind of method that reclaims high purity aromatic hydrocarbons from contain aromatic hydrocarbons and non-aromatics mixture, raw material is gone through extraction tower, extractive distillation column, stripping tower, water separation column and is obtained high purity aromatic hydrocarbons, and solvent is the N-N-formyl morpholine N-.Many covering devices are at home and abroad gone into operation, and have created considerable economic benefit.US Patent No. Patent Number 6514387 discloses a kind of partition tower apparatus, and it assembles a partition tower with extractive distillation column, raw material recovery tower, has realized the integrated of quality and energy.
US Patent No. Patent Number 3944483, US Patent Number 4488936, US Patent Number 4776927 etc. all carry out associated description to the aromatic hydrocarbons extraction technique, and progressively to the prior art transformation, but all do not relate to according to component changes in distribution in the operating unit, and respond different separation method coupled configuration, and then improve aromatic hydrocarbons separating effect combination process.
Summary of the invention
The invention provides aromatic hydrocarbons purifying plant and technology for hydrofining coking crude benzene, adopt N-N-formyl morpholine N-solvent, the method that is coupled by extracting rectifying and liquid-liquid extraction gas-liquid, thus improve the aromatic hydrocarbons separating effect, and reduce process cost.
In the coking crude benzene hydrogenation technique, aromaticity content is usually greater than 90% at the bottom of the preliminary fractionator, and this hydrogenated oil is not suitable for liquid-liquid extraction, but can take extracting rectifying.Extractive distillation column from the bottom of the tower to cat head, aromaticity content progressively reduces, especially rectifying section is formed the distribution abrupt change, its balance system is more suitable for liquid-liquid extraction to be separated.Therefore, extractive distillation column and liquid-liquid extraction tower gas-liquid are coupled in this technology, the extraction of extractive distillation column rectifying section side line gas phase, mix aromaticity content lower (less than 70%) in its component distribution of back with the cat head discharging, preferablyly take liquid-liquid extraction operation, enter that to be separated into rich aromatic hydrocarbons heavy phase behind the liquid-liquid extraction tower mutually light with poor aromatic hydrocarbons.Rich aromatic hydrocarbons heavy phase is introduced the extracting rectifying cat head again as backflow, and poor aromatic hydrocarbons gently is mainly non-aromatics in mutually, enters downstream section and handles.
This flow process adopts process system engineering methodology to realize that the mass-heat quantity set becomes, be coupled by extracting rectifying and liquid-liquid extraction gas-liquid, not only improve aromatic hydrocarbons and non-aromatics separating effect, improve aromatic recovery rate and purity simultaneously, and reduce solvent when condenser and reboiler.Simultaneously, the optimization synthesis heat exchanger network is realized that waste heat recovery, branch's aromatic hydrocarbons are carried and is heated up in a steamer lean solvent at the bottom of the tower, one preheating material crude benzol, and another is as extracting rectifying tower bottom reboiler thermal source, and then the preheating material hydrogenated oil, thereby reduces plant energy consumption.
Technical scheme of the present invention is as follows:
A kind of aromatic hydrocarbons purifying plant for hydrofining coking crude benzene, comprising that extractive distillation column, liquid-liquid extraction tower, aromatic hydrocarbons are carried heats up in a steamer tower, crude benzol preheater, hydrogenated oil preheater, water cooler, air cooler, material mixer, goes out feed mixer and divider.Material mixer links to each other with the extractive distillation column side line, extracting rectifying top of tower and rectifying section discharging side line all with go out feed mixer and link to each other, be provided with water cooler after going out feed mixer, water cooler connects liquid-liquid extraction tower bottom opening for feed, liquid-liquid extraction tower bottom discharge port links to each other with the extracting rectifying top of tower again, extracting rectifying tower bottom and aromatic hydrocarbons are carried and are heated up in a steamer the tower opening for feed and link to each other, aromatic hydrocarbons is carried and is heated up in a steamer tower bottom connection divider, export distributor is divided into two-way and connects: after (1) connected the crude benzol preheater, the outlet of crude benzol preheater connected the liquid-liquid extraction top of tower again; (2) connect extractive distillation column reboiler, hydrogenated oil preheater, air cooler, material mixer successively by connection line.
Its technological process is as follows:
(1) enters extractive distillation column after raw material hydrogenated oil and the heat exchange of lean solvent N-N-formyl morpholine N-, tower top pressure is 10-80kPa, balance progression is 25-50, solvent ratio is 4-8, the hydrogenated oil feed entrance point is the 8-12 level, and N-N-formyl morpholine N-feed entrance point is the 2-5 level, the place's side line gas phase extraction of rectifying section 1-5 level, the rich aromatic hydrocarbons heavy phase of liquid-liquid extraction tower enters the extracting rectifying cat head and crosses cold reflux, and double tower coupling reflux ratio is 0.5-0.9.
(2) after extractive distillation column ejects material and the gas phase side line mixes, be cooled to 30 ℃-50 ℃, enter at the bottom of the liquid-liquid extraction tower, liquid-liquid extraction tower counter-flow atmospheric operation; Balance progression is 4-8, and service temperature is 20 ℃-60 ℃, and extraction agent is the N-N-formyl morpholine N-, and solvent ratio is 3-5.Extraction phase is respectively with extracting phase: be that the rich aromatic hydrocarbons heavy phase of solvent is mutually light with the poor aromatic hydrocarbons that is solvent with the non-aromatics with the N-N-formyl morpholine N-.Wherein rich aromatic hydrocarbons heavy phase enters the extracting rectifying cat head, crosses cold reflux as rectifying section, and poor aromatic hydrocarbons gently is mainly non-aromatics in mutually, enters downstream section and handles.
(3) consist of N-N-formyl morpholine N-and aromatic hydrocarbons at the bottom of the extractive distillation column, rich solvent enters aromatic hydrocarbons and carries and heat up in a steamer tower and separate.Aromatic hydrocarbons is carried and is heated up in a steamer the tower vacuum operating, and balance progression is 10-20, and reflux ratio is 0.5-1, and the rich solvent feed entrance point is the 4-7 level.Cat head obtains pure aromatics, is that lean solvent N-N-formyl morpholine N-recycles at the bottom of the tower.
(4) lean solvent N-N-formyl morpholine N-is divided into the two-way circulation, and allocation proportion is 1:8-10, introduces the liquid-liquid extraction tower after the one heat exchange, returns extractive distillation column after another heat exchange.The N-N-formyl morpholine N-has small loss in the working cycle, replenishes a small amount of novel solvent at the extracting rectifying cat head.
Compare with existing flow process, aromatic hydrocarbons purity of the present invention reaches more than 99.7%, and the rate of recovery reaches more than 99.9%.Solvent ratio reduces more than 10%, and cold and hot general facilities consumption reduces, and recovery of heat increases more than 7%.
Description of drawings
Fig. 1 is aromatic hydrocarbons extractor structural representation.
Fig. 2 is the process flow sheet of aromatic hydrocarbons extracting.
Among the figure: 1 air cooler; 2 hydrogenated oil preheaters; 3 material mixers; 4 extractive distillation columns; 5 reboilers; 6 go out feed mixer; 7 water coolers; 8 liquid-liquid extraction towers; 9 aromatic hydrocarbons are carried and are heated up in a steamer tower; 10 dividers; 11 crude benzol preheaters.
Embodiment
Below in conjunction with technical scheme and accompanying drawing, be described in detail the specific embodiment of the present invention.
As shown in Figure 1, material mixer 3 links to each other with extractive distillation column 4 side lines, extractive distillation column 4 tops and rectifying section discharging side line with go out feed mixer 6 and link to each other, be provided with water cooler 7 after going out feed mixer 6, water cooler 7 connects liquid-liquid extraction tower 8 bottom feed mouths, liquid-liquid extraction tower 8 bottom discharge mouths link to each other with extractive distillation column 4 tops again, extractive distillation column 4 bottoms and aromatic hydrocarbons are carried and are heated up in a steamer tower 9 opening for feeds and link to each other, aromatic hydrocarbons is carried and is heated up in a steamer tower 9 bottoms connection divider 10, divider 10 outlets are divided into two-way and connect: one, after connecting crude benzol preheater 11,11 outlets of crude benzol preheater connect liquid-liquid extraction tower 8 tops again; Its two, connect extractive distillation column reboiler 5, hydrogenated oil preheater 2, air cooler 1, material mixer 3 successively by connection line.
Detailed process is:
As shown in Figure 1, raw material hydrogenated oil temperature is 87.7 ℃, and mass rate is 5457.4 kg/h.After interchanger E101 and lean solvent heat exchange, temperature reaches 98.8 ℃, enters extractive distillation column T101 again, and pressure is 55kPa, and tower top temperature is 72.83 ℃, and column bottom temperature is 150.8 ℃.The extraction of rectifying section side line gas phase, flow is 408.27 kg/h.
Cat head discharging and side line mix through mixing tank M102, are cooled to 40 ℃ by interchanger E103 again, enter at the bottom of the liquid-liquid extraction tower T102 tower.Extraction tower is the normal pressure counter-current operation, and extraction agent is the N-N-formyl morpholine N-.Extraction phase is respectively with extracting phase: rich aromatic hydrocarbons heavy phase is mutually light with poor aromatic hydrocarbons.Rich aromatic hydrocarbons heavy phase is mainly aromatic hydrocarbons and N-N-formyl morpholine N-, reenters the extracting rectifying cat head, crosses cold reflux.The light phase mass rate of poor aromatic hydrocarbons is 183kg/h, and non-aromatics content is more than 97%.
Rich solvent enters aromatic hydrocarbons and carries and heat up in a steamer tower T103, and tower top pressure is-39kPa, and tower top temperature is 54.7 ℃, and column bottom temperature is 206.9 ℃.Cat head obtains pure aromatics, and mass rate is 5267.8kg/h, is lean solvent N-N-formyl morpholine N-at the bottom of the tower, and mass rate is 34704kg/h.
Lean solvent N-N-formyl morpholine N-is divided into the two-way circulation through divider S101, one enters interchanger E104 preheating material crude benzol, introduce liquid-liquid extraction tower T102 again, another is as extractive distillation column T101 tower bottom reboiler E102 thermal source, enter interchanger E101 preheating hydrogenated oil again, be cooled to 120 ℃ finally by air cooler A101, enter extractive distillation column T101.The N-N-formyl morpholine N-has small loss in the working cycle, replenishes a small amount of novel solvent at the extracting rectifying cat head.

Claims (2)

1. aromatic hydrocarbons purifying technique device that is used for hydrofining coking crude benzene, comprising that extractive distillation column, liquid-liquid extraction tower, aromatic hydrocarbons are carried heats up in a steamer tower, crude benzol preheater, hydrogenated oil preheater, water cooler, air cooler, material mixer, goes out feed mixer and divider; Material mixer links to each other with the extractive distillation column side line, extracting rectifying top of tower and rectifying section discharging side line all with go out feed mixer and link to each other, be provided with water cooler after going out feed mixer, water cooler connects liquid-liquid extraction tower bottom opening for feed, liquid-liquid extraction tower bottom discharge port links to each other with the extracting rectifying top of tower again, extracting rectifying tower bottom and aromatic hydrocarbons are carried and are heated up in a steamer the tower opening for feed and link to each other, aromatic hydrocarbons is carried and is heated up in a steamer tower bottom connection divider, export distributor is divided into two-way and connects: after (1) connected the crude benzol preheater, the outlet of crude benzol preheater connected the liquid-liquid extraction top of tower again; (2) connect extractive distillation column reboiler, hydrogenated oil preheater, air cooler, material mixer successively by connection line.
2. an aromatic hydrocarbons purifying technique that is used for hydrofining coking crude benzene is characterized in that, adopts the described device of claim 1, adopts following steps:
(1) enters extractive distillation column after raw material hydrogenated oil and the heat exchange of lean solvent N-N-formyl morpholine N-, extractive distillation column and liquid-liquid extraction tower gas-liquid are coupled, the place's side line gas phase extraction of extractive distillation column rectifying section 1-5 level, mix the back aromaticity content with the cat head discharging less than 70%, enter the liquid-liquid extraction tower after being cooled to 30 ℃-50 ℃ again.Liquid-liquid extraction tower counter-flow atmospheric operation, balance progression are 4-8, and service temperature is 20 ℃-60 ℃; Extraction phase and extracting phase are respectively that rich aromatic hydrocarbons heavy phase is mutually light with poor aromatic hydrocarbons, and rich aromatic hydrocarbons heavy phase is introduced the extracting rectifying cat head again as backflow, and double tower coupling reflux ratio is 0.5-0.9;
(2) rich solvent enters aromatic hydrocarbons and carries and heat up in a steamer tower and separate at the bottom of the extractive distillation column, and cat head obtains pure aromatics, is that lean solvent N-N-formyl morpholine N-recycles at the bottom of the tower;
(3) optimization synthesis heat exchanger network, branch's aromatic hydrocarbons are carried and are heated up in a steamer lean solvent at the bottom of the tower, and partition ratio is 1:8-10, one preheating material crude benzol, and another is as extracting rectifying tower bottom reboiler thermal source, and then the preheating material hydrogenated oil.
CN2013101166546A 2013-04-05 2013-04-05 Aromatic hydrocarbon purification apparatus and process used in hydrofining of coking crude benzene Pending CN103232317A (en)

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Cited By (8)

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CN104694158A (en) * 2015-02-03 2015-06-10 杨志强 Aromatic hydrocarbon extraction method
CN106008457A (en) * 2016-07-21 2016-10-12 中冶焦耐(大连)工程技术有限公司 Solvent regenerating process and device for crude benzene refining process
CN106831299A (en) * 2017-04-01 2017-06-13 天津奥展兴达化工技术有限公司 A kind of aromatic hydrocarbons extraction system of efficient energy-saving
WO2019149212A1 (en) 2018-02-01 2019-08-08 中国石油化工股份有限公司 Method for separating aromatic hydrocarbon using extractive distillation
CN114229938A (en) * 2021-09-23 2022-03-25 大连理工大学 Method for producing heavy oxygen water and heavy water in bidirectional strengthening manner
CN114470834A (en) * 2020-10-27 2022-05-13 湖南中岭化工有限责任公司 Crude benzene hydrogenation extraction device
CN114989856A (en) * 2021-03-02 2022-09-02 中国石油化工股份有限公司 Method and device for separating aromatic hydrocarbon or sulfur-containing compound from gasoline fraction
RU2785840C2 (en) * 2018-02-01 2022-12-14 Чайна Петролеум Энд Кемикал Корпорейшн Method for separation of aromatic hydrocarbons, using extraction distillation

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CN104694158A (en) * 2015-02-03 2015-06-10 杨志强 Aromatic hydrocarbon extraction method
CN106008457A (en) * 2016-07-21 2016-10-12 中冶焦耐(大连)工程技术有限公司 Solvent regenerating process and device for crude benzene refining process
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WO2019149212A1 (en) 2018-02-01 2019-08-08 中国石油化工股份有限公司 Method for separating aromatic hydrocarbon using extractive distillation
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RU2785840C2 (en) * 2018-02-01 2022-12-14 Чайна Петролеум Энд Кемикал Корпорейшн Method for separation of aromatic hydrocarbons, using extraction distillation
CN111954654B (en) * 2018-02-01 2023-03-17 中国石油化工股份有限公司 Method for separating aromatic hydrocarbon by extractive distillation
US11731922B2 (en) 2018-02-01 2023-08-22 China Petroleum & Chemical Corporation Method for separating aromatic hydrocarbon using extractive distillation
CN114470834A (en) * 2020-10-27 2022-05-13 湖南中岭化工有限责任公司 Crude benzene hydrogenation extraction device
CN114989856A (en) * 2021-03-02 2022-09-02 中国石油化工股份有限公司 Method and device for separating aromatic hydrocarbon or sulfur-containing compound from gasoline fraction
CN114989856B (en) * 2021-03-02 2023-09-05 中国石油化工股份有限公司 Method and device for separating aromatic hydrocarbon or sulfur-containing compound from gasoline fraction
CN114229938A (en) * 2021-09-23 2022-03-25 大连理工大学 Method for producing heavy oxygen water and heavy water in bidirectional strengthening manner

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Application publication date: 20130807