CN102180759B - Method for preparing hexane - Google Patents

Method for preparing hexane Download PDF

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Publication number
CN102180759B
CN102180759B CN 201110070148 CN201110070148A CN102180759B CN 102180759 B CN102180759 B CN 102180759B CN 201110070148 CN201110070148 CN 201110070148 CN 201110070148 A CN201110070148 A CN 201110070148A CN 102180759 B CN102180759 B CN 102180759B
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hexane
tower
preparing
distillation
thick
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CN102180759A (en
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张殿明
李荣忠
侯云亭
王建
徐文静
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BEIJING YANSHAN JILIAN PETROLEUM CHEMICAL Co Ltd
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BEIJING YANSHAN JILIAN PETROLEUM CHEMICAL Co Ltd
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Abstract

The invention discloses a method for preparing hexane from raffinate oil serving as a raw material, which comprises the following steps of: (a) performing primary distillation, namely feeding the raffinate oil into a first distillation tower, controlling the tower top temperature to be between 54 and 64 DEG C, condensing components evaporated on the tower top to obtain condensate, refluxing one part of condensate, extracting the other part of condensate serving as residual liquid, and cooling tower bottom liquid; (b) performing secondary distillation, namely feeding the cooled tower bottom liquid into a hexane distillation tower, ensuring that the tower top temperature is between 64 and 74 DEG C, and condensing components evaporated on the tower top to obtain crude hexane; and (c) performing hydrogenation on the hexane, namely feeding the crude hexane into a hydrogenation reactor, performing hydrogenation, and separating to obtain the hexane. The raw material in the method for preparing the hexane is sufficient, the key is rectification separation, and various hexane products with different n-hexane content can be obtained, and the source of the hexane is greatly expanded. A cutting unit adopts a two-tower continuous rectification process, a gas phase fixed bed adiabatic reactor is adopted, and safety is facilitated while hydrogen is prevented from being circulated.

Description

A kind of method for preparing hexane
Technical field
The present invention relates to a kind of method for preparing hexane, relating in particular to a kind of is the method for feedstock production hexane to raffinate oil.
Background technology
The method for preparing normal hexane in the prior art is a lot, but complex process.Catalytic reformate (reformed gasoline) remaining distillate behind extraction (or extracting) aromatic hydrocarbons of raffinating oil and referring generally to be rich in aromatic hydrocarbons, its main component is alkane and a certain amount of naphthenic hydrocarbon of C5~C10.With the preparation normal hexane of raffinating oil, raw material abundance, mainly be rectifying separation.Can obtain the multiple hexane product of different normal hexane content.Yet in the prior art and the report of being difficult to raffinate oil into the feedstock production hexane.
Summary of the invention
The present invention is intended to overcome the deficiency that above prior art exists, and a kind of method for preparing hexane is provided, and expands the source of hexane.
Technical solution problem of the present invention adopts following technical scheme:
A kind of method for preparing hexane is characterized in that, comprises the steps:
(a) single flash of raffinating oil: will raffinate oil be preheated to 45~95 ℃ with preheater after, be delivered to first distillation tower, 54~64 ℃ of control tower top temperatures, cat head steams component and sends into condenser condenses and get phlegma, part phlegma is delivered to described distillation tower cat head as backflow, another part, cools off tower bottoms with the tower charging to residual liquid tank as the raffinate extraction;
(b) second distillation of raffinating oil: cooled tower bottoms is delivered to the hexane distillation tower, 64~74 ℃ of control tower top temperatures, and it is thick hexane that cat head steams component, and a part is delivered to hexane distillation tower cat head and is refluxed after the thick hexane condensation, and a part is delivered to thick hexane jar;
(c) hexane hydrogenation: deliver to hydrogenator after the thick hexane of gained in the step (b) is heated to 100~150 ℃, alkene in the thick hexane and benzene hydrogenation are generated saturated alkane, condensation separation gets the hexane phlegma then.
Further, control the tower top temperature of first distillation tower in the step (a) by the quantity of steam of tower bottom reboiler, cat head steam component send into condenser after uncondensed gas enter tail gas condenser, use the chilled brine condensation.
Further, the thick hexane recirculated water condensation that cat head steams in the step (b), the chilled brine condensation of uncooled tail gas.
Further, raffinate oil in the step (a) and before entering preheater, in interchanger, carry out preheating with tower bottoms.
Further, with the thick hexane of gained in the step (b) with being steam heated to 100~150 ℃.
Further, be filled with NCG-6 type benzene hydrogenating catalyst in the hydrogenator in the step (c).
Further, in the step (c) the exess of H2 gas in the hydrogenation process through the blow-down pipe skirt to eminence emptying.
Further, hydrogenation reaction adopts the gas phase fixed bed adiabatic reactor in the step (c).
The present invention prepares the method raw material abundance of hexane, mainly is rectifying separation.Can obtain the multiple hexane product of different normal hexane content, greatly expand the source of hexane.Cutter unit adopts two tower continuous rectification flow processs, deviates from light component earlier, steams thick hexane again; The hexane hydrogenation unit is used NCG-6 type hydrogenation catalyst, adopts the gas phase fixed bed adiabatic reactor, when having avoided hydrogen recycle, also helps safety.
Description of drawings
Fig. 1 prepares the distillatory device schema first time of the method for hexane for the present invention;
Fig. 2 prepares the distillatory device schema second time of the method for hexane for the present invention;
Fig. 3 prepares the device schema of hexane hydrogenation reaction of the method for hexane for the present invention;
Fig. 4 coagulates isolating device schema for this bright hydrogenation reaction air cooling for preparing the method for hexane.
Embodiment
Embodiment 1
Main raw and auxiliary material: raffinate oil, hydrogen, NCG-6 type hydrogenation catalyst, wherein NCG-6 type hydrogenation catalyst is Primary Catalysts with nickel, is main carrier with aluminum oxide.120~130 ℃ have activity, 140~180 ℃ of general use temperatures, and being higher than 200 ℃ of life-time service can influence its activity and life-span, and muriate, sulfide, oily substance can both make its poisoning, and specification is as follows:
Outward appearance: black or grey black cylindrical particle; Diameter: 3.5~4mm; Highly: 3~4mm; Bulk density: 0.9~1.3Kg/L
Specific surface: 90~180M 2/ g;
Name of product: industrial hexane (smart hexane)
Main production process: what refinery came raffinates oil through hexane cutter unit (comprising distillation for the first time and distillation for the second time), adopts the flow process of two tower continuous rectifications, deviates from light component earlier, steams thick hexane again; Thick hexane is through the hexane hydrogenation unit, and under the effect of NCG-6 type hydrogenation catalyst, benzene and alkene and hydrogen generation hydrogenation reaction generation stable hydrocarbon that thick hexane is included obtain the industrial hexane product.
Described hexane cutter unit and hexane hydrogenation unit concrete operations flow process are as follows:
The hexane cutter unit
Accumulating workshop section raffinates oil through the flux cumulating table with the refinery reformer that the pumping of raffinating oil comes, after regulating, the metering of Flow-rate adjustment instrument enters tower still water cooler 2 tube sides of first distillation tower 3 by the tower bottoms preheating, enter the preheater 111 of raffinating oil again, 112, use tower bottom reboiler 4 at this, 12 steam condensation water is heated to 70 ± 25 ℃, enter first distillation tower 3, regulate the quantity of steam of the tower bottom reboiler 4 of first distillation tower 3,59 ± 5 ℃ of control tower top temperatures, cat head steams component and enters first distillation column condenser, 6 shell sides, cool off with the recirculated water condensation, uncondensed gas enters the first distillation tower tail gas condenser, 5 shell sides, with chilled brine its condensation is cooled off, lime set flows into the first distillation tower return tank 7, part lime set is with the first distillation tower reflux pump 731,741 deliver to first distillation tower, 3 cats head as backflow, another part is by the first distillation tower return tank, 7 liquid level regulating and controlling instrument L2 dominant discharge, deliver to residual liquid tank 131,132, tower bottoms is after 2 coolings of the first distillation tower still liquid water cooler, with the first distillation tower still liquid pump 71,72 send into second column 8.Regulate the quantity of steam of second column 8 tower still reboilers 12,69 ± 5 ℃ of control tower top temperatures, cat head steams component (thick hexane) and enters hexane tower condenser 9 shell sides, cool off with the recirculated water condensation, uncondensed gas enters hexane tower tail gas condenser 10 shell sides, with chilled brine its condensation is cooled off, lime set flows into hexane tower return tank 11, part lime set hexane tower reflux pump 77,78 deliver to hexane tower second column 8 tops as refluxing, another part is by hexane tower return tank 11 liquid level regulating and controlling instrument dominant discharge, deliver to thick hexane jar 151,152, tower bottoms is after 14 coolings of hexane tower bottoms water cooler, with hexane tower bottoms pump 75,76 send into residual liquid tank 131,132.Material in the residual liquid tank 131,132 is delivered to refinery or accumulating tank field with tail pump 73,74.
The hexane hydrogenation unit
Contain a spot of benzene and alkene in the thick hexane in the thick hexane basin 151,152, its hydrogenation need be saturated to alkane.With hexane pump 771,781 after the Flow-rate adjustment instrument is regulated flow, thick hexane is sent into vaporizer 16, hydrogen is through hydrogen pressure control instruments and hydrogen gas buffer 18 decompression voltage stabilizings simultaneously, with flow control instrument dominant discharge, enter vaporizer 16 from the bottom, snake type heating tube is arranged in the vaporizer 16, with liquid level regulation meter steam regulation amount, control vaporizer 16 liquid levels are below 40%, hydrogen is through hexane liquid layer bubbling and hexane vapor mixing, after the wire cloth mist eliminator is removed entrained drip, enter preheater 17 again,, enter hydrogenator 19 with being steam heated to 100~150 ℃.Hydrogenator 19 is a fixed bed adiabatic reactor, in fill out NCG-6 type benzene hydrogenating catalyst, gas mixture is behind hydrogenator 19, benzene in the thick hexane and alkene and hydrogen generation hydrogenation reaction generate saturated alkane, obtain the mixed gas of industrial hexane and hydrogen, mixed gas is introduced into hydrogenation condenser 2011,2012 shell sides, with recirculated water its condensation is cooled off, uncondensed gas enters smart hexane tail gas condenser 202 shell sides, with chilled brine with its condensation cool off the hexane lime set, the hexane lime set enters smart hexane basin 211,212, qualified by analysis after, with smart hexane pump 791,792 regularly deliver to the accumulating tank field.The exess of H2 gas in the hydrogenation process, from smart hexane tail gas condenser 202 blow-down pipe skirts to the 8 top emptying of hexane tower.
Embodiment recited above is described preferred implementation of the present utility model; be not that design of the present utility model and scope are limited; do not breaking away under the utility model design prerequisite; common engineering technical personnel make the technical solution of the utility model in this area various modification and improvement; all should fall into protection domain of the present utility model; the technology contents that the utility model is asked for protection all is documented in claims.

Claims (8)

1. a method for preparing hexane is characterized in that, is raw material to raffinate oil, and the preparation method comprises the steps:
(a) single flash of raffinating oil: will raffinate oil be preheated to 45~95 ℃ with preheater after, be delivered to first distillation tower, 54~64 ℃ of control tower top temperatures, cat head steams component and sends into condenser condenses and get phlegma, part phlegma is delivered to described distillation tower cat head as backflow, another part, and cools off tower bottoms with the tower charging to residual liquid tank as the raffinate extraction;
(b) second distillation of raffinating oil: cooled tower bottoms is delivered to the hexane distillation tower, 64~74 ℃ of control tower top temperatures, and it is thick hexane that cat head steams component, and a part is delivered to hexane distillation tower cat head and is refluxed after the thick hexane condensation, and a part is delivered to thick hexane jar;
(c) hexane hydrogenation: deliver to hydrogenator after the thick hexane of gained in the step (b) is heated to 100~150 ℃, alkene in the thick hexane and benzene hydrogenation are generated saturated alkane, condensation separation gets the hexane phlegma then.
2. the method for preparing hexane according to claim 1, it is characterized in that: the tower top temperature of controlling first distillation tower in the step (a) by the quantity of steam of tower bottom reboiler, cat head steam component send into condenser after uncondensed gas enter tail gas condenser, use the chilled brine condensation.
3. the method for preparing hexane according to claim 1 is characterized in that: the thick hexane recirculated water condensation that cat head steams in the step (b), the chilled brine condensation of uncooled tail gas.
4. the method for preparing hexane according to claim 1 is characterized in that: raffinate oil in the step (a) and carry out preheating with tower bottoms in interchanger before entering preheater.
5. the method for preparing hexane according to claim 1 is characterized in that: with the thick hexane of gained in the step (c) with being steam heated to 100~150 ℃.
6. the method for preparing hexane according to claim 1 is characterized in that: be filled with NCG-6 type benzene hydrogenating catalyst in the hydrogenator in the step (c).
7. the method for preparing hexane according to claim 1 is characterized in that: the exess of H2 gas in the step (c) in the hydrogenation process through the blow-down pipe skirt to eminence emptying.
8. the method for preparing hexane according to claim 1 is characterized in that: hydrogenation reaction adopts the gas phase fixed bed adiabatic reactor in the step (c).
CN 201110070148 2011-03-23 2011-03-23 Method for preparing hexane Active CN102180759B (en)

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Publication number Priority date Publication date Assignee Title
CN103588603B (en) * 2012-08-13 2015-06-03 中国石油天然气股份有限公司 Process for producing n-hexane by using reformate raffinate oil
CN103073383B (en) * 2013-02-07 2015-07-01 天津大学 Method and device for separating isohexane, n-hexane and benzene
CN104280381A (en) * 2013-07-01 2015-01-14 北京瑞利分析仪器有限公司 Device saving potassium borohydride using amount of atomic fluorescence spectrometer
CN106799059A (en) * 2017-03-17 2017-06-06 河南中托力合化学有限公司 Energy-saving hexane precise distillation apparatus
CN114935107A (en) * 2022-06-15 2022-08-23 浙江浙能航天氢能技术有限公司 Simple hydrogenation device

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Publication number Priority date Publication date Assignee Title
CN1351982A (en) * 2000-11-14 2002-06-05 南化集团研究院 Low temperature and low pressure hydrofining process for production of high quality n-hexane
CN1569782A (en) * 2004-04-27 2005-01-26 广州赫尔普化工有限公司 Method for preparing isohexane solvent
CN101974347A (en) * 2010-09-17 2011-02-16 天津精华石化有限公司 Process for producing solvent oil by removing aromatic hydrocarbon from raffinate oil

Patent Citations (3)

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Publication number Priority date Publication date Assignee Title
CN1351982A (en) * 2000-11-14 2002-06-05 南化集团研究院 Low temperature and low pressure hydrofining process for production of high quality n-hexane
CN1569782A (en) * 2004-04-27 2005-01-26 广州赫尔普化工有限公司 Method for preparing isohexane solvent
CN101974347A (en) * 2010-09-17 2011-02-16 天津精华石化有限公司 Process for producing solvent oil by removing aromatic hydrocarbon from raffinate oil

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