CN102585887A - Naphtha adsorbing separation and optimized utilization method - Google Patents
Naphtha adsorbing separation and optimized utilization method Download PDFInfo
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- CN102585887A CN102585887A CN2012100508062A CN201210050806A CN102585887A CN 102585887 A CN102585887 A CN 102585887A CN 2012100508062 A CN2012100508062 A CN 2012100508062A CN 201210050806 A CN201210050806 A CN 201210050806A CN 102585887 A CN102585887 A CN 102585887A
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Abstract
The invention provides a naphtha adsorbing separation and optimized utilization method. The method comprises the following steps: 1, filling naphtha into a simulation moving bed adsorbing separator filled with 5A molecular sieves under a liquid phase maintenance condition; 2, obtaining desorption effluents and raffinate effluents through a liquid-solid absorbing separation continuous technology; and 3, respectively recovering the desorption effluents and the raffinate effluents by a desorption agent to obtain desorption oil rich in n-alkanes and raffinate oil rich in non-normal alkanes, wherein the desorption oil contains 90-100wt% of the n-alkanes, and the raffinate oil contains 90-100wt% of the non-normal alkanes. The invention also provides a naphtha optimized utilization method. The adsorbing separation method provided in the invention, which has the advantages of low operation temperature, continuous operation, high yield, low desorption agent loss, and high molecular sieve utilization rate, couples a separating technology with subsequent processing technologies, and realizes the reasonable configuration of a resource.
Description
Technical field
The fractionation by adsorption and the optimization that the present invention relates to a kind of petroleum naphtha utilize method, thereby relate more specifically to adopt the simulation moving-bed liquid-solid fractionation by adsorption continuous processing of molecular sieve to make in the petroleum naphtha normal paraffin and non-n-alkane molecular level high efficiency separation realize optimizing the method for utilizing.
Background technology
Petroleum naphtha is meant in the crude oil and begins distilled temperature (being over point) to the lighting end 200 ℃ (or 180 ℃) from air distillation that its hydrocarbon composition carbon number distribution is at C
4～C
10Between.Mainly consist of normal paraffin, isoparaffin, naphthenic hydrocarbon and aromatic hydrocarbons, wherein the content of normal paraffin is 20%-50%, and non-positive structure hydrocarbon content is 50%-80%.
Traditional refining of petroleum flow process is taked the cut management Strategy, promptly according to the distillation characteristics of material the mixture in the crude oil is cut into the product of different boiling ranges, gives corresponding use according to the character of product then.Resource often can not obtain reasonable use the most under this management mode.Such as, the purposes of petroleum naphtha in petroleum refining industry mainly contains three kinds at present: (1) produces stop bracket gasoline or aromatic hydrocarbon product as the raw material of CR; (2) as the cracking of ethylene raw material; (3) be used for the allotment of vehicle fuel gasoline, but can run into the underproof problem of vp, contain a large amount of normal paraffins in the petroleum naphtha simultaneously, octane value is very low.
Consider with the ecological environment-friendly type social requirement from building resource-conserving how to optimize that to utilize naphtha resource be to be worth the problem further studied.The present situation present about China be, because crude oil in China lays particular stress on, the yield of petroleum naphtha is lower, and the problem that exists cracking of ethylene and CR to contend over raw materials for a long time is in order to satisfy the raw material supply of ethylene industry, the reformer under-capacity operation of many refineries as far as possible.
English Patent 2119398 openly comes selective adsorption to separate positive isomeric hydrocarbon and sulphur compound with the 5A molecular sieve, and certain specific structure of molecular sieve that emphasical is is used for adsorbing positive structure hydrocarbon and repels non-positive structure hydrocarbon, and has stressed the centrifugation to sulfide.The disclosed molecular sieve crystal that is to use in this patent is of a size of 1500 dusts to 0.5 micron, is not suitable for large-scale industrial application.
H.J.Bieser is at USP 4006197, and S.Kulprathipanja discloses employing continuous simulation moving-bed (SMB) adsorption separating method respectively at USP 4455444 and has been used for the normal paraffin recovery.The carbon number range of the typical feedstock that this patent is directed against is 10-15.As this scheme is applied to normal paraffin in the petroleum naphtha that carbon number is 5-10 when separating, can't obtain effective separation.This possibly be owing in sepn process, be difficult to realize liquid-phase operation than light hydrocarbon component, and a little less than the intermolecular displacement adsorption desorption of the different normal paraffin ability, and then cause being difficult to separating.
The optimization that Chinese patent CN 1621497A discloses a kind of petroleum naphtha utilizes method; This technology adopts the method for extracting and separating, petroleum naphtha is separated into raffinates oil and extract oil out, and the extraction oil that is obtained is as the reformer raw material; Raffinate oil as the ethylene cracker raw material; Because the selective problems of extraction process, it is difficult to reach the clear level of cutting apart of molecule management, in the time of will raffinating oil as the cracking of ethylene raw material; Owing to raffinate oil is the mixture of normal paraffin and isoparaffin, and it is main raw material that yield of ethene is starkly lower than with the normal paraffin.
Chinese patent CN 1710030A discloses a kind of 5A molecular sieve fixed-bed process based on molecule management the optimization of petroleum naphtha has been utilized method; This technology is through the ADSORPTION IN A FIXED BED sepn process; Petroleum naphtha is divided into desorption oil prodn that is rich in normal paraffin and the residual oil absorber that is rich in non-n-alkane, and efficiently utilizes respectively.But should technology be the periodical operation process that gas-solid is adsorbed mutually, have that productive rate is low, bed molecular sieve utilization ratio is difficult to improve and problem such as petroleum naphtha heating vaporization processing safety.
In sum, how this area shortage is a kind of carries out the isolating method of active adsorption to petroleum naphtha, and how to optimize the method for utilizing naphtha resource.
Therefore; This area presses for low, the operate continuously of a kind of service temperature of exploitation, productive rate is high, the desorbing agent loss is low, product yield is high and the adsorption separating method of the petroleum naphtha that the molecular sieve utilization ratio is high; And need exploitation with separating technology and subsequent machining technology coupling, realize the technical scheme of reasonable resources configuration.
Summary of the invention
First purpose of the present invention is to obtain that a kind of service temperature is low, operate continuously, productive rate is high, the desorbing agent loss is low, product yield is high and the molecular sieve utilization ratio is high adsorption separating method; And can separating technology and subsequent machining technology coupling be realized the reasonable resources configuration.
Second purpose of the present invention is to obtain that a kind of service temperature is low, operate continuously, productive rate is high, the desorbing agent loss is low, product yield is high and the molecular sieve utilization ratio is high optimization utilize method; And can separating technology and subsequent machining technology coupling be realized the reasonable resources configuration.
The 3rd purpose of the present invention is to obtain that a kind of service temperature is low, operate continuously, productive rate is high, the desorbing agent loss is low, product yield is high and the molecular sieve utilization ratio is high optimization utilization; Can separating technology and subsequent machining technology coupling be realized the reasonable resources configuration.
In first aspect of the present invention, a kind of adsorption separating method of petroleum naphtha is provided, it comprises the steps:
Petroleum naphtha is being kept feeding the simulated moving bed adsorption tripping device that is filled with the 5A molecular sieve under the liquid-phase condition;
Through liquid-solid fractionation by adsorption continuous processing, obtain the desorption elute and inhale surplus elute;
Said desorption elute with inhale surplus elute and reclaim the desorption oil that the back obtains to be rich in normal paraffin through desorbing agent respectively, and the suction excess oil that is rich in non-n-alkane;
Wherein, the weight content of normal paraffin is 90～100% in the said desorption oil; The weight content of non-n-alkane is 90～100% in the said suction excess oil.
In an embodiment of the present invention, in the said simulated moving bed adsorption tripping device, bed temperature is 100-190 ℃, and the naphtha feed air speed is 0.05-1.5h
-1, liquid desorbing agent charging air speed is 0.05-10h
-1
In an embodiment of the present invention, in the said simulated moving bed adsorption tripping device, the simulated moving bed adsorption separator column of employing is series connection multicolumn tower joint, and the aspect ratio that is filled with the single-column of 5A molecular sieve in the said tower joint is 2～20: 1.
In an embodiment of the present invention, said tower joint is cylinder tower joint.
In an embodiment of the present invention, said desorbing agent is Skellysolve A or normal hexane.
In an embodiment of the present invention, described petroleum naphtha is virgin naphtha, hydrogen cracking petroleum naphtha or hydrocracking petroleum naphtha.
Second aspect of the present invention provides a kind of optimization of petroleum naphtha to utilize method, and it comprises the steps:
By method of the present invention, petroleum naphtha is carried out fractionation by adsorption, obtain being rich in the desorption oil of normal paraffin, and the suction excess oil that is rich in non-n-alkane;
Said desorption oil is as the raw material of ethene steam cracking device or cut into close-cut fraction through rectifier unit and produce solvent oil;
Said suction excess oil is as raw materials for catalytic reforming device or as the blend component of high-octane rating clean gasoline.
In an embodiment of the present invention, the heater outlet temperature of said ethene steam cracking device is 700-940 ℃, and the residence time is 0.15-0.9 second, and dilution steam generation is 0.2-1.0 with said desorption oil quality ratio.
In an embodiment of the present invention, said suction excess oil gets into catalytic reforming unit, and temperature of reaction is 350-550 ℃, and reaction pressure is 0.2-3.5Mpa, hydrogen and the mol ratio 1-8 that inhales excess oil.
The third aspect of the invention provides a kind of simulated moving bed adsorption of the present invention fractionation by adsorption that is separated in petroleum naphtha and the purposes of optimizing utilization.
Description of drawings
Fig. 1 is the schema of method of the present invention.
Fig. 2 is simulated moving bed technology and subsequent machining technology coupled synoptic diagram (desorption product as high-quality cracking of ethylene raw material, inhale surplus product as the high-quality catalytic reforming raw material).
Fig. 3 is simulated moving bed technology and subsequent machining technology coupled synoptic diagram (desorption product as high-quality cracking of ethylene raw material, inhale surplus product as the high-octane rating blend component).
Fig. 4 is simulated moving bed technology and subsequent machining technology coupled synoptic diagram (the desorption product is as producing high-quality solvent oil raw material, inhaling surplus product as the stop bracket gasoline blend component).
Fig. 5 is simulated moving bed technology and subsequent machining technology coupled synoptic diagram (the desorption product is as producing high-quality solvent oil raw material, inhaling surplus product as the high-quality catalytic reforming raw material).
Embodiment
The inventor is through extensive and deep research; Through improving preparation technology; Obtained to have that service temperature is low, the desorbing agent loss is few and molecular sieve utilization ratio advantages of higher; And the adsorption separating method of the petroleum naphtha of desorbing agent reusable edible, and with this separating technology and subsequent machining technology coupling, the optimization that obtains a kind of petroleum naphtha utilizes novel method; Simulated moving bed technology with liquid-solid absorption continuous processing overcomes the defective that prior art exists, will based on the suitable alkene of molecule management then alkene, suitable Fang Zefang, should oily then oily naphtha resource high efficiency separation and optimization utilize skill upgrading to arrive new height.Accomplished the present invention on this basis.
Technical conceive of the present invention is following:
The invention relates to the novel technical method that a kind of naphtha resource optimization utilizes.Through the simulation moving-bed fractionation by adsorption successive processes of liquid phase, petroleum naphtha is divided into desolventizing desorption oil prodn that is rich in normal paraffin and the desolventizing residual oil absorber that is rich in non-n-alkane.Desolventizing desorption oil can be used as the fine steam crack material or cuts into close-cut fraction through rectifying.Desolventizing is inhaled excess oil and can be used as fine catalytic reforming raw material or high-octane rating clean gasoline blend component.According to naphtha resource quantity and market requirement situation, can realize the reasonable resources configuration neatly with simulation moving-bed adsorptive separation technology of petroleum naphtha liquid phase and subsequent machining technology coupling.This technology with class methods relatively, have that service temperature is low, operate continuously, output is high, the desorbing agent loss is low, product yield is high and molecular sieve utilization ratio advantages of higher.
Among the present invention, term " contains " or the various compositions of " comprising " expression can be applied in mixture of the present invention or the compsn together.Therefore, term " mainly by ... form " be included in " by ... composition " that term " contains " or in " comprising ".
Below detail to various aspects of the present invention:
The adsorption separating method of petroleum naphtha
The adsorption separating method of petroleum naphtha of the present invention mainly comprises:
Petroleum naphtha is being kept feeding the simulated moving bed adsorption tripping device that is filled with the 5A molecular sieve under the liquid-phase condition;
Through liquid-solid fractionation by adsorption continuous processing, obtain containing the desorption elute and the surplus elute of suction of desorbing agent;
Said desorption elute with inhale surplus elute and reclaim the desorption oil that the back obtains to be rich in normal paraffin through desorbing agent respectively, and the suction excess oil that is rich in non-n-alkane;
Wherein, the weight content of normal paraffin is 90～100% in the said desorption oil, in the gross weight of said desorption oil; The weight content of non-positive structure hydrocarbon is 90～100% in the said suction excess oil, in the gross weight of said suction excess oil.
Petroleum naphtha
Method of the present invention can be fit to the various petroleum naphthas of prior art, also is that " begin distilled temperature (being over point) to the lighting end 200 ℃ (or 180 ℃) from air distillation in the crude oil, its hydrocarbon composition carbon number distribution is at C
4～C
10Between.Mainly consist of normal paraffin, isoparaffin, naphthenic hydrocarbon and aromatic hydrocarbons, wherein the content of normal paraffin is 20%-50%, and non-positive structure hydrocarbon content is 50%-80%.”
More specifically, petroleum naphtha of the present invention can be virgin naphtha, hydrogen cracking petroleum naphtha or hydrocracking petroleum naphtha.
The 5A molecular sieve
In the present invention, adopted the simulated moving bed adsorption tripping device that is filled with the 5A molecular sieve.The contriver thinks, from petroleum naphtha, separating the most economical and effective means of normal paraffin is to utilize the shape absorption principle of selecting of 5A molecular sieve to carry out fractionation by adsorption.The mean pore size in 5A microporous molecular sieve road can get in the microporous molecular sieve road for the diameter of
normal paraffin molecule is about
; But not the molecular diameter of positive structure hydrocarbon is greater than this, then can not be adsorbed.Because the aperture homogeneous of molecular sieve pore passage, separation efficiency is very high.
5A molecular sieve of the present invention can commercially availablely obtain.
The simulated moving bed adsorption tripping device
In an embodiment of the present invention, in the said simulated moving bed adsorption tripping device, bed temperature is 100-190 ℃, and the naphtha feed air speed is 0.05-1.5h
-1, liquid desorbing agent charging air speed is 0.05-10h
-1Preferred, liquid naphtha feed air speed is 0.3-0.7h
-1, desorbing agent charging air speed is 1.2-2.8h
-1, be 750-900s switching time.
In an embodiment of the present invention, in the said simulated moving bed adsorption tripping device, the simulated moving bed adsorption separator column of employing is series connection multicolumn tower joint, and the aspect ratio that is filled with the single-column of 5A molecular sieve in the said tower joint is 2～20: 1.
In an embodiment, said tower joint is cylinder tower joint.
The present invention separates and the desorbing agent removal process through simulated moving bed adsorption, obtains two kinds of products: desolventizing is inhaled excess oil and desolventizing desorption oil.Desolventizing desorption oil is the oil product that is rich in normal paraffin, C
4～C
10The content of positive structure hydrocarbon is 90%-100%, and the content of non-positive structure hydrocarbon (comprising isoparaffin, naphthenic hydrocarbon and aromatic hydrocarbons) is 0%-10%.It is the oil product that is rich in non-positive structure hydrocarbon that desolventizing is inhaled excess oil, and the content of non-positive structure hydrocarbon (comprising isoparaffin, naphthenic hydrocarbon and aromatic hydrocarbons) is 90%-100%, and positive structure hydrocarbon content is 0%-10%.
Than fixed bed, advantage such as the inventive method has realized under the suitable prerequisite of separating effect that liquid-phase operation, service temperature are low, operate continuously productive rate height and molecular sieve bed utilization ratio height.
Because crude oil in China lays particular stress on, the yield of petroleum naphtha is lower, and the problem that exists cracking of ethylene and CR to contend over raw materials for a long time is in order to satisfy the raw material supply of ethylene industry, the reformer under-capacity operation of many refineries as far as possible.
In order to improve the utilising efficiency of petroleum naphtha, alleviate this contradiction, the molecule management mode more and more demonstrates its meliority.The molecule management is that the separating mixture component is made the best use of everything to reach according to the specific requirement of different purposes to products molecule.For petroleum naphtha; Thinking according to the molecule management; Isolate wherein normal paraffin as high-quality cracking of ethylene raw material or cut into close-cut fraction and produce the solvent oil product, non-positive structure part (mainly being isoparaffin, naphthenic hydrocarbon and aromatic hydrocarbons) is as high-quality catalytic reforming raw material or stop bracket gasoline blend component.
Desorbing agent
In the embodiment of the present invention, said desorbing agent is Skellysolve A or normal hexane.
Preferred implementation
The present invention is heated to 150-170 ℃ with petroleum naphtha and desorbing agent; Feed simulation moving-bed material inlet (F) and the desorbing agent import (D) that is filled with the 5A molecular sieve respectively; The desorbing agent that normal paraffin in the petroleum naphtha adsorbs in the mid-molecular sieve that swaps out of simulation moving-bed adsorption zone (III district) and being attracted in the molecular sieve pore passage, the suction excess oil after the adsorption treatment flows out the simulated moving bed adsorption tripping device, is cooled to 10～30 ℃; The suction excess oil is condensed; Liquefaction, through obtaining to be rich in the desolventizing suction excess oil of non-n-alkane behind the desorbing agent regenerating column, non-positive structure hydrocarbon weight content is 90～100% in the desolventizing suction excess oil again; The normal paraffin that desorbing agent adsorbs in the mid-molecular sieve that swaps out in simulation moving-bed desorption district (I district) is also taken out of by desorption oil export (AD); Be cooled to 10～30 ℃; Desorption oil is condensed; Liquefaction, through obtaining to be rich in the desolventizing desorption oil of positive structure hydrocarbon behind the desorbing agent regenerating column, positive structure hydrocarbon weight content is 90～100% in the desolventizing desorption oil again;
The optimization of petroleum naphtha utilizes method
The optimization of petroleum naphtha of the present invention utilizes method, and it comprises the steps:
By above-mentioned method petroleum naphtha is carried out fractionation by adsorption, obtain being rich in the desorption oil of normal paraffin, and the suction excess oil that is rich in non-n-alkane;
Said desorption oil is as the raw material of ethene steam cracking device or cut into close-cut fraction through rectifier unit and produce solvent oil;
Said suction excess oil is as raw materials for catalytic reforming device or as the blend component of high-octane rating clean gasoline.
Desorption oil
Said desorption oil is as the raw material of ethene steam cracking device or cut into close-cut fraction through rectifier unit and produce solvent oil.
In an embodiment of the present invention, the heater outlet temperature of said ethene steam cracking device is 700-940 ℃, and the residence time is 0.15-0.9 second, and dilution steam generation is 0.2-1.0 with said desorption oil quality ratio.
The pyrolyzer of said ethene steam cracking can adopt prior art, like SH type and CBL type pyrolyzer.Because the desolventizing desorption oil to be rich in normal paraffin is the ethane cracking furnace charging, yield of ethene and triolefin total recovery have significantly raising than existing ethylene raw petroleum naphtha.
In preparing ethylene by steam cracking technology, expense of raw materials accounts for 60%～80% of ethylene production total cost.As cracking stock, the yield of ethene of cracking technology is the highest with normal paraffin.Present good linear dependence between the BMCI of yield of ethene and cracking stock (Bureau of Mines Correlation Index, the correlation index) value.The BMCI value of hydro carbons is more little, and the expression fatty is strong more, and then the yield of ethene is high more.The BMCI value of normal paraffin approaches zero, therefore is best cracking of ethylene raw material.
The added value of solvent oil is far above fuel gasoline, but the refining bottleneck that often becomes the production of restriction solvent oil of solvent oil.The defective phenomenon that solvent oil the most often occurs be that aromaticity content exceeds standard, boiling range is wide and flash-point defective etc., treating process tends to make the solvent oil yield to descend, production cost rises.The desorption oil of fractionation by adsorption is rich in normal paraffin; Aromatic free; And the relative volatility between each component is big, is easy to separate through the means of rectifying, produces reagent products such as high-quality solvent oil product or polymerization-grade normal hexane, the high-purity normal hexane of pharmaceutical grade, normal heptane.
Inhale excess oil
In an embodiment of the present invention; Desolventizing is inhaled excess oil and is got into catalytic reforming unit as catalytic reforming raw material, obtains aromatic hydrocarbon product, and operational condition is following: temperature of reaction is 350-550 ℃; Reaction pressure is 0.2-3.5Mpa, and hydrogen and desolventizing are inhaled the mol ratio 1-8 of excess oil.
In the above-mentioned embodiment, aromatics yield improves 10-15 percentage point than corresponding petroleum naphtha.
Said catalytic reforming reactor can adopt prior art, like S.R device and CCR device.Because to be rich in the high desolventizing suction excess oil of non-positive structure hydrocarbon arene underwater content is catalytic reforming raw material, aromatics yield is significantly increased than existing reformer feed petroleum naphtha.
The oil product arene underwater content that has removed normal paraffin is high, the catalytic reforming raw material of doing preferably.The normal paraffin dehydrocyclization becomes the speed of reaction of aromatic hydrocarbons very slow, and transformation efficiency is low.Can add the carrying out of fast response though improve temperature of reaction, but can aggravate catalyst junction carbon, the production cycle is shortened, also higher to the requirement of operation and equipment.The minimizing of normal paraffin content will significantly help improving aromatics yield and the severity that reduces reaction conditions in the reformer feed.
Perhaps, desolventizing is inhaled the blend component of excess oil as the high-octane rating clean gasoline.Its octane value improves 20 more than the unit than corresponding petroleum naphtha.
The octane value of gasoline and its hydrocarbon composition are in close relations.Aromatic hydrocarbon and isoparaffin octane value are the highest, can reach more than 100, and alkene and naphthenic hydrocarbon take second place, and normal paraffin is minimum, are zero like normal heptane, and octane is a negative value.Normal paraffin content is high in the petroleum naphtha, and octane value is lower, usually about 60.After normal paraffin in the gasoline removed, the octane value of inhaling excess oil had raising by a relatively large margin, can be used as the stop bracket gasoline blend component.
Advantage of the present invention
The present invention is owing to adopt the simulation moving-bed fractionation by adsorption of 5A molecular sieve liquid phase; And adopt petroleum naphtha and desorbing agent to pass through bed with liquid phase; Than other existing patented technologies have that service temperature is low, operate continuously, productive rate is high, the desorbing agent loss is few, product yield is high and molecular sieve utilization ratio advantages of higher, and desorbing agent reusable edible.
The inventive method, adsorption process and desorption process are simultaneously, carry out continuously.Technology of the present invention can also realize the reasonable resources configuration with separating technology and subsequent machining technology coupling.
Visible by above-mentioned disclosed technical scheme; Method of the present invention can significantly improve the utilising efficiency of petroleum naphtha; And for downstream complete processing (cracking of ethylene and CR) high quality raw material are provided, blend component or high-quality solvent wet goods cleaning chemistry article that simultaneously can coproduction high-octane rating clean gasoline.According to naphtha resource quantity and market requirement situation, can realize the reasonable resources configuration neatly with petroleum naphtha adsorptive separation technology and subsequent machining technology coupling.
Specify like nothing, various raw materials of the present invention all can obtain through commercially available; Or prepare according to the ordinary method of this area.Only if definition or explanation are arranged in addition, the same meaning that all specialties used herein and scientific words and those skilled in the art are familiar with.Any in addition with the institute similar content of putting down in writing or the equalization method and material all can be applicable in the inventive method.
Other aspects of the present invention are because the disclosure of this paper is conspicuous to those skilled in the art.
Below in conjunction with specific embodiment, further set forth the present invention.Should be understood that these embodiment only to be used to the present invention is described and be not used in the restriction scope of the present invention.The experimental technique of unreceipted actual conditions in the following example is measured according to national standard usually.If there is not a corresponding national standards, then carry out according to general international standard, normal condition or according to the condition that manufacturer advises.Unless otherwise indicated, otherwise all umbers are weight part, and all per-cents are weight percentage, and described polymericular weight is a number-average molecular weight.
Only if definition or explanation are arranged in addition, the same meaning that all specialties used herein and scientific words and those skilled in the art are familiar with.Any in addition with the institute similar content of putting down in writing or the equalization method and material all can be applicable in the inventive method.
Referring to the technical process of Fig. 1, technical process of the present invention comprises the steps:
Liquid petroleum naphtha and desorbing agent are fed separator column III district and the I district that is filled with the 5A molecular sieve respectively, and the normal paraffin in the petroleum naphtha is attracted in the microchannel of I district bed molecular sieve, and the suction excess oil after the adsorption treatment flows out simulation moving-bed separator column III district; Cooling; The suction excess oil is condensed, and obtains to be rich in the suction excess oil of non-n-alkane, sends into catalytic reforming unit 3; Obtain reformate, like benzene, toluene and YLENE;
Simultaneously, desorbing agent carries out desorption in simulation moving-bed separator column I district, and the desorption agent flow that carries normal paraffin goes out simulation moving-bed separator column I district; Normal paraffin is condensed, and the desorption oil of positive structure hydrocarbon is rich in liquefaction, acquisition; Send into and get into ethene steam cracking device 2; Obtain the cracking product, like ethene, the third rare and divinyl, desorbing agent recycles;
Then through rotary valve 7, with the move forward position of a separator column of simulation moving-bed import and export position synchronous, the fractionation by adsorption principle is same as described above.
The boiling range that contains mass concentration and be 30% normal paraffin is that the liquid petroleum naphtha 5kg of 40-180 ℃ of straight run is 170 ℃ simulation moving-bed molecular sieve bed through temperature; Filling 3.4kg 5A molecular sieve in the bed; Bed height is 30cm, and aspect ratio is 10: 1, and the naphtha feed air speed is 0.34h
-1, desorbing agent Skellysolve A charging air speed is 1.37h
-1Be 900 seconds switching time; Obtain after the condensation inhaling surplus in the middle of oil and desorption oil, with inhale surplus in the middle of in the surplus middle oil of desolventizing suction that obtains after through the desorbing agent removal process of oil and desorption oil the non-n-alkane mass concentration be 85%, the normal paraffin mass concentration is 98% in the desolventizing desorption oil that obtains.
Desolventizing is inhaled surplus middle oil feed the simulation moving-bed fractionation by adsorption of carrying out once more also through after the desorbing agent removal process as raw material; The non-n-alkane mass concentration is 92% in the desolventizing suction excess oil that obtains, and the normal paraffin mass concentration is 98% in the desolventizing desorption oil that obtains.Desolventizing is inhaled the excess oil yield and is about 70%, and desolventizing desorption oil yield is about 30%.
Because simulation moving-bed bed is made up of several end to end single-columns, petroleum naphtha separates to accomplish through all single-column beds a switching cycle domestic demand with desorbing agent.So for simulated moving bed technology, molecular sieve bed utilization ratio is 100%.For the simulated moving bed technology in the present embodiment, petroleum naphtha year treatment capacity be 1944kg/a.
Desolventizing desorption oil is as the cracking of ethylene raw material, and cracking condition is: the residence time is 0.40s, and the dilution steam generation ratio is 0.6, and the cracking temperature out is 840 ℃.Compare with feed naphtha, gas recovery ratio brings up to 94.8% by 85.8%, and yield of ethene brings up to 47.2% from 30.7%, and ethene, propylene and divinyl triolefin total recovery bring up to 72.1% from 55.5%.
The operational condition of catalytic reforming unit is that the temperature of reaction of CR is 450 ℃, and reaction pressure is 1.5Mpa, hydrogen/oil mol ratio 2.The aromatics yield of suction excess oil is compared from 55.4% with corresponding raw material petroleum naphtha and is elevated to 70.5%.
The octane value of inhaling excess oil is compared with the raw material petroleum naphtha from 65 and is brought up to 86, has improved 21 units.
Technical process of the present invention is as shown in Figure 1.
The boiling range that contains mass concentration and be 30% normal paraffin is that the liquid petroleum naphtha 5kg of 40-180 ℃ of straight run is 150 ℃ simulation moving-bed molecular sieve bed through temperature; Filling 3.4kg 5A molecular sieve in the bed; Bed height is 30cm, and aspect ratio is 10: 1, and the naphtha feed air speed is 0.17h
-1, desorbing agent Skellysolve A charging air speed is 0.68h
-1Be 900 seconds switching time; Obtain after the condensation inhaling surplus in the middle of oil and desorption oil, with inhale surplus in the middle of in the surplus middle oil of desolventizing suction that obtains after through the desorbing agent removal process of oil and desorption oil the non-n-alkane mass concentration be 82%, the normal paraffin mass concentration is 95% in the desolventizing desorption oil that obtains.
Desolventizing is inhaled surplus middle oil feed the simulation moving-bed fractionation by adsorption of carrying out once more also through after the desorbing agent removal process as raw material; The non-n-alkane mass concentration is 90% in the desolventizing suction excess oil that obtains, and the normal paraffin mass concentration is 95% in the desolventizing desorption oil that obtains.Desolventizing is inhaled the excess oil yield and is about 70%, and desolventizing desorption oil yield is about 30%.
Desolventizing desorption oil is as the cracking of ethylene raw material, and cracking condition is: the residence time is 0.40s, and the dilution steam generation ratio is 0.6, and the cracking temperature out is 840 ℃.Compare with feed naphtha, gas recovery ratio brings up to 94.3% by 85.8%, and yield of ethene brings up to 46.9% from 30.7%, and ethene, propylene and divinyl triolefin total recovery bring up to 71.8% from 55.5%.
The operational condition of catalytic reforming unit is that the temperature of reaction of CR is 450 ℃, and reaction pressure is 1.5Mpa, hydrogen/oil mol ratio 2.The aromatics yield of suction excess oil is compared from 55.4% with corresponding raw material petroleum naphtha and is elevated to 70.1%.
The octane value of inhaling excess oil is compared with the raw material petroleum naphtha from 65 and is brought up to 85, has improved 20 units.
Technical process of the present invention is as shown in Figure 1.
The boiling range that contains mass concentration and be 25% normal paraffin is that 44-182 ℃ of hydrogen cracking petroleum naphtha 5kg is 170 ℃ simulation moving-bed molecular sieve bed through temperature; Filling 3.4kg 5A molecular sieve in the bed; Bed height is 30cm, and aspect ratio is 10: 1, and the naphtha feed air speed is 0.17h
-1, desorbing agent Skellysolve A charging air speed is 0.86h
-1Be 700 seconds switching time; Obtain after the condensation inhaling surplus in the middle of oil and desorption oil, with inhale surplus in the middle of in the surplus middle oil of desolventizing suction that obtains after through the desorbing agent removal process of oil and desorption oil the non-n-alkane mass concentration be 88%, the normal paraffin mass concentration is 95% in the desolventizing desorption oil that obtains.
Desolventizing is inhaled surplus middle oil feed the simulation moving-bed fractionation by adsorption of carrying out once more also through after the desorbing agent removal process as raw material; The non-n-alkane mass concentration is 94% in the desolventizing suction excess oil that obtains, and the normal paraffin mass concentration is 95% in the desolventizing desorption oil that obtains.Desolventizing is inhaled the excess oil yield and is about 70%, and desolventizing desorption oil yield is about 30%.
Desolventizing desorption oil is as the cracking of ethylene raw material, and cracking condition is: the residence time is 0.40s, and the dilution steam generation ratio is 0.6, and the cracking temperature out is 840 ℃.Compare with feed naphtha, gas recovery ratio brings up to 93.5% by 86.0%, and yield of ethene brings up to 46.4% from 30.2%, and ethene, propylene and divinyl triolefin total recovery bring up to 70.6% from 54.3%.
The operational condition of catalytic reforming unit is that the temperature of reaction of CR is 450 ℃, and reaction pressure is 1.5Mpa, hydrogen/oil mol ratio 2.The aromatics yield of suction excess oil is compared from 55.4% with corresponding raw material petroleum naphtha and is elevated to 70.7%.
The octane value of inhaling excess oil is compared with the raw material petroleum naphtha from 63 and is brought up to 85, has improved 22 units.
Embodiment 4
Technical process of the present invention is as shown in Figure 1.
The boiling range that contains mass concentration and be 30% normal paraffin is that 50-190 ℃ of hydrocracking petroleum naphtha 5kg is 170 ℃ simulation moving-bed molecular sieve bed through temperature; Filling 3.4kg 5A molecular sieve in the bed; Bed height is 30cm, and aspect ratio is 10: 1, and the naphtha feed air speed is 0.34h
-1, desorbing agent normal hexane charging air speed is 1.37h
-1Be 900 seconds switching time; Obtain after the condensation inhaling surplus in the middle of oil and desorption oil, with inhale surplus in the middle of in the surplus middle oil of desolventizing suction that obtains after through the desorbing agent removal process of oil and desorption oil the non-n-alkane mass concentration be 82%, the normal paraffin mass concentration is 95% in the desolventizing desorption oil that obtains.
Desolventizing is inhaled surplus middle oil feed the simulation moving-bed fractionation by adsorption of carrying out once more also through after the desorbing agent removal process as raw material; The non-n-alkane mass concentration is 90% in the desolventizing suction excess oil that obtains, and the normal paraffin mass concentration is 95% in the desolventizing desorption oil that obtains.Desolventizing is inhaled the excess oil yield and is about 70%, and desolventizing desorption oil yield is about 30%.
Desolventizing desorption oil is as the cracking of ethylene raw material, and cracking condition is: the residence time is 0.40s, and the dilution steam generation ratio is 0.6, and the cracking temperature out is 840 ℃.Compare with feed naphtha, gas recovery ratio brings up to 94.3% by 85.8%, and yield of ethene brings up to 46.9% from 30.7%, and ethene, propylene and divinyl triolefin total recovery bring up to 71.8% from 55.5%.
The operational condition of catalytic reforming unit is that the temperature of reaction of CR is 450 ℃, and reaction pressure is 1.5Mpa, hydrogen/oil mol ratio 2.The aromatics yield of suction excess oil is compared from 55.4% with corresponding raw material petroleum naphtha and is elevated to 70.1%.
The octane value of inhaling excess oil is compared with the raw material petroleum naphtha from 65 and is brought up to 85, has improved 20 units.
Embodiment 5
Technical process of the present invention is as shown in Figure 1.
The boiling range that contains mass concentration and be 35% normal paraffin is that 50-190 ℃ of hydrocracking petroleum naphtha 5kg is 180 ℃ simulation moving-bed molecular sieve bed through temperature; Filling 3.4kg 5A molecular sieve in the bed; Bed height is 30cm, and aspect ratio is 10: 1, and the naphtha feed air speed is 0.34h
-1, desorbing agent normal hexane charging air speed is 1.37h
-1Be 900 seconds switching time; Obtain after the condensation inhaling surplus in the middle of oil and desorption oil, with inhale surplus in the middle of in the surplus middle oil of desolventizing suction that obtains after through the desorbing agent removal process of oil and desorption oil the non-n-alkane mass concentration be 83%, the normal paraffin mass concentration is 98% in the desolventizing desorption oil that obtains.
Desolventizing is inhaled surplus middle oil feed the simulation moving-bed fractionation by adsorption of carrying out once more also through after the desorbing agent removal process as raw material; The non-n-alkane mass concentration is 91% in the desolventizing suction excess oil that obtains, and the normal paraffin mass concentration is 98% in the desolventizing desorption oil that obtains.Desolventizing is inhaled the excess oil yield and is about 65%, and desolventizing desorption oil yield is about 35%.
Desolventizing desorption oil is as the cracking of ethylene raw material, and cracking condition is: the residence time is 0.40s, and the dilution steam generation ratio is 0.6, and the cracking temperature out is 840 ℃.Compare with feed naphtha, gas recovery ratio brings up to 94.8% by 85.8%, and yield of ethene brings up to 47.2% from 30.7%, and ethene, propylene and divinyl triolefin total recovery bring up to 72.1% from 55.5%.
The operational condition of catalytic reforming unit is that the temperature of reaction of CR is 450 ℃, and reaction pressure is 1.5Mpa, hydrogen/oil mol ratio 2.The aromatics yield of suction excess oil is compared from 55.4% with corresponding raw material petroleum naphtha and is elevated to 70.5%.
The octane value of inhaling excess oil is compared with the raw material petroleum naphtha from 65 and is brought up to 86, has improved 21 units.
Comparative Examples 1
According to traditional work flow, it is that the boiling range of 30% normal paraffin is a 40-180 ℃ of virgin naphtha that 5kg is contained mass concentration, is divided into two portions of 1.90kg and 3.10kg, respectively as cracking of ethylene raw material and catalytic reforming raw material.
1.90kg contain mass concentration and be the boiling range of 30% normal paraffin and be 40-180 ℃ of virgin naphtha as the cracking of ethylene raw material, cracking condition is: the residence time is 0.80s, the dilution steam generation ratio is 0.6, and the cracking temperature out is 900 ℃.Obtain ethene 0.63g, ethene, propylene and divinyl triolefin total amount 1.04kg.
3.10kg containing mass concentration and be the boiling range of 30% normal paraffin is that 40-180 ℃ of virgin naphtha advances catalytic reforming unit, operational condition is that the temperature of reaction of CR is 450 ℃, and reaction pressure is 2.0Mpa, hydrogen/oil mol ratio 2.Obtain aromatic hydrocarbon product 1.55kg.
Can know that by embodiment and Comparative Examples it is that the boiling range of 30% normal paraffin is that 40-180 ℃ of virgin naphtha directly seen table 1 as cracking of ethylene and catalytic reforming raw material with the product production of using integrated optimization technology of the present invention that 5kg contains mass concentration.
Table 1
Comparative Examples 2
The boiling range that contains mass concentration and be 30% normal paraffin is that the liquid petroleum naphtha 5kg of 40-180 ℃ of straight run is 300 ℃ fixed bed molecular sieve bed through temperature; Filling 3.4kg 5A molecular sieve in the bed; Obtain being rich in the desorption oil prodn and the residual oil absorber that is rich in non-n-alkane of normal paraffin, the product purity that its product purity and simulated moving bed technology obtain is suitable.This fixed-bed process petroleum naphtha year treatment capacity is 972kg/a, and molecular sieve bed utilization ratio is about 95%.
Can be known that by embodiment and Comparative Examples handling 5kg respectively by simulated moving bed technology and fixed-bed process, to contain mass concentration be that the boiling range of 30% normal paraffin is a 40-180 ℃ of virgin naphtha, table 2 is seen in its each item index contrast.
Table 2
| Index | Simulated moving bed technology | Fixed-bed process |
| The operation phase | Liquid phase | Gas phase |
| Service temperature (℃) | 170 | 300 |
| Product yield (%) | 0.99-1.00 | 0.88-0.95 |
| Year treatment capacity (kg/a) | 1944 | 972 |
| Molecular sieve utilization ratio (%) | 100 | 95-98 |
The above is merely preferred embodiment of the present invention; Be not in order to limit essence technology contents scope of the present invention; Essence technology contents of the present invention is broadly to be defined in the claim scope of application, and if any technological entity or method that other people accomplish are defined identical with the claim scope of application; Also or a kind of change of equivalence, all will be regarded as and be covered by among this claim scope.
All documents in that the present invention mentions are all quoted as a reference in this application, are just quoted such as a reference separately as each piece document.Should be understood that in addition that after having read foregoing of the present invention those skilled in the art can do various changes or modification to the present invention, these equivalent form of values fall within the application's appended claims institute restricted portion equally.
Claims (10)
1. the adsorption separating method of a petroleum naphtha is characterized in that, comprises the steps:
Petroleum naphtha is being kept feeding the simulated moving bed adsorption tripping device that is filled with the 5A molecular sieve under the liquid-phase condition;
Through liquid-solid fractionation by adsorption continuous processing, obtain the desorption elute and inhale surplus elute;
Said desorption elute with inhale surplus elute and reclaim the desorption oil that the back obtains to be rich in normal paraffin through desorbing agent respectively, and the suction excess oil that is rich in non-n-alkane;
Wherein, the weight content of normal paraffin is 90～100% in the said desorption oil; The weight content of non-n-alkane is 90～100% in the said suction excess oil.
2. adsorption separating method as claimed in claim 1 is characterized in that, in the said simulated moving bed adsorption tripping device, bed temperature is 100-190 ℃, and the naphtha feed air speed is 0.05-1.5h
-1, liquid desorbing agent charging air speed is 0.05-10h
-1
3. adsorption separating method as claimed in claim 1; It is characterized in that; In the said simulated moving bed adsorption tripping device, the simulated moving bed adsorption separator column of employing is series connection multicolumn tower joint, and the aspect ratio that is filled with the single-column of 5A molecular sieve in the said tower joint is 2～20: 1.
4. adsorption separating method as claimed in claim 3 is characterized in that, said tower joint is cylinder tower joint.
5. adsorption separating method as claimed in claim 1 is characterized in that, said desorbing agent is Skellysolve A or normal hexane.
6. adsorption separating method as claimed in claim 1 is characterized in that, described petroleum naphtha is virgin naphtha, hydrogen cracking petroleum naphtha or hydrocracking petroleum naphtha.
7. the optimization of a petroleum naphtha utilizes method, it is characterized in that, comprises the steps:
By the method for claim 1, petroleum naphtha is carried out fractionation by adsorption, obtain being rich in the desorption oil of normal paraffin, and the suction excess oil that is rich in non-n-alkane;
Said desorption oil is as the raw material of ethene steam cracking device or cut into close-cut fraction through rectifier unit and produce solvent oil;
Said suction excess oil is as raw materials for catalytic reforming device or as the blend component of high-octane rating clean gasoline.
8. optimization as claimed in claim 7 utilizes method, it is characterized in that, the heater outlet temperature of said ethene steam cracking device is 700-940 ℃, and the residence time is 0.15-0.9 second, and dilution steam generation is 0.2-1.0 with said desorption oil quality ratio.
9. optimization as claimed in claim 7 utilizes method, it is characterized in that,
Said suction excess oil gets into catalytic reforming unit, and temperature of reaction is 350-550 ℃, and reaction pressure is 0.2-3.5Mpa, hydrogen and the mol ratio 1-8 that inhales excess oil.
10. a simulated moving bed adsorption as claimed in claim 1 is separated in the purposes that petroleum naphtha optimization utilizes the aspect.
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| CN104974790A (en) * | 2014-04-08 | 2015-10-14 | 中石化洛阳工程有限公司 | Method of producing high-octane gasoline from naphtha |
| CN106433742A (en) * | 2015-08-06 | 2017-02-22 | 中国石油化工股份有限公司 | Method for adsorbing and separating n-alkane from distillate oil containing n-alkane |
| CN106675649A (en) * | 2016-12-28 | 2017-05-17 | 神华集团有限责任公司 | Method for preparing coal-based light liquid paraffin from coal indirect liquefied oil product and coal-based light liquid paraffin obtained through method |
| CN106861614A (en) * | 2017-04-06 | 2017-06-20 | 中触媒新材料股份有限公司 | 5A adsorbent of molecular sieve containing n-alkane distillate adsorbing separation and preparation method thereof |
| CN111471488A (en) * | 2019-01-23 | 2020-07-31 | 内蒙古伊泰宁能精细化工有限公司 | High-purity environment-friendly isoparaffin solvent oil and application thereof |
| CN111589434A (en) * | 2020-05-25 | 2020-08-28 | 南京工业大学 | Regeneration method for inactivation of 5A molecular sieve for naphtha adsorption separation |
| CN112409121A (en) * | 2020-12-02 | 2021-02-26 | 恒力石化(大连)化工有限公司 | Low-carbon olefin and aromatic hydrocarbon yield increasing method and system |
| CN112441868A (en) * | 2020-12-02 | 2021-03-05 | 恒力石化(大连)化工有限公司 | Method and system for increasing yield of ethylene by using refinery dry gas |
| CN114088832A (en) * | 2021-11-12 | 2022-02-25 | 中国科学院西北生态环境资源研究院 | Deep-ultra-deep hydrocarbon source rock normal paraffin light component and isotope analysis system and method |
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| CN104974790A (en) * | 2014-04-08 | 2015-10-14 | 中石化洛阳工程有限公司 | Method of producing high-octane gasoline from naphtha |
| CN106433742A (en) * | 2015-08-06 | 2017-02-22 | 中国石油化工股份有限公司 | Method for adsorbing and separating n-alkane from distillate oil containing n-alkane |
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| CN106861614A (en) * | 2017-04-06 | 2017-06-20 | 中触媒新材料股份有限公司 | 5A adsorbent of molecular sieve containing n-alkane distillate adsorbing separation and preparation method thereof |
| CN111471488A (en) * | 2019-01-23 | 2020-07-31 | 内蒙古伊泰宁能精细化工有限公司 | High-purity environment-friendly isoparaffin solvent oil and application thereof |
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| CN112409121A (en) * | 2020-12-02 | 2021-02-26 | 恒力石化(大连)化工有限公司 | Low-carbon olefin and aromatic hydrocarbon yield increasing method and system |
| CN112441868A (en) * | 2020-12-02 | 2021-03-05 | 恒力石化(大连)化工有限公司 | Method and system for increasing yield of ethylene by using refinery dry gas |
| CN112409121B (en) * | 2020-12-02 | 2023-07-11 | 恒力石化(大连)化工有限公司 | Yield increasing method and system for low-carbon olefin and aromatic hydrocarbon |
| CN114088832A (en) * | 2021-11-12 | 2022-02-25 | 中国科学院西北生态环境资源研究院 | Deep-ultra-deep hydrocarbon source rock normal paraffin light component and isotope analysis system and method |
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