CN103073383A - Method and device for separating isohexane, n-hexane and benzene - Google Patents
Method and device for separating isohexane, n-hexane and benzene Download PDFInfo
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Abstract
The invention relates to a method and device for separating isohexane, n-hexane and benzene. A rectifying and extractive distillation combined method is adopted. The device comprises a light component removing unit, a hexane extractive distillation unit, a hexane separating unit, a first solvent recovery unit, a benzene extractive distillation unit, a second solvent recovery unit and a solvent regenerating unit. Impurities with boiling point lower than that of 2-methyl pentane are firstly removed from the mixed hydrocarbon raw materials, such as raffinate oil, pyrolysis gasoline, straight distilling gasoline, from an aromatics extraction device, and then an extractive distillation method is adopted for separating the mixed hexane without benzene; the mixed hexane is further separated into an isohexane product and a n-hexane product; the material separated from the mixed hexane is separated by adopting the extractive distillation method, so that a benzene product is obtained; the total mass fraction of the isohexane product 2-methyl pentane and 3-methyl pentane is not less than 95% and the benzene content is less than 100ppm; and the n-hexane product meets the national standard GB16629-2008 and the mass fraction is not less than 99%.
Description
Technical field
The present invention relates to separation method and the equipment of a kind of isohexane, normal hexane and benzene, relate to especially the separation method that a kind of conventional distillation and extracting rectifying combine.
Background technology
Normal hexane is a kind of colourless transparent liquid, is one of varsol of widespread use, is the most representative non-polar solvent.The industrial hexane solvent oil can be used in the industries such as medicine, chemical industry, macromolecular material, rubber industry and food.As the edible oil industrial extractant, require the hexane solvent oil distillate more narrow better, benzene content is more low better simultaneously, and these two indexs directly have influence on quality, oil yield and the energy consumption etc. of edible oil.When normal hexane is used as the solvent of propylene polymerization, require benzene content more few better.This not only is conducive to improve the speed of polypropylene polymerization, and also beneficial to guaranteeing polyacrylic quality.In addition, highly purified normal hexane also is that the assay laboratory carries out scientific research, one of important organic solvent of analytical test.The market demand of the high-end normal hexane product of high purity, low benzene content is very large.
The isohexane main component is 2-methyl-pentane and 3-methyl-pentane, as the short-side chain varsol with its lower boiling, narrow boiling range, gasification latent heat is low and more and more do not favored in edible oil industry in the advantages such as row of polluted air objectionable impurities.As the edible oil extraction agent, the benzene content in the isohexane product has strict demand equally.
Hexane production is often adopted catalytic reforming generation oil, hydrogenated pyrolysis gasoline or aromatic hydrocarbons to raffinate oil and is made raw material.Often component is various in these raw materials, alkane, naphthenic hydrocarbon, aromatic hydrocarbons and a small amount of alkene are arranged, in every class component multiple isomers is arranged again, and the boiling point between these compound things differs very little, what have also can form azeotropic, lower 5.4 ℃ than normal hexane boiling point such as the 3-methylpentane; Methylcyclopentane is higher 3.1 ℃ than normal hexane boiling point; Normal hexane and benzene can form minimum azeotropic mixture.This minimum azeotropic mixture can cause not only that benzene is difficult to remove in the normal hexane product, can cause also that benzene is difficult to remove in the isohexane product.This shows, production high purity normal hexane, the isohexane that does not contain benzene only depend on the conventional distillation method to separate and can not realize.
The technique that rectifying and hydrogenation combine is one of main method of producing at present hexane.Usually the scheme of rectifying and hydrogenation production normal hexane has two kinds, is respectively rectifying behind first rectifying repeated hydrogenation and the first hydrogenation.Current, although it is quite ripe to separate the method that obtains thick normal hexane with rectificating method or the concentrated double tower of platformate raffinate hydrogenation from straight run or raffinating oil, its purity is all 60% ~ 90%.Yet the production technique of domestic current normal hexane and output all can't satisfy the demand of industrial market, and the high purity normal hexane relies on import substantially.Therefore, improve the normal hexane production technique, the production technology of exploitation high purity normal hexane is significant.
The method of employing shortening removes the benzene in the normal hexane raw material, and is still applicable for the situation that benzene content is lower, adopts the method not only can cause energy consumption high when benzene content is higher, also can cause the benzene wasting of resources.When benzene content was high in the raw material, with after normal hexane separates, it is better that the one-step refining of going forward side by side becomes purity to reach the benzaldehyde product economy that relevant criterion requires with benzene.
The object of the invention is to develop a kind of production without the benzene isohexane with without the separation method of benzene normal hexane, produce simultaneously high-purity benzaldehyde product.
Summary of the invention
The object of the invention is to develop a kind of without benzene isohexane and high-purity, without the separation method of benzene normal hexane, produce simultaneously high-purity benzaldehyde product.The present invention proposes the separation method of a kind of normal hexane, isohexane and benzaldehyde product, the method that particularly adopts conventional distillation and extracting rectifying to combine.
According to the present invention, from mixed feedstocks of hydrocarbons such as the raffinating oil of aromatic extraction unit, pyrolysis gasoline or straight-run spirit, at first remove than the low-boiling impurity of 2-methylpentane, then isolate the mixing hexane that does not contain benzene by extraction rectifying method.Mix hexane and further be separated into isohexane product and normal hexane product.Remove the material that mixes behind the hexane, obtaining benzaldehyde product after separating through follow-up extraction rectifying method.
Technical scheme of the present invention is as follows:
A kind of method of separating isohexane, normal hexane and benzaldehyde product; Comprise lights removal unit, hexane extraction rectification cell, hexane separating unit, the first solvent recovery unit, benzene extracting rectifying unit, the second solvent recovery unit and solvent reclamation unit; From mixed feedstocks of hydrocarbons such as the raffinating oil of aromatic extraction unit, pyrolysis gasoline or straight-run spirit, at first remove than the low-boiling impurity of 2-methylpentane, then isolate the mixing hexane that does not contain benzene by extraction rectifying method; Mix hexane and further be separated into isohexane product and normal hexane product; Remove the material that mixes behind the hexane, obtaining benzaldehyde product after separating through extraction rectifying method again.
Realize the equipment of separation isohexane of the present invention, normal hexane and benzaldehyde product, be composed in series with flow direction of material by lightness-removing column 101, hexane extraction rectifying tower 105, hexane knockout tower 109, the first solvent recovery tower 114, benzene extractive distillation column 119 and the second solvent recovery tower 124; Each tower top is provided with condenser, condenser is connected with return tank, and the bottom is provided with reboiler; Hexane knockout tower 109 tower reactors connect normal hexane bleaching earth adsorption bed 303; The second solvent recovery tower 124 return tank of top of the tower 127 connect benzene bleaching earth adsorption bed 403; The first solvent recovery tower 114 be connected solvent recovery tower 124 tower reactors and connect solvent reclamation vaporizer 201.
Adopt linking device of the present invention to separate the method for isohexane, normal hexane and benzaldehyde product, from the mixed feedstocks of hydrocarbons outside the battery limit (BL) after the feed preheater preheating, send into lightness-removing column 101, from lightness-removing column 101 removed overhead than the low-boiling light constituent impurity of 2-methylpentane after, send into hexane extraction rectifying tower 105 again and separate, hexane extraction rectifying tower 105 overhead extractions do not contain the mixing hexane stream thigh of benzene; The mixture flow thigh of hexane extraction rectifying tower 105 tower reactor extraction solvents, benzene and a small amount of non-aromatics; Mixing hexane stream thigh is sent into hexane knockout tower 109 and is separated, send into basin at hexane knockout tower 109 overhead extractions stream thigh as the isohexane product, obtain normal hexane product after the normal hexane stream stock-traders' know-how bleaching earth adsorption bed 303 of hexane knockout tower 109 tower reactor extraction is processed and send into basin; Hexane extraction rectifying tower 105 still materials are sent into the first solvent recovery tower 114 and are separated, be recycled solvent in the first solvent recovery tower 114 tower reactors, major part is returned hexane and is got rectifying tower 105 Reusabilities after cooling, rest part send solvent reclamation vaporizer 201 to carry out impurities removal; The first solvent recovery tower 114 cats head obtain the mixture of benzene and non-aromatics impurity, and send into benzene extractive distillation column 119 and separate, and from benzene extracting rectifying 119 removed overhead non-aromatics impurity, and send into basin as the solvent oil product; Benzene extracting rectifying 119 tower reactors are the mixed flow thigh of benzene and extraction agent, send the second solvent recovery tower 124 to separate, be recycled solvent in the second solvent recovery tower 124 tower reactors, major part is returned benzene extractive distillation column 119 Reusabilities after cooling, rest part send solvent reclamation vaporizer 201 to carry out impurities removal; After the benzene stream stock-traders' know-how bleaching earth adsorption bed 403 of the second solvent recovery tower 124 overhead extractions is processed, after cooling, get benzaldehyde product.
In mixed feedstocks of hydrocarbons, do not contain the restructuring timesharing such as toluene, can obtain benzaldehyde product without the benzene refining unit.Be specially from the mixed feedstocks of hydrocarbons outside the battery limit (BL) after the feed preheater preheating, send into lightness-removing column, from removed overhead than the low-boiling light constituent impurity of 2-methylpentane after, send into again the hexane extraction rectifying tower and separate, overhead extraction does not contain the mixing hexane stream strand of benzene.The mixture flow thigh of tower reactor extraction solvent, benzene and a small amount of non-aromatics.Mix hexane stream and strand send into the hexane knockout tower and separate, strand send into basin as the isohexane product at hexane knockout tower overhead extraction stream, obtain normal hexane product after the normal hexane stream stock-traders' know-how bleaching earth adsorption bed of tower reactor extraction is processed and send into basin.Hexane extraction rectifying tower reactor material is sent into the first solvent recovery tower and is separated, and is recycled solvent in tower reactor, and major part is returned hexane and got the rectifying tower Reusability after cooling, and small part is sent the solvent reclamation unit to take off rearrangement and mixed; Cat head obtains the mixture of benzene and non-aromatics impurity.The first solvent recuperation cat head stream strand is sent into the benzene extractive distillation column and is separated, and from removed overhead non-aromatics impurity, and sends into basin as the solvent oil product; Tower reactor is the mixed flow thigh of benzene and extraction agent, send the second solvent recovery tower to separate, and is recycled solvent in tower reactor, and major part is returned benzene extractive distillation column Reusability after cooling, and small part is sent the solvent reclamation unit to take off rearrangement and mixed; After the benzene stream stock-traders' know-how bleaching earth adsorption bed of overhead extraction is processed, obtain benzaldehyde product through cooling again and send basin.
Described lightness-removing column working pressure is absolute pressure 130 ~ 300kPa; Hexane extraction rectifying tower, hexane knockout tower, benzene extractive distillation column and benzene refining tower working pressure are normal pressure; The first solvent recovery tower and the second solvent recovery tower vacuum operating, the working pressure of this two tower is absolute pressure 20 ~ 60kPa.Regeneration vaporizer 201 is falling-film evaporator, and working pressure is absolute pressure 20 ~ 60kPa; Filler particles carclazyte in the bleaching earth adsorption bed, the service temperature of bleaching earth adsorption bed 303 is 120 ℃ ~ 200 ℃, working pressure is than the high 100 ~ 200kPa of saturated vapor pressure of normal hexane under the selected service temperature; The service temperature of bleaching earth adsorption bed 403 is 120 ℃ ~ 200 ℃, and working pressure is than the high 100 ~ 200kPa of saturation pressure of benzene under the selected service temperature.
Described isohexane, normal hexane and benzaldehyde product separation method are characterised in that hexane extraction rectifying tower and benzene extractive distillation column tower adopt the method for extracting rectifying, and all the other each towers are the conventional distillation method.
The extraction agent that described hexane extraction rectifying tower and benzene extractive distillation column use comprises glycols, N-Methyl pyrrolidone, tetramethylene sulfone, dimethyl sulfoxide (DMSO), N-formyl morpholine or is one or several the composite extractant in above-mentioned; Two extractive distillation columns can be selected identical extraction agent, also can select different extraction agents, and the add-on of extraction agent is 3～6 times of inlet amount.
The tower reactor extraction solvent cycle of the first solvent recovery tower and the second solvent recovery tower is used.
The packed bed that is characterized as granular carclazyte of described bleaching earth adsorption bed, the micro-nitrogenous compound that the alkene that it is characterized in that removing in the product trace improves the product bromine number and produces because of solvolysis, and can improve product colourity, adoptable granular carclazyte comprises JH-01 and NC-01.
Described solvent reclamation unit is characterised in that employing falling-film evaporator system, is shared by the first solvent recovery tower and the second solvent recovery tower, and vacuum operating, working pressure are absolute pressure 30kPa.
Described benzene refining tower is characterised in that the restructuring minute impurity such as toluene that can remove in the benzene, and has certain function that removes light constituent impurity; Be further characterized in that whether to move according to restructuring minute decisions such as whether containing toluene in the raw material.
The isohexane product 2-methylpentane and the 3-methylpentane total mass mark that adopt the technology of the present invention to produce are not less than 95%, and benzene content is less than 100ppm.
Adopt normal hexane product indices that the technology of the present invention produces except can being up to state standards GB16629-2008, outside the company standard Q/SH PRD0406-2011 of China PetroChemical Corporation, and can reach the normal hexane massfraction and be not less than 99% requirement.
The benzaldehyde product that adopts the technology of the present invention the to produce GB3405-89 that is up to state standards.
Description of drawings
The schematic flow sheet that the isohexane of Fig. 1 embodiment 1, normal hexane and benzene separate.
The schematic flow sheet of Fig. 2 solvent regeneration system of the present invention.
Fig. 3 normal hexane bleaching earth adsorption of the present invention bed schematic flow sheet.
Fig. 4 benzene adsorption bed of the present invention schematic flow sheet.
The schematic flow sheet that the isohexane of Fig. 5 embodiment 2, normal hexane and benzene separate.
Embodiment
The invention will be further described below in conjunction with accompanying drawing 1 ~ Fig. 4:
Equipment of the present invention is as follows: by lightness-removing column 101, hexane extraction rectifying tower 105, hexane knockout tower 109, the first solvent recovery tower 114, benzene extractive distillation column 119, the second solvent recovery tower 124, benzene refining tower 129 is composed in series; Each tower top is provided with condenser, condenser is connected with return tank, and the bottom is provided with reboiler; Hexane knockout tower 109 tower reactors connect normal hexane bleaching earth adsorption bed 303; The second solvent recovery tower 124 return tank of top of the tower 127 connect benzene bleaching earth adsorption bed 403; The first solvent recovery tower 114 be connected solvent recovery tower 124 tower reactors and connect solvent reclamation vaporizer 201.
Embodiment 1
Separation method according to a kind of isohexane of the present invention, normal hexane and benzene, from not containing the restructuring timesharing such as toluene in the mixed feedstocks of hydrocarbons such as the raffinating oil of aromatic extraction unit, pyrolysis gasoline or straight-run spirit, sepn process and embodiment one are basic identical, at first remove than the low-boiling impurity of 2-methylpentane, then isolate the mixing hexane that does not contain benzene by extraction rectifying method.Mix hexane and further be separated into isohexane product and normal hexane product.Remove the material that mixes behind the hexane, obtaining benzaldehyde product after separating through follow-up extraction rectifying method.
Technical process mainly comprises such as lower unit: lights removal unit, hexane extraction rectification cell, hexane separating unit, the first solvent recovery unit, benzene extracting rectifying unit, the second solvent recovery unit and solvent reclamation unit.Below in conjunction with accompanying drawing above-mentioned each unit is described.
From the total hydrocarbon feed outside the battery limit (BL) after the feed preheater preheating, from lightness-removing column 101 top chargings, overhead vapours is after condenser of light component removal column 102 condensations, and lime set enters lightness-removing column return tank 103 part and refluxes, another part as the light constituent product from the return tank extraction.The lightness-removing column still arranges reboiler 104.This tower adopts pressurized operation to guarantee that overhead vapours can be recycled cooling water condensation, and working pressure is that absolute pressure 160kPa(is suitable in 130kPa ~ 300kPa scope).The component of overhead extraction stream thigh is mainly pentamethylene, the boiling point light hydrocarbons impurity lower than 2-methylpentane such as 2,2-methylbutane.Lightness-removing column 101 a tower reactors stream strand chief component is isohexane, normal hexane and benzene, sends into hexane extraction rectifying tower 105 and carries out later separation.
From the stream thigh of lightness-removing column still from the 105 middle part chargings of hexane extraction rectifying tower, the extraction agent N-Methyl pyrrolidone (just exemplifies a kind of extraction agent here, the extraction agent that summary of the invention is mentioned all is suitable for) from feed plate top charging, the add-on of extraction agent is 6 times (all being suitable for 3 times ~ 6 times scopes) of inlet amount.The effect of extraction agent has increased hexane and methylcyclopentane, the relative volatility of hexane and benzene, thus the clear cutting of hexane and benzene is achieved.Under the effect of extraction agent, material is interior through repeatedly gasification at hexane extraction rectifying tower 105, realize behind the multiple condensation separating, overhead vapours obtains mixing hexane after hexane is got 106 condensations of rectifying tower condenser, enter hexane and get rectifying tower return tank 107, a part refluxes, and rest part send hexane knockout tower 109 further to separate.Interchanger 108 is hexane extraction rectifying tower reactor reboiler, and the rich benzene extraction agent solution that tower reactor obtains is sent into the first solvent recovery tower 114 and carried out solvent recuperation.
After the mixing hexane entered hexane knockout tower 109, isohexane was realized separating with normal hexane behind abundant vapour-liquid heat and mass, and overhead vapours enters hexane knockout tower return tank 111 after 110 condensations of hexane separation column condenser, and a part refluxes; Rest part is as the extraction of isohexane product, and wherein 2-methylpentane and 3-methylpentane total concn are about 95%, and benzene content is lower than 100ppm.Interchanger 112 is the tower reactor reboiler of hexane knockout tower 109.Normal hexane for the tower reactor extraction, massfraction is higher than 99.0%, wherein benzene content is less than 100ppm, after delivering to normal hexane the first preheater 301 and normal hexane the second preheater 302 and being preheated to 170 ℃ after (all being suitable for 120 ℃ ~ 200 ℃ scopes), process through bleaching earth adsorption bed 303 again, can make the normal hexane product indices GB16629-2008 that can be up to state standards, the company standard Q/SH PRD0406-2011 of China PetroChemical Corporation, and the normal hexane massfraction is not less than 99%.
Rich benzene extraction agent solution is realized separating behind the 114 interior process vapour-liquids heat transfers of the first solvent recovery tower, mass transfer, cat head steams benzene and non-aromatics mixture, enters the first solvent recovery tower return tank 117 after the first solvent recovery tower condenser 115 and 116 condensations of the first solvent recovery tower aftercooler.This tower adopts vacuum operating, and working pressure is that absolute pressure 30kPa(is suitable in 20kPa ~ 60kPa scope), the non-condensable gas of the first solvent recovery tower aftercooler 116 is extracted out by vacuum pump 133.Wherein the first solvent recovery tower condenser 115 adopts recirculated cooling water to do heat-eliminating medium, and temperature out is controlled in 37 ~ 47 ℃ of scopes; The first solvent recovery tower aftercooler 116 adopts low-temperature cooling water to make heat-eliminating medium, and temperature out is controlled in 20 ~ 30 ℃ of scopes.The first solvent recovery tower return tank 117 interior material parts reflux, and all the other are sent into benzene extractive distillation column 119 and further separate.The first solvent recovery tower 114 tower reactors reclaim extraction agent N-methyl-pyrrolidone, and major part is returned hexane extraction rectifying tower 107 and recycled after 113 coolings of extraction agent water cooler, and small part send 201 to carry out manipulation of regeneration.Interchanger 118 is the tower reactor reboiler of the first solvent recovery tower 114.
Benzene and non-aromatics mixture from the first solvent recovery tower return tank 117, top charging from benzene extractive distillation column 119, extraction agent N-methyl-pyrrolidone (just exemplifies a kind of extraction agent here, the extraction agent that summary of the invention is mentioned all is suitable for) added by the feed plate top, the add-on of extraction agent is 6 times (all being suitable for 3 ~ 6 times of scopes) of benzene extractive distillation column 119 inlet amounies.Under the effect of extraction agent, aromatic hydrocarbons and non-aromatics realize separating, the steam of non-aromatic hydro carbons by 120 condensations of benzene extractive distillation column condenser after, enter benzene extractive distillation column return tank 121 parts and reflux, rest part is as the extraction of solvent oil product.Interchanger 122 is the tower reactor reboiler of benzene extractive distillation column 119, and the mixture of benzene and extraction agent is sent into the second molten recovery tower 124 and recycled from the tower reactor extraction.
Separate at the second solvent recovery tower 124 from the benzene of benzene extractive distillation column 119 tower reactors and the mixture of extraction agent, overhead vapours is after the second solvent recovery tower condenser 125 and 126 condensations of the second solvent recovery tower aftercooler, enter the second solvent recovery tower return tank 127, partial reflux, the rest part extraction.The material of extraction part after (all being suitable in 120 ℃ ~ 200 ℃ scopes), being delivered to bleaching earth adsorption bed 403 and is removed the impurity such as alkene after benzene the first preheater 401 and benzene the second preheater 402 are preheated to 170 ℃.Remove material behind the alkene from bleaching earth adsorption bed 403, through benzene the first preheater 401 with from the material-heat-exchanging of the second solvent recovery tower return tank 127 after again, can obtain benzaldehyde product through further cooling again, product index can reach GB3405-89, and the benzene massfraction is not less than 99.9%.
The second solvent recovery tower 124 towers adopt vacuum operating, and working pressure is that absolute pressure 30kPa(is suitable at 20kPa ~ 60kPa).The second solvent recovery tower condenser 125 adopts recirculated cooling water to do heat-eliminating medium, and temperature out is controlled in 37 ~ 47 ℃ of scopes; The second solvent recovery tower aftercooler 126 adopts low-temperature cooling water to make heat-eliminating medium, and temperature out is controlled in 20 ~ 30 ℃ of scopes.The non-condensable gas of the second solvent recovery tower aftercooler 126 is extracted out by vacuum pump 134.The second solvent recovery tower 124 tower reactors are solvent N-methyl-pyrrolidone, and major part is returned the benzene extractive distillation column through extraction agent and recycled after water cooler 123 coolings, and small portion send solvent reclamation vaporizer 201 to carry out manipulation of regeneration.
The extraction agent that recycles, because causing, the coking meeting contains solid particle polluter in the solvent, need regularly or continuously to remove, from the first solvent recovery tower 114 or the second solvent recovery tower 124 tower reactors, intermittently drawing one sends into solvent reclamation vaporizer 201 and carries out manipulation of regeneration, the solvent that steams enters regenerated solvent tank 205 after by regenerated solvent condenser 203 and 204 condensations of regenerated solvent aftercooler, and returns thus solvent systems and reuse.Restructuring minute impurity is discharged by regenerated solvent surge tank 202 bottoms.Solvent regeneration system adopts vacuum operating, and working pressure is that absolute pressure 30kPa(is suitable at 20kPa ~ 60kPa), the non-condensable gas of regenerated solvent aftercooler 204 is extracted out by vacuum pump 206.
The isohexane product 2-methylpentane and the 3-methylpentane total mass mark that adopt the technology of the present invention to produce are not less than 95%, and benzene content is less than 100ppm.
Adopt normal hexane product indices that the technology of the present invention produces except can being up to state standards GB16629-2008, outside the company standard Q/SH PRD0406-2011 of China PetroChemical Corporation, and can reach the normal hexane massfraction and be not less than 99% requirement.
The benzaldehyde product that adopts the technology of the present invention the to produce GB3405-89 that is up to state standards.
Embodiment 2
Separation method according to a kind of isohexane of the present invention, normal hexane and benzene, from mixed feedstocks of hydrocarbons such as the raffinating oil of aromatic extraction unit, pyrolysis gasoline or straight-run spirit, at first remove than the low-boiling impurity of 2-methylpentane, then isolate the mixing hexane that does not contain benzene by extraction rectifying method.Mix hexane and further be separated into isohexane product and normal hexane product.Remove the material that mixes behind the hexane, obtaining benzaldehyde product after separating through follow-up extraction rectifying method.The difference of the present embodiment and embodiment one is, adopt the benzene refining unit to obtain benzaldehyde product.
Technical process mainly comprises such as lower unit: lights removal unit, hexane extraction rectification cell, hexane separating unit, the first solvent recovery unit, benzene extracting rectifying unit, the second solvent recovery unit, benzene refining unit and solvent reclamation unit.Below in conjunction with accompanying drawing above-mentioned each unit is described.
From the total hydrocarbon feed outside the battery limit (BL) after the feed preheater preheating, from lightness-removing column 101 top chargings, overhead vapours is after condenser of light component removal column 102 condensations, and lime set enters lightness-removing column return tank 103 part and refluxes, another part as the light constituent product from the return tank extraction.The lightness-removing column still arranges reboiler 104.This tower adopts pressurized operation to guarantee that overhead vapours can be recycled cooling water condensation, and working pressure is that absolute pressure 130kPa(is suitable at 150kPa ~ 300kPa).The component of overhead extraction stream thigh is mainly pentamethylene, the boiling point light hydrocarbons impurity lower than 2-methylpentane such as 2,2-methylbutane.Lightness-removing column 101 a tower reactors stream strand chief component is isohexane, normal hexane and benzene, sends into hexane extraction rectifying tower 105 and carries out later separation.
From the stream thigh of lightness-removing column still from the 105 middle part chargings of hexane extraction rectifying tower, the extraction agent N-Methyl pyrrolidone (just exemplifies a kind of extraction agent here, the extraction agent that summary of the invention is mentioned all is suitable for) from feed plate top charging, the add-on of extraction agent is 4 times (they can also be 3 times ~ 6 times) of inlet amount.The effect of extraction agent has increased hexane and methylcyclopentane, the relative volatility of hexane and benzene, thus the clear cutting of hexane and benzene is achieved.Under the effect of extraction agent, material is interior through repeatedly gasification at hexane extraction rectifying tower 105, realize behind the multiple condensation separating, overhead vapours obtains mixing hexane after 106 condensations of hexane extraction rectifying tower condenser, enter hexane and get rectifying tower return tank 107, a part refluxes, and the rest part extraction send hexane knockout tower 109 further to separate.Interchanger 108 is hexane extraction rectifying tower reactor reboiler, and the rich benzene extraction agent solution that tower reactor obtains is sent into the first solvent recovery tower 114 and carried out solvent recuperation.
After the mixing hexane entered hexane knockout tower 109, isohexane was realized separating with normal hexane behind abundant vapour-liquid heat and mass, and overhead vapours enters hexane knockout tower return tank 111 after 110 condensations of hexane separation column condenser, and a part refluxes; Rest part is as the extraction of isohexane product, and wherein 2-methylpentane and 3-methylpentane total concn are about 95%, and benzene content is lower than 100ppm.Interchanger 112 is the tower reactor reboiler of hexane knockout tower 109.Normal hexane for the tower reactor extraction, massfraction is higher than 99.0%, wherein benzene content is less than 100ppm, after delivering to normal hexane the first preheater 301 and normal hexane the second preheater 302 and being preheated to 150 ℃ (can also be 120 ℃ ~ 200 ℃), process through bleaching earth adsorption bed 303 again, can make the normal hexane product indices GB16629-2008 that can be up to state standards, the company standard Q/SH PRD0406-2011 of China PetroChemical Corporation, and the normal hexane massfraction is not less than 99%.
Rich benzene extraction agent solution is realized separating behind the 114 interior process vapour-liquids heat transfers of the first solvent recovery tower, mass transfer, cat head steams benzene and non-aromatics mixture, enters the first solvent recovery tower return tank 117 after the first solvent recovery tower condenser 115 and 116 condensations of the first solvent recovery tower aftercooler.This tower adopts vacuum operating, and working pressure is that absolute pressure 30kPa(is suitable in 20kPa ~ 60kPa scope), the non-condensable gas of the first solvent recovery tower aftercooler 116 is extracted out by vacuum pump 133.Wherein the first solvent recovery tower condenser 115 adopts recirculated cooling water to do heat-eliminating medium, and temperature out is controlled in 37 ~ 47 ℃ of scopes; The first solvent recovery tower aftercooler 116 adopts low-temperature cooling water to make heat-eliminating medium, and temperature out is controlled in 20 ~ 30 ℃ of scopes.The first solvent recovery tower return tank 117 interior material parts reflux, and all the other are sent into benzene extractive distillation column 119 and further separate.The first solvent recovery tower 114 tower reactors reclaim extraction agent N-methyl-pyrrolidone, and major part is returned hexane extraction rectifying tower 107 and recycled after 113 coolings of extraction agent water cooler, and small part send 201 to carry out manipulation of regeneration.Interchanger 118 is the tower reactor reboiler of the first solvent recovery tower 114.
Benzene and non-aromatics mixture from the first solvent recovery tower return tank 117, top charging from benzene extractive distillation column 119, extraction agent N-methyl-pyrrolidone (just exemplifies a kind of extraction agent here, the extraction agent that summary of the invention is mentioned all is suitable for) added by the feed plate top, the add-on of extraction agent is 5 times (all being suitable for 3 ~ 6 times of scopes) of benzene extractive distillation column 119 inlet amounies.Under the effect of extraction agent, aromatic hydrocarbons and non-aromatics realize separating, the steam of non-aromatic hydro carbons by 120 condensations of benzene extractive distillation column condenser after, enter benzene extractive distillation column return tank 121 parts and reflux, rest part is as the extraction of solvent oil product.Interchanger 122 is the tower reactor reboiler of benzene extractive distillation column 119, and the mixture of benzene and extraction agent is sent into the second molten recovery tower 124 and recycled from the tower reactor extraction.
Separate at the second solvent recovery tower 124 from the benzene of benzene extractive distillation column 119 tower reactors and the mixture of extraction agent, overhead vapours is after the second solvent recovery tower condenser 125 and 126 condensations of the second solvent recovery tower aftercooler, enter the second solvent recovery tower return tank 127, partial reflux, the rest part extraction.The material of extraction part is delivered to bleaching earth adsorption bed 403 and is removed the impurity such as alkene after benzene the first preheater 401 and benzene the second preheater 402 are preheated to 150 ℃ (can also be 120 ℃ ~ 200 ℃), delivers to benzene refining tower 129 further refining again.
The second solvent recovery tower 124 towers adopt vacuum operating, and working pressure is that absolute pressure 30kPa(is suitable in 20kPa ~ 60kPa scope).The second solvent recovery tower condenser 125 adopts recirculated cooling water to do heat-eliminating medium, and temperature out is controlled in 37 ~ 47 ℃ of scopes; The second solvent recovery tower aftercooler 126 adopts low-temperature cooling water to make heat-eliminating medium, and temperature out is controlled in 20 ~ 30 ℃ of scopes.The non-condensable gas of the second solvent recovery tower aftercooler 126 is extracted out by vacuum pump 134.The second solvent recovery tower 124 tower reactors are solvent N-methyl-pyrrolidone, and major part is returned the benzene extractive distillation column through extraction agent and recycled after water cooler 123 coolings, and small portion send solvent reclamation vaporizer 201 to carry out manipulation of regeneration.
From the material of bleaching earth adsorption bed 403, behind benzene the first preheater 401 and the material-heat-exchanging from the second solvent recovery tower return tank 127, send into benzene refining tower 129 and separate.Benzene refining tower 129 overhead vapours enter benzene refining tower return tank 131 after 130 condensations of benzene refining tower condenser, the most of backflow, intermittently extraction light constituent impurity.Benzaldehyde product is by the top side line extraction of benzene refining tower 129, and the benzaldehyde product index can reach GB3405-89, and the benzene massfraction is not less than 99.9%.
The extraction agent that recycles, because causing, the coking meeting contains solid particle polluter in the solvent, need regularly or continuously to remove, from the first solvent recovery tower 114 or the second solvent recovery tower 124 tower reactors, intermittently drawing one sends into solvent reclamation vaporizer 201 and carries out manipulation of regeneration, the solvent that steams enters regenerated solvent tank 205 after by regenerated solvent condenser 203 and 204 condensations of regenerated solvent aftercooler, and returns thus solvent systems and reuse.Restructuring minute impurity is discharged by regenerated solvent surge tank 202 bottoms.Solvent regeneration system adopts vacuum operating, and working pressure is that absolute pressure 30kPa(is suitable in 20kPa ~ 60kPa scope), the non-condensable gas of regenerated solvent aftercooler 204 is extracted out by vacuum pump 206.
The isohexane product 2-methylpentane and the 3-methylpentane total mass mark that adopt the technology of the present invention to produce are not less than 95%, and benzene content is less than 100ppm.
Adopt normal hexane product indices that the technology of the present invention produces except can being up to state standards GB16629-2008, outside the company standard Q/SH PRD0406-2011 of China PetroChemical Corporation, and can reach the normal hexane massfraction and be not less than 99% requirement.
The benzaldehyde product that adopts the technology of the present invention the to produce GB3405-89 that is up to state standards.
Claims (6)
1. method of separating isohexane, normal hexane and benzaldehyde product: it is characterized in that comprising lights removal unit, hexane extraction rectification cell, hexane separating unit, the first solvent recovery unit, benzene extracting rectifying unit, the second solvent recovery unit and solvent reclamation unit; From mixed feedstocks of hydrocarbons such as the raffinating oil of aromatic extraction unit, pyrolysis gasoline or straight-run spirit, at first remove than the low-boiling impurity of 2-methylpentane, then isolate the mixing hexane that does not contain benzene by extraction rectifying method; Mix hexane and further be separated into isohexane product and normal hexane product; Remove the material that mixes behind the hexane, obtaining benzaldehyde product after separating through extraction rectifying method again.
2. realize the equipment of claim 2 method, it is characterized in that being composed in series with flow direction of material by lightness-removing column (101), hexane extraction rectifying tower (105), hexane knockout tower (109), the first solvent recovery tower (114), benzene extractive distillation column (119) and the second solvent recovery tower (124); Each tower top is provided with condenser, condenser is connected with return tank, and the bottom is provided with reboiler; Hexane knockout tower (109) tower reactor connects normal hexane bleaching earth adsorption bed (303); The second solvent recovery tower (124) return tank of top of the tower (127) connects benzene bleaching earth adsorption bed (403); The first solvent recovery tower (114) be connected solvent recovery tower (124) tower reactor and connect solvent reclamation vaporizer (201).
3. adopt equipment as claimed in claim 2 to separate the method for isohexane, normal hexane and benzaldehyde product, it is characterized in that from the mixed feedstocks of hydrocarbons outside the battery limit (BL) after the feed preheater preheating, send into lightness-removing column (101), from lightness-removing column (101) removed overhead than the low-boiling light constituent impurity of 2-methylpentane after, send into hexane extraction rectifying tower (105) again and separate, hexane extraction rectifying tower (105) overhead extraction does not contain the mixing hexane stream thigh of benzene; The mixture flow thigh of hexane extraction rectifying tower (105) tower reactor extraction solvent, benzene and a small amount of non-aromatics; Mixing hexane stream thigh is sent into hexane knockout tower (109) and is separated, send into basin at hexane knockout tower (109) overhead extraction stream thigh as the isohexane product, obtain normal hexane product after the normal hexane stream stock-traders' know-how bleaching earth adsorption bed (303) of hexane knockout tower (109) tower reactor extraction is processed and send into basin; Hexane extraction rectifying tower (105) still material is sent into the first solvent recovery tower (114) and is separated, be recycled solvent in the first solvent recovery tower (114) tower reactor, major part is returned hexane and is got rectifying tower (105) Reusability after cooling, rest part send solvent reclamation vaporizer (201) to carry out impurities removal; The first solvent recovery tower (114) cat head obtains the mixture of benzene and non-aromatics impurity, and sends into benzene extractive distillation column (119) and separate, and from benzene extracting rectifying (119) removed overhead non-aromatics impurity, and sends into basin as the solvent oil product; Benzene extracting rectifying (119) tower reactor is the mixed flow thigh of benzene and extraction agent, send the second solvent recovery tower (124) to separate, be recycled solvent in the second solvent recovery tower (124) tower reactor, major part is returned benzene extractive distillation column (119) Reusability after cooling, rest part send solvent reclamation vaporizer (201) to carry out impurities removal; After the benzene stream stock-traders' know-how bleaching earth adsorption bed (403) of the second solvent recovery tower (124) overhead extraction is processed, after cooling, get benzaldehyde product.
4. method as claimed in claim 3 is characterized in that the lightness-removing column working pressure is absolute pressure 130 ~ 300kPa; Hexane extraction rectifying tower, hexane knockout tower, benzene extractive distillation column and benzene refining tower working pressure are normal pressure; The first solvent recovery tower and the second solvent recovery tower vacuum operating, the working pressure of this two tower is absolute pressure 20 ~ 60kPa; Regeneration vaporizer 201 is falling-film evaporator, and working pressure is absolute pressure 20 ~ 60kPa; Filler particles carclazyte in the bleaching earth adsorption bed, the service temperature of bleaching earth adsorption bed 303 is 120 ℃ ~ 200 ℃, working pressure is than the high 100 ~ 200kPa of saturated vapor pressure of normal hexane under the selected service temperature; The service temperature of bleaching earth adsorption bed 403 is 120 ℃ ~ 200 ℃, and working pressure is than the high 100 ~ 200kPa of saturation pressure of benzene under the selected service temperature.
5. method as claimed in claim 3 is characterized in that hexane extraction rectifying tower and the adoptable extraction agent of benzene extractive distillation column comprise glycols, N-Methyl pyrrolidone, tetramethylene sulfone, dimethyl sulfoxide (DMSO), N-formyl morpholine or be one or several the composite extractant in above-mentioned; Extraction agent and n-hexane extraction rectifying tower that benzene extracting rectification tower adopts are identical or different.
6. method as claimed in claim 5 is characterized in that the tower extraction agent is added by the feed plate top, and add-on is 3 ~ 6 times of hexane tower charging quality.
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| RU2568114C2 (en) * | 2014-03-13 | 2015-11-10 | Общество с ограниченной ответственностью "Производственное объединение "Киришинефтеоргсинтез" | Method of separating benzene from mixtures with non-aromatic hydrocarbons |
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| CN110819442A (en) * | 2019-11-07 | 2020-02-21 | 岳阳金瀚高新技术股份有限公司 | Grease leaching solvent and preparation method thereof |
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