CN104692995A - Process for producing benzene, methylbenzene and xylene from crude benzene - Google Patents
Process for producing benzene, methylbenzene and xylene from crude benzene Download PDFInfo
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Abstract
The invention discloses a process for producing benzene, methylbenzene and xylene from crude benzene. Various impurities, mainly containing thiophene, in the crude benzene are all removed by use of a low-temperature hydrogenation method, wherein all the sulfides (such as thiophene, methylthiophene and carbon disulfide) are converted into H2S and low carbon hydrocarbons, the nitrides are converted into NH3 and arenes or alkanes, the oxides are converted into H2O and arenes or alkanes, and the unsaturated hydrocarbons are saturated by hydrogenation; and next, the impurities are removed by virtue of conventional rectification and extraction rectification. As a result, the benzene, the methylbenzene and the xylene all having good quality can be produced.
Description
Technical field
The present invention relates to crude benzol reprocessing technical field, particularly relate to a kind of technique producing benzene, toluene and dimethylbenzene from crude benzol.
Background technology
Benzene is one of important petrochemical industry work basic raw material, can be used for a series of important Chemicals such as synthetic rubber, synthetic resins, synthon, medicine, agricultural chemicals, explosive and dyestuff.Also can be used as coating, rubber equal solvent simultaneously; In petroleum refining industry, benzene is the dopant improving gasoline octane rating.The production technology level of benzene and output have become one of important symbol of a measurement national oil development of chemical industry level.
Current benzene has 6 kinds of sources: catalytic reforming, pyrolysis gasoline, toluene disproportionation, Toluene Hydrogenation dealkylation, coke furnace light oil, coal tar.Wherein catalytic reforming and pyrolysis gasoline benzene respectively account for 38%, and toluene disproportionation accounts for 13%, and the benzene that Toluene Hydrogenation dealkylation is produced is 6%, and coking benzene is 5%.But the production and supply situation of country variant and regional benzene is not quite similar, and the benzene of the U.S. mainly obtains from reformed gasoline, and West Europe mainly obtains from pyrolysis gasoline.The downstream derivative thing of benzene mainly contains ethylbenzene, isopropyl benzene, hexanaphthene, oil of mirbane, and other derivative also has alkylbenzene, cis-butenedioic anhydride (maleic anhydride) and Benzene Chloride etc.
China is the country of an oil shortage, and coal resources are comparatively abundant, and country increases the dynamics of coal resource exploitation in recent years.The coke output of current China has reached more than 2.25 hundred million tons, and in the production process of coke, its coking benzene has more than 1,800,000 tons.Coking crude benzene because of its sulphur content higher, benzene content is more lower slightly than petroleum benzene, and its use range is restricted, and generally uses as solvent, but its price lower (with the price difference of petroleum benzene at 1500-2500 yuan/ton).Coking crude benzene is processed by hydrogenating desulfurization technology, coking crude benzene is under Hydrobon catalyst effect, adopt lower hydrogen partial pressure (about 1.0Mpa), lower temperature of reaction (200--280 DEG C), the sulphur content of coking crude benzene is made to be reduced to 2.0 below g/g by 1500 g/g--3750 g/g, nitrogen content is at 1.0 below g/g, and the saturation exponent of benzene is at below 1.0m%, benzene content is at more than 99.0m%, the content of benzene+hexanaphthene is at more than 99.80m%, quality product is improved greatly, both can be used as senior solvent, also can be used as preparing cyclohexanone, the raw material of hexanaphthene.
The benzene that current China produces, one is the coking benzene from coke by-products, and two is from the petroleum benzene of oil refining with ethylene unit.
The production equipment of current China aromatic hydrocarbons mainly adopts the reformer of refinery, the cracking of ethylene gasoline of petroleum chemical plant and aromatics production machinery and coker etc.In general, the ethylene producing device of 600,000 tons/year can coproduction benzene 120,000 ~ 140,000 tons/year, toluene 90,000 ~ 1.1 ten thousand tons/year, dimethylbenzene 80,000 ~ 90,000 tons/year; The reformer of 1000000 tons/year can produce benzene 60,000 ~ 70,000 tons/year, toluene 240,000 ~ 250,000 tons/year, dimethylbenzene 190,000 ~ 200,000 t/a; 5000000 tons/year of cokers can by-product crude benzol 50,000 ~ 70,000 tons/year, toluene and dimethylbenzene about totally 2 ten thousand tons/year.Toluene dealkylation, toluene disproportionation and transalkylation technology also can be utilized in addition by toluene and C
9/ C
10aromatic conversion is Mixed XYLENE and benzene, and in large-scale Aromatic Hydrocarbon United Plant, Mixed XYLENE over half is all produced by this technology, and this method is the main path of increasing yield of p-xylene. in addition, selective disproportionation of toluene is also a new way of producing p-Xylol.
Along with China's expanding economy, the import volume of triphen (benzene,toluene,xylene) and derived product thereof is increasing, although China's benzene yield reached record-breaking 306.11 ten thousand tons in 2005, the equivalent consumption of domestic nearly 8,000,000 tons far can not be met; In addition the equivalent consumption of China's p-Xylol has reached 8,450,000 tons, and domestic supply only has about 2,400,000 tons, can only the amount of satisfying the demands 28%.
China's development of iron & steel industry was very fast in recent years, had promoted the development of coking industry.Within 2005, China's coke ultimate production reaches 2.25 hundred million tons, increases by 27% on a year-on-year basis.Increasing substantially as the recovery of crude benzol and processing and utilization provide favourable condition of coke output.
Domestic and world market is in great demand to benzene,toluene,xylene at present, therefore need the higher more practical technique of efficiency from crude benzol, produce benzene, toluene and dimethylbenzene.
Summary of the invention
Object of the present invention is just to provide a kind of technique producing benzene, toluene and dimethylbenzene from crude benzol.The present invention adopts low temperature hydrogenation method all to be removed by the various impurity based on thiophene in crude benzol, and its medium sulphide content all (thiophene, thiotolene, dithiocarbonic anhydride etc.) is converted into H
2s and lower carbon number hydrocarbons, nitride converted is NH
3with aromatic hydrocarbons or alkane, oxygenate conversion is H
2o and aromatic hydrocarbons or alkane, hydrogenation of unsaturated hydrocarbons is saturated; Then conventional rectification and extracting rectifying removing impurity is adopted.Thus produce high-quality benzene, toluene and dimethylbenzene.
A kind of process technology scheme producing benzene, toluene and dimethylbenzene from crude benzol of the present invention is, crude benzol is after rectifying is except heavy seeds, and adopt low temperature hydrogenation method by the various impurity removings based on thiophene in crude benzol, wherein sulphidic conversion is H
2s and lower carbon number hydrocarbons, nitride converted is NH
3with aromatic hydrocarbons or alkane, oxygenate conversion is H
2o and aromatic hydrocarbons or alkane, hydrogenation of unsaturated hydrocarbons is saturated; Then adopt rectifying and extracting rectifying removing impurity, produce benzene, toluene and dimethylbenzene.
Crude benzol of the present invention is coking benzene.
Described a kind of technique producing benzene, toluene and dimethylbenzene from crude benzol, comprising:
(1) raw materials pretreatment operation;
(2) compression section;
(3) hydrogenation process;
(4) pre-rectification working process;
(5) rectification working process.
Step (1) is specially: coking crude benzene is squeezed in the middle part of hexichol tower by feedstock pump through under meter, the constant temperature thermal oil of 260 DEG C is adopted to utilize material in reboiler tower to heat up at the bottom of tower, automatically thermal oil flow is regulated according to column bottom temperature with variable valve, column bottom temperature is made to remain on about 200 DEG C, tower bottom pressure is pressure-fired, tower top fraction enters hexichol tower condensate cooler (water cooler employing air cooler), be cooled to 15-30 DEG C, then enter Horizontal oil-water separator and carry out oily water separation, the light benzene part separated is returned stream through under meter to tower top and is remained on 82-88 DEG C to make tower top temperature, tower top pressure is tiny structure, another part delivers to tank field storage through under meter, the heavy benzol of extraction at the bottom of hexichol tower is cooled to about 100 DEG C by water cooler, then delivers to tank field heavy benzol storage tank by pump through under meter.
Step (2) is specially: 1.0 ~ 1.2MPa(G) first fresh hydrogen enters hydrogen gas buffer, in surge tank, free-water and mechanical impurity precipitate under gravity, discharged by surge tank bottom blow-down valve timing, thus reach the object of free-water and the mechanical impurity separated wherein, and be then forced into 3.5MPa(G through hydrogen gas compressor) send into hydrogenation system; The circulating hydrogen that hydrogenation comes enters recycle hydrogen press and divides flow container, enters recycle hydrogen press, be forced into 3.5MPa(G with same principle after separating free-water wherein and mechanical impurity), send back to hydrogenation process.
Step (3) is specially: through pretreated light benzene as raw material by hydrogenating materials oil pump from tank field through under meter squeeze into stock oil interchanger and the heat exchange of hydrogenation reaction gas to 95-105 DEG C after, carry out mixing with the bottom that the circulating hydrogen after heating enters vaporizer simultaneously and vaporize, circulating hydrogen after the pressurization of recycle hydrogen press is introduced into hydrogen interchanger and the heat exchange of hydrogenation reaction gas to 135-145 DEG C, and flow is 1 cubic metre of raw material: 650-800 cube circulating hydrogen according to the ratio of circulating hydrogen and raw material, base of evaporator adopts 260 DEG C of constant temperature heat-conducting oil heating to 160-170 DEG C, discharges the evaporation Residual oil containing polymkeric substance from base of evaporator, after the slagging-off of evaporation Residual oil strainer, removes 100# heavy benzene water-and-oil separator, the mixed gas of top being discharged benzene class steam and hydrogen carries out heat exchange through interchanger and hydrogenation reaction gas, 180 DEG C are heated to by 260 DEG C of constant temperature heat-conducting oil heating at well heater, pre-reactor is entered by top, in the effect overdraft of NiMo catalyzer at 2.5-3.5 MPa(G) unsaturated compound hydrotreated lube base oil, reaction is thermopositive reaction, the mixture of reacted oil gas and hydrogen, out oil gas heat exchanger is entered bottom pre-reactor, be warming up to 220 DEG C laggard enter main reactor process furnace, be heated to 260 DEG C, after enter two series connection main reactors, under the effect of CoMo series catalysts, carry out desulfurization, decarburization, deoxidation, de-alkyl and non-aromatics scission reaction obtain hydrogenated oil, main reactor pressure is 2.5-3.5 MPa(G), bed temperature is 290 DEG C, reaction is thermopositive reaction, for controlling the temperature rise in reactor, add new hydrogen in the middle of main reactor, mixed gas is hydrogenation reaction gas, and new hydrogen temperature is room temperature, and the heat that reaction produces is walked by the hydrogenation reaction band of gas,
In step (3), from main reactor out add hydrogen mixed gas, through a series of interchanger and unstripped gas, circulating hydrogen heat exchange, lower the temperature after enter oil gas water cooler and be cooled to 25 ~ 30 DEG C, gas-liquid two-phase all enters that high-pressure separator carries out gas, liquid is separated; Isolated gas phase recycles; The hydrogenated oil separated goes to carry out rectification and purification;
The reaction occurred in pre-reactor is as follows:
Main reaction: (1) cyclopentadiene+hydrogen=pentamethylene
(2) other diolefine+hydrogen=monoolefines
(3) vinylbenzene+hydrogen=ethylbenzene
(4) indenes+hydrogen=indane
(5) dithiocarbonic anhydride+hydrogen=methane+hydrogen sulfide;
React in main reactor as follows:
Main reaction: (1) monoolefine+hydrogen=alkene
(2) mercaptan+hydrogen=ethane+hydrogen sulfide
(3) thiophene+hydrogen=butane+hydrogen sulfide
(4) phenol+hydrogen=benzene+water
(5) coumarone+hydrogen=ethylbenzene+water
(6) pyridine+hydrogen=pentane+ammonia
(7) aniline+hydrogen=ethane+ammonia
Side reaction: the hydrogenation reaction of (1) aromatic hydrocarbons
(2) benzene+hydrogen=hexanaphthene
(3) toluene+hydrogen=methylcyclohexane
In step (3), in order to suppress the polymerization of light benzene impurity, from stopper header tank by stopper according to 0.1 kilogram of stopper: the ratio of 1 ton of crude benzol, adds in the pipeline of conveying lightweight benzene oil; With soft water force (forcing) pump, soft water is squeezed into soft water header tank, then be that 600L to add in hydrogenation products solubilized and washes away partial impurities through metering by flow per hour; In circulation gas, density of hydrogen is more than 85%, need continuous blow-down part circulating hydrogen to gas line, simultaneously supplement a part of fresh hydrogen to maintain system balancing by compressor to system, magnitude of recruitment according to maintenance system pressure at 2.5-3.5 MPa(G) to carry out adjustment supplementary.
Step (4) is specially: the hydrogenated oil that step (3) obtains enters stabilizer tower through under meter governor valve control under High Pressure, at the bottom of stabilizer tower tower with thermal oil warm in 180 DEG C to stabilizer reboiler laser heating, column bottom temperature is made to remain on 145-150 DEG C, hydrogenated oil distills in tower, hydro carbons and the H be dissolved in hydrogenated oil of below C5
2the sour gas such as S are distilled out of is discharged by tower top; Overhead product is after below cold solidifying but to 40 of stabilizer tower condenser DEG C, enter stabilizer tower water-and-oil separator and carry out gas, water, oily three phase separation, gas phase is that non-condensable gases enters periodic off-gases pipeline through under meter governor valve control, oil phase leads back to stabilizer tower top and controls tower top temperature as backflow, tower top temperature is stabilized in about 90 DEG C, aqueous phase is discharged into sewage disposal, discharges BTX cut at the bottom of stabilizer tower tower;
BTX cut enters rectifying in the middle part of pre-distillation column, with 280 DEG C of high temperature heat conductive oils, reboiler is heated bottom pre-rectifying tower, column bottom temperature is made to remain on about 205 DEG C, tower bottom pressure remains on about 0.39 MPa, the hydro carbons such as hexanaphthene and Benzene and Toluene thing are discharged by tower top, go to enter water-and-oil separator to after the heating of purified petroleum benzin rectifying tower reboiler, oil phase part reflux pump after being separated is delivered to tower top and is returned stream and remain at the bottom of 137-139 DEG C of tower to control tower top temperature, tower top pressure is 0.3-0.4MPa, another part and BT component are delivered to tank field through under meter and are treated refining further under pressure itself, still liquid at the bottom of tower is delivered to tank field and is treated refining further.
Step (5) is specially: the BT component from tank field enters in the middle part of extraction tower by pump through under meter; At the bottom of extraction tower tower with thermal oil warm in 180 DEG C to extraction tower reboiler laser heating, maintain about 144 DEG C at the bottom of tower, tower bottom pressure is 28-35 Kpa, N-formyl morpholine N-be extraction agent by the charging of tower top, extraction agent: charging BT component is by weight=1:5.5-6.The stable hydrocarbon of carbon four, carbon five and carbon six carbon seven is discharged by tower top; Overhead product is delivered to tower top through condenser condenses to 25-30 DEG C of rear portion extraction tower reflux pump and is returned stream to control column bottom temperature 64-70 DEG C, and tower bottom pressure is-5K about Pa, and another part is that non-aromatics delivers to tank field storage;
Enter recycling design in the middle part of solvent regeneration tower from the rich solvent at the bottom of extraction tower tower, at the bottom of solvent regeneration tower tower with 260 DEG C of high temperature heat conductive oils to solvent tower reboiler laser heating, make to maintain about 170 DEG C at the bottom of tower, Benzene and Toluene is discharged by tower top; Overhead product is cooled to 15-35 DEG C of rear portion through condenser condenses and is used as trim the top of column, and control tower top temperature is 42-50 DEG C, and another part enters in the middle part of purified petroleum benzin rectifying tower; Solvent regeneration tower tower base solvent is squeezed into extraction tower reboiler by solvent pump and is reclaimed heat, then enters extraction tower feed heater and reclaim heat further; Solvent regeneration tower adopts negative-pressure operation, vacuumizes, make tower internal pressure remain on-0.072 MPa with vacuum pump set from tower top to solvent regeneration tower;
Benzene and Toluene tower from solvent regeneration tower enters in the middle part of purified petroleum benzin rectifying tower, with the benzene class steam heated reboiler laser heating that pre-rectifying tower tower top flows out at the bottom of tower, column bottom temperature is about 114 DEG C, tower bottom pressure 6-8 KPa, Benzene and Toluene is separated in tower, and purified petroleum benzin is discharged by tower top, and overhead product is cooled to 15-30 DEG C of rear portion through condenser condenses and returns stream through under meter to tower top, control column bottom temperature is 65-68 DEG C, and tower bottom pressure is-15 MPa; Another part purified petroleum benzin product delivers to tank field storage through under meter; After toluene product discharges cooling by tower reactor liquid phase, tank sending district stores;
Pre-rectifying tower still liquid XS component from tank field delivers to benzenol hydrorefining batch fractionating; In order at the bottom of the benzenol hydrorefining reboiler laser heating tower of warm heat-conducting oil heating in 160 DEG C at the bottom of benzenol hydrorefining tower, tower bottom pressure 15-30 KPa, XS component is distilled in tower, and the low-boiling point material such as dimethylbenzene, ethylbenzene is discharged by tower top; Overhead product is cooled to 15-30 DEG C of laggard top through condenser condenses and returns stream, controls column bottom temperature and is no more than 143 DEG C, and a part delivers to tank field storage through under meter as product; Benzenol hydrorefining tower bottoms tank sending district stores.
Beneficial effect of the present invention is: the present invention adopts coking benzene as waste benzene, toluene and dimethylbenzene, process costs is low, easy to operate, be convenient to suitability for industrialized production, practicality is high, can produce high-quality benzene, toluene and dimethylbenzene, quality product is up to state standards simultaneously, fully can meet domestic and world market to the demand of benzene,toluene,xylene.
embodiment:
In order to understand the present invention better, describe technical scheme of the present invention in detail with specific examples below, but the present invention is not limited thereto.
Raw material of the present invention is coking benzene.
Embodiment 1
A kind of process technology scheme producing benzene, toluene and dimethylbenzene from crude benzol of the present invention is, crude benzol is after rectifying is except heavy seeds, and adopt low temperature hydrogenation method by the various impurity removings based on thiophene in crude benzol, wherein sulphidic conversion is H
2s and lower carbon number hydrocarbons, nitride converted is NH
3with aromatic hydrocarbons or alkane, oxygenate conversion is H
2o and aromatic hydrocarbons or alkane, hydrogenation of unsaturated hydrocarbons is saturated; Then adopt rectifying and extracting rectifying removing impurity, produce benzene, toluene and dimethylbenzene.
Crude benzol of the present invention is coking benzene.
Described a kind of technique producing benzene, toluene and dimethylbenzene from crude benzol, comprising:
(1) raw materials pretreatment operation;
(2) compression section;
(3) hydrogenation process;
(4) pre-rectification working process;
(5) rectification working process.
Step (1) is specially: coking crude benzene is squeezed in the middle part of hexichol tower by feedstock pump through under meter, the constant temperature thermal oil of 260 DEG C is adopted to utilize material in reboiler tower to heat up at the bottom of tower, automatically thermal oil flow is regulated according to column bottom temperature with variable valve, column bottom temperature is made to remain on about 200 DEG C, tower bottom pressure is pressure-fired, tower top fraction enters hexichol tower condensate cooler (water cooler employing air cooler), be cooled to 15-30 DEG C, then enter Horizontal oil-water separator and carry out oily water separation, the light benzene part separated is returned stream through under meter to tower top and is remained on 82-88 DEG C to make tower top temperature, tower top pressure is tiny structure, another part delivers to tank field storage through under meter, the heavy benzol of extraction at the bottom of hexichol tower is cooled to about 100 DEG C by water cooler, then delivers to tank field heavy benzol storage tank by pump through under meter.
Step (2) is specially: 1.0 ~ 1.2MPa(G) first fresh hydrogen enters hydrogen gas buffer, in surge tank, free-water and mechanical impurity precipitate under gravity, discharged by surge tank bottom blow-down valve timing, thus reach the object of free-water and the mechanical impurity separated wherein, and be then forced into 3.5MPa(G through hydrogen gas compressor) send into hydrogenation system; The circulating hydrogen that hydrogenation comes enters recycle hydrogen press and divides flow container, enters recycle hydrogen press, be forced into 3.5MPa(G with same principle after separating free-water wherein and mechanical impurity), send back to hydrogenation process.
Step (3) is specially: through pretreated light benzene as raw material by hydrogenating materials oil pump from tank field through under meter squeeze into stock oil interchanger and the heat exchange of hydrogenation reaction gas to 95-105 DEG C after, carry out mixing with the bottom that the circulating hydrogen after heating enters vaporizer simultaneously and vaporize, circulating hydrogen after the pressurization of recycle hydrogen press is introduced into hydrogen interchanger and the heat exchange of hydrogenation reaction gas to 135-145 DEG C, and flow is 1 cubic metre of raw material: 650-800 cube circulating hydrogen according to the ratio of circulating hydrogen and raw material, base of evaporator adopts 260 DEG C of constant temperature heat-conducting oil heating to 160-170 DEG C, discharges the evaporation Residual oil containing polymkeric substance from base of evaporator, after the slagging-off of evaporation Residual oil strainer, removes 100# heavy benzene water-and-oil separator, the mixed gas of top being discharged benzene class steam and hydrogen carries out heat exchange through interchanger and hydrogenation reaction gas, 180 DEG C are heated to by 260 DEG C of constant temperature heat-conducting oil heating at well heater, pre-reactor is entered by top, in the effect overdraft of NiMo catalyzer at 2.5-3.5 MPa(G) unsaturated compound hydrotreated lube base oil, reaction is thermopositive reaction, the mixture of reacted oil gas and hydrogen, out oil gas heat exchanger is entered bottom pre-reactor, be warming up to 220 DEG C laggard enter main reactor process furnace, be heated to 260 DEG C, after enter two series connection main reactors, under the effect of CoMo series catalysts, carry out desulfurization, decarburization, deoxidation, de-alkyl and non-aromatics scission reaction obtain hydrogenated oil, main reactor pressure is 2.5-3.5 MPa(G), bed temperature is 290 DEG C, reaction is thermopositive reaction, for controlling the temperature rise in reactor, add new hydrogen in the middle of main reactor, mixed gas is hydrogenation reaction gas, and new hydrogen temperature is room temperature, and the heat that reaction produces is walked by the hydrogenation reaction band of gas,
In step (3), from main reactor out add hydrogen mixed gas, through a series of interchanger and unstripped gas, circulating hydrogen heat exchange, lower the temperature after enter oil gas water cooler and be cooled to 25 ~ 30 DEG C, gas-liquid two-phase all enters that high-pressure separator carries out gas, liquid is separated; Isolated gas phase recycles; The hydrogenated oil separated goes to carry out rectification and purification;
The reaction occurred in pre-reactor is as follows:
Main reaction: (1) cyclopentadiene+hydrogen=pentamethylene
(2) other diolefine+hydrogen=monoolefines
(3) vinylbenzene+hydrogen=ethylbenzene
(4) indenes+hydrogen=indane
(5) dithiocarbonic anhydride+hydrogen=methane+hydrogen sulfide;
React in main reactor as follows:
Main reaction: (1) monoolefine+hydrogen=alkene
(2) mercaptan+hydrogen=ethane+hydrogen sulfide
(3) thiophene+hydrogen=butane+hydrogen sulfide
(4) phenol+hydrogen=benzene+water
(5) coumarone+hydrogen=ethylbenzene+water
(6) pyridine+hydrogen=pentane+ammonia
(7) aniline+hydrogen=ethane+ammonia
Side reaction: the hydrogenation reaction of (1) aromatic hydrocarbons
(2) benzene+hydrogen=hexanaphthene
(3) toluene+hydrogen=methylcyclohexane
In step (3), in order to suppress the polymerization of light benzene impurity, from stopper header tank by stopper according to 0.1 kilogram of stopper: the ratio of 1 ton of crude benzol, adds in the pipeline of conveying lightweight benzene oil; With soft water force (forcing) pump, soft water is squeezed into soft water header tank, then be that 600L to add in hydrogenation products solubilized and washes away partial impurities through metering by flow per hour; In circulation gas, density of hydrogen is more than 85%, need continuous blow-down part circulating hydrogen to gas line, simultaneously supplement a part of fresh hydrogen to maintain system balancing by compressor to system, magnitude of recruitment according to maintenance system pressure at 2.5-3.5 MPa(G) to carry out adjustment supplementary.
Step (4) is specially: the hydrogenated oil that step (3) obtains enters stabilizer tower through under meter governor valve control under High Pressure, at the bottom of stabilizer tower tower with thermal oil warm in 180 DEG C to stabilizer reboiler laser heating, column bottom temperature is made to remain on 145-150 DEG C, hydrogenated oil distills in tower, hydro carbons and the H be dissolved in hydrogenated oil of below C5
2the sour gas such as S are distilled out of is discharged by tower top; Overhead product is after below cold solidifying but to 40 of stabilizer tower condenser DEG C, enter stabilizer tower water-and-oil separator and carry out gas, water, oily three phase separation, gas phase is that non-condensable gases enters periodic off-gases pipeline through under meter governor valve control, oil phase leads back to stabilizer tower top and controls tower top temperature as backflow, tower top temperature is stabilized in about 90 DEG C, aqueous phase is discharged into sewage disposal, discharges BTX cut at the bottom of stabilizer tower tower;
BTX cut enters rectifying in the middle part of pre-distillation column, with 280 DEG C of high temperature heat conductive oils, reboiler is heated bottom pre-rectifying tower, column bottom temperature is made to remain on about 205 DEG C, tower bottom pressure remains on about 0.39 MPa, the hydro carbons such as hexanaphthene and Benzene and Toluene thing are discharged by tower top, go to enter water-and-oil separator to after the heating of purified petroleum benzin rectifying tower reboiler, oil phase part reflux pump after being separated is delivered to tower top and is returned stream and remain at the bottom of 137-139 DEG C of tower to control tower top temperature, tower top pressure is 0.3-0.4MPa, another part and BT component are delivered to tank field through under meter and are treated refining further under pressure itself, still liquid at the bottom of tower is delivered to tank field and is treated refining further.
Step (5) is specially: the BT component from tank field enters in the middle part of extraction tower by pump through under meter; At the bottom of extraction tower tower with thermal oil warm in 180 DEG C to extraction tower reboiler laser heating, maintain about 144 DEG C at the bottom of tower, tower bottom pressure is 28-35 Kpa, N-formyl morpholine N-be extraction agent by the charging of tower top, extraction agent: charging BT component is by weight=1:5.5-6.The stable hydrocarbon of carbon four, carbon five and carbon six carbon seven is discharged by tower top; Overhead product is delivered to tower top through condenser condenses to 25-30 DEG C of rear portion extraction tower reflux pump and is returned stream to control column bottom temperature 64-70 DEG C, and tower bottom pressure is-5K about Pa, and another part is that non-aromatics delivers to tank field storage;
Enter recycling design in the middle part of solvent regeneration tower from the rich solvent at the bottom of extraction tower tower, at the bottom of solvent regeneration tower tower with 260 DEG C of high temperature heat conductive oils to solvent tower reboiler laser heating, make to maintain about 170 DEG C at the bottom of tower, Benzene and Toluene is discharged by tower top; Overhead product is cooled to 15-35 DEG C of rear portion through condenser condenses and is used as trim the top of column, and control tower top temperature is 42-50 DEG C, and another part enters in the middle part of purified petroleum benzin rectifying tower; Solvent regeneration tower tower base solvent is squeezed into extraction tower reboiler by solvent pump and is reclaimed heat, then enters extraction tower feed heater and reclaim heat further; Solvent regeneration tower adopts negative-pressure operation, vacuumizes, make tower internal pressure remain on-0.072 MPa with vacuum pump set from tower top to solvent regeneration tower;
Benzene and Toluene tower from solvent regeneration tower enters in the middle part of purified petroleum benzin rectifying tower, with the benzene class steam heated reboiler laser heating that pre-rectifying tower tower top flows out at the bottom of tower, column bottom temperature is about 114 DEG C, tower bottom pressure 6-8 KPa, Benzene and Toluene is separated in tower, and purified petroleum benzin is discharged by tower top, and overhead product is cooled to 15-30 DEG C of rear portion through condenser condenses and returns stream through under meter to tower top, control column bottom temperature is 65-68 DEG C, and tower bottom pressure is-15 MPa; Another part purified petroleum benzin product delivers to tank field storage through under meter; After toluene product discharges cooling by tower reactor liquid phase, tank sending district stores;
Pre-rectifying tower still liquid XS component from tank field delivers to benzenol hydrorefining batch fractionating; In order at the bottom of the benzenol hydrorefining reboiler laser heating tower of warm heat-conducting oil heating in 160 DEG C at the bottom of benzenol hydrorefining tower, tower bottom pressure 15-30 KPa, XS component is distilled in tower, and the low-boiling point material such as dimethylbenzene, ethylbenzene is discharged by tower top; Overhead product is cooled to 15-30 DEG C of laggard top through condenser condenses and returns stream, controls column bottom temperature and is no more than 143 DEG C, and a part delivers to tank field storage through under meter as product; Benzenol hydrorefining tower bottoms tank sending district stores.
Purified petroleum benzin quality prepared by present invention process is as shown in table 1
table 1
。
Toluene quality prepared by present invention process is as shown in table 2
table 2
。
Xylene mass prepared by present invention process is as shown in table 3
table 3
。
Claims (9)
1. from crude benzol, produce a technique for benzene, toluene and dimethylbenzene, it is characterized in that, crude benzol is after rectifying is except heavy seeds, and adopt low temperature hydrogenation method by the various impurity removings based on thiophene in crude benzol, wherein sulphidic conversion is H
2s and lower carbon number hydrocarbons, nitride converted is NH
3with aromatic hydrocarbons or alkane, oxygenate conversion is H
2o and aromatic hydrocarbons or alkane, hydrogenation of unsaturated hydrocarbons is saturated; Then adopt rectifying and extracting rectifying removing impurity, produce benzene, toluene and dimethylbenzene.
2. a kind of technique producing benzene, toluene and dimethylbenzene from crude benzol according to claim 1, is characterized in that, crude benzol of the present invention is coking benzene.
3. a kind of technique producing benzene, toluene and dimethylbenzene from crude benzol according to claim 1, is characterized in that, comprising:
(1) raw materials pretreatment operation;
(2) compression section;
(3) hydrogenation process;
(4) pre-rectification working process;
(5) rectification working process.
4. one according to claim 3 produces benzene from crude benzol, the technique of toluene and dimethylbenzene, it is characterized in that, step (1) is specially: coking crude benzene is squeezed in the middle part of hexichol tower by feedstock pump through under meter, the constant temperature thermal oil of 260 DEG C is adopted to utilize material in reboiler tower to heat up at the bottom of tower, automatically thermal oil flow is regulated according to column bottom temperature with variable valve, column bottom temperature is made to remain on about 200 DEG C, tower bottom pressure is pressure-fired, tower top fraction enters hexichol tower condensate cooler, be cooled to 15-30 DEG C, then enter Horizontal oil-water separator and carry out oily water separation, the light benzene part separated is returned stream through under meter to tower top and is remained on 82-88 DEG C to make tower top temperature, tower top pressure is tiny structure, another part delivers to tank field storage through under meter, the heavy benzol of extraction at the bottom of hexichol tower is cooled to about 100 DEG C by water cooler, then delivers to tank field heavy benzol storage tank by pump through under meter.
5. a kind of technique producing benzene, toluene and dimethylbenzene from crude benzol according to claim 3, it is characterized in that, step (2) is specially: first 1.0 ~ 1.2MPa fresh hydrogen enters hydrogen gas buffer, in surge tank, free-water and mechanical impurity precipitate under gravity, discharged by surge tank bottom blow-down valve timing, thus reach the object of free-water and the mechanical impurity separated wherein, be then forced into 3.5MPa through hydrogen gas compressor and send into hydrogenation system; The circulating hydrogen that hydrogenation comes enters recycle hydrogen press and divides flow container, enters recycle hydrogen press, be forced into 3.5MPa, send back to hydrogenation process with same principle after separating free-water wherein and mechanical impurity.
6. a kind of technique producing benzene, toluene and dimethylbenzene from crude benzol according to claim 4, it is characterized in that, step (3) is specially: through pretreated light benzene as raw material by hydrogenating materials oil pump from tank field through under meter squeeze into stock oil interchanger and the heat exchange of hydrogenation reaction gas to 95-105 DEG C after, carry out mixing with the bottom that the circulating hydrogen after heating enters vaporizer simultaneously and vaporize, circulating hydrogen after the pressurization of recycle hydrogen press is introduced into hydrogen interchanger and the heat exchange of hydrogenation reaction gas to 135-145 DEG C, and flow is 1 cubic metre of raw material: 650-800 cube circulating hydrogen according to the ratio of circulating hydrogen and raw material, base of evaporator adopts 260 DEG C of constant temperature heat-conducting oil heating to 160-170 DEG C, discharges the evaporation Residual oil containing polymkeric substance from base of evaporator, after the slagging-off of evaporation Residual oil strainer, removes 100# heavy benzene water-and-oil separator, the mixed gas of top being discharged benzene class steam and hydrogen carries out heat exchange through interchanger and hydrogenation reaction gas, 180 DEG C are heated to by 260 DEG C of constant temperature heat-conducting oil heating at well heater, pre-reactor is entered by top, in the effect overdraft of NiMo catalyzer at 2.5-3.5 MPa unsaturated compound hydrotreated lube base oil, reaction is thermopositive reaction, the mixture of reacted oil gas and hydrogen, out oil gas heat exchanger is entered bottom pre-reactor, be warming up to 220 DEG C laggard enter main reactor process furnace, be heated to 260 DEG C, after enter two series connection main reactors, under the effect of CoMo series catalysts, carry out desulfurization, decarburization, deoxidation, de-alkyl and non-aromatics scission reaction obtain hydrogenated oil, main reactor pressure is 2.5-3.5 MPa, bed temperature is 290 DEG C, reaction is thermopositive reaction, for controlling the temperature rise in reactor, add new hydrogen in the middle of main reactor, mixed gas is hydrogenation reaction gas, and new hydrogen temperature is room temperature, and the heat that reaction produces is walked by the hydrogenation reaction band of gas,
A kind of technique producing benzene, toluene and dimethylbenzene from crude benzol according to claim 5, it is characterized in that, in step (3), from main reactor out add hydrogen mixed gas, through a series of interchanger and unstripped gas, circulating hydrogen heat exchange, lower the temperature after enter oil gas water cooler and be cooled to 25 ~ 30 DEG C, gas-liquid two-phase all enters that high-pressure separator carries out gas, liquid is separated; Isolated gas phase recycles; The hydrogenated oil separated goes to carry out rectification and purification;
The reaction occurred in pre-reactor is as follows:
Main reaction: (1) cyclopentadiene+hydrogen=pentamethylene
(2) other diolefine+hydrogen=monoolefines
(3) vinylbenzene+hydrogen=ethylbenzene
(4) indenes+hydrogen=indane
(5) dithiocarbonic anhydride+hydrogen=methane+hydrogen sulfide;
React in main reactor as follows:
Main reaction: (1) monoolefine+hydrogen=alkene
(2) mercaptan+hydrogen=ethane+hydrogen sulfide
(3) thiophene+hydrogen=butane+hydrogen sulfide
(4) phenol+hydrogen=benzene+water
(5) coumarone+hydrogen=ethylbenzene+water
(6) pyridine+hydrogen=pentane+ammonia
(7) aniline+hydrogen=ethane+ammonia
Side reaction: the hydrogenation reaction of (1) aromatic hydrocarbons
(2) benzene+hydrogen=hexanaphthene
(3) toluene+hydrogen=methylcyclohexane
A kind of technique producing benzene, toluene and dimethylbenzene from crude benzol according to claim 6, it is characterized in that, in step (3), in order to suppress the polymerization of light benzene impurity, from stopper header tank by stopper according to 0.1 kilogram of stopper: the ratio of 1 ton of crude benzol, adds in the pipeline of conveying lightweight benzene oil; With soft water force (forcing) pump, soft water is squeezed into soft water header tank, then be that 600L to add in hydrogenation products solubilized and washes away partial impurities through metering by flow per hour; In circulation gas, density of hydrogen is more than 85%, need continuous blow-down part circulating hydrogen to gas line, supplement a part of fresh hydrogen to maintain system balancing by compressor to system, magnitude of recruitment carries out adjustment according to maintenance system pressure at 2.5-3.5 MPa and supplements simultaneously.
7. a kind of technique producing benzene, toluene and dimethylbenzene from crude benzol according to claim 7, it is characterized in that, step (4) is specially: the hydrogenated oil that step (3) obtains enters stabilizer tower through under meter governor valve control under High Pressure, at the bottom of stabilizer tower tower with thermal oil warm in 180 DEG C to stabilizer reboiler laser heating, column bottom temperature is made to remain on 145-150 DEG C, hydrogenated oil distills in tower, hydro carbons and the H be dissolved in hydrogenated oil of below C5
2the sour gas such as S are distilled out of is discharged by tower top; Overhead product is after below cold solidifying but to 40 of stabilizer tower condenser DEG C, enter stabilizer tower water-and-oil separator and carry out gas, water, oily three phase separation, gas phase is that non-condensable gases enters periodic off-gases pipeline through under meter governor valve control, oil phase leads back to stabilizer tower top and controls tower top temperature as backflow, tower top temperature is stabilized in about 90 DEG C, aqueous phase is discharged into sewage disposal, discharges BTX cut at the bottom of stabilizer tower tower;
BTX cut enters rectifying in the middle part of pre-distillation column, with 280 DEG C of high temperature heat conductive oils, reboiler is heated bottom pre-rectifying tower, column bottom temperature is made to remain on about 205 DEG C, tower bottom pressure remains on about 0.39 MPa, the hydro carbons such as hexanaphthene and Benzene and Toluene thing are discharged by tower top, go to enter water-and-oil separator to after the heating of purified petroleum benzin rectifying tower reboiler, oil phase part reflux pump after being separated is delivered to tower top and is returned stream and remain at the bottom of 137-139 DEG C of tower to control tower top temperature, tower top pressure is 0.3-0.4MPa, another part and BT component are delivered to tank field through under meter and are treated refining further under pressure itself, still liquid at the bottom of tower is delivered to tank field and is treated refining further.
8. a kind of technique producing benzene, toluene and dimethylbenzene from crude benzol according to claim 8, is characterized in that, step (5) is specially: the BT component from tank field enters in the middle part of extraction tower by pump through under meter; At the bottom of extraction tower tower with thermal oil warm in 180 DEG C to extraction tower reboiler laser heating, maintain about 144 DEG C at the bottom of tower, tower bottom pressure is 28-35 Kpa, N-formyl morpholine N-be extraction agent by the charging of tower top, extraction agent: charging BT component is by weight=1:5.5-6.
9. the stable hydrocarbon of carbon four, carbon five and carbon six carbon seven is discharged by tower top; Overhead product is delivered to tower top through condenser condenses to 25-30 DEG C of rear portion extraction tower reflux pump and is returned stream to control column bottom temperature 64-70 DEG C, and tower bottom pressure is-5K about Pa, and another part is that non-aromatics delivers to tank field storage;
Enter recycling design in the middle part of solvent regeneration tower from the rich solvent at the bottom of extraction tower tower, at the bottom of solvent regeneration tower tower with 260 DEG C of high temperature heat conductive oils to solvent tower reboiler laser heating, make to maintain about 170 DEG C at the bottom of tower, Benzene and Toluene is discharged by tower top; Overhead product is cooled to 15-35 DEG C of rear portion through condenser condenses and is used as trim the top of column, and control tower top temperature is 42-50 DEG C, and another part enters in the middle part of purified petroleum benzin rectifying tower; Solvent regeneration tower tower base solvent is squeezed into extraction tower reboiler by solvent pump and is reclaimed heat, then enters extraction tower feed heater and reclaim heat further; Solvent regeneration tower adopts negative-pressure operation, vacuumizes, make tower internal pressure remain on-0.072 MPa with vacuum pump set from tower top to solvent regeneration tower;
Benzene and Toluene tower from solvent regeneration tower enters in the middle part of purified petroleum benzin rectifying tower, with the benzene class steam heated reboiler laser heating that pre-rectifying tower tower top flows out at the bottom of tower, column bottom temperature is about 114 DEG C, tower bottom pressure 6-8 KPa, Benzene and Toluene is separated in tower, and purified petroleum benzin is discharged by tower top, and overhead product is cooled to 15-30 DEG C of rear portion through condenser condenses and returns stream through under meter to tower top, control column bottom temperature is 65-68 DEG C, and tower bottom pressure is-15 MPa; Another part purified petroleum benzin product delivers to tank field storage through under meter; After toluene product discharges cooling by tower reactor liquid phase, tank sending district stores;
Pre-rectifying tower still liquid XS component from tank field delivers to benzenol hydrorefining batch fractionating; In order at the bottom of the benzenol hydrorefining reboiler laser heating tower of warm heat-conducting oil heating in 160 DEG C at the bottom of benzenol hydrorefining tower, tower bottom pressure 15-30 KPa, XS component is distilled in tower, and the low-boiling point material such as dimethylbenzene, ethylbenzene is discharged by tower top; Overhead product is cooled to 15-30 DEG C of laggard top through condenser condenses and returns stream, controls column bottom temperature and is no more than 143 DEG C, and a part delivers to tank field storage through under meter as product; Benzenol hydrorefining tower bottoms tank sending district stores.
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| CN107200673A (en) * | 2017-07-07 | 2017-09-26 | 安徽卓泰化工科技有限公司 | A kind of xylene production device |
| CN109135800A (en) * | 2018-09-13 | 2019-01-04 | 大庆亿鑫化工股份有限公司 | A kind of light aromatic hydrocarbons add hydrogen reduced pressure distillation process |
| CN109181750A (en) * | 2018-09-13 | 2019-01-11 | 大庆亿鑫化工股份有限公司 | A kind of light aromatic hydrocarbons add hydrogen transformation device and its operating method |
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| CN109135800A (en) * | 2018-09-13 | 2019-01-04 | 大庆亿鑫化工股份有限公司 | A kind of light aromatic hydrocarbons add hydrogen reduced pressure distillation process |
| CN109181750A (en) * | 2018-09-13 | 2019-01-11 | 大庆亿鑫化工股份有限公司 | A kind of light aromatic hydrocarbons add hydrogen transformation device and its operating method |
| CN109181752A (en) * | 2018-09-13 | 2019-01-11 | 大庆亿鑫化工股份有限公司 | A kind of light aromatic hydrocarbons add the main hydrogenation technique of hydrogen |
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| CN109181766A (en) * | 2018-09-13 | 2019-01-11 | 大庆亿鑫化工股份有限公司 | A kind of modified light aromatic hydrocarbons hydrogenation plant and its operating method |
| CN109181751A (en) * | 2018-09-13 | 2019-01-11 | 大庆亿鑫化工股份有限公司 | A kind of light aromatic hydrocarbons add hydrogen transformation device and operating method |
| CN109181753A (en) * | 2018-09-13 | 2019-01-11 | 大庆亿鑫化工股份有限公司 | A kind of light aromatic hydrocarbons add the pre- hydrogenation technique of hydrogen |
| CN112279745A (en) * | 2019-07-25 | 2021-01-29 | 江苏合一金属新材料科技有限公司 | Crude benzene hydrofining process |
| CN111348981A (en) * | 2019-12-24 | 2020-06-30 | 国家能源集团煤焦化有限责任公司 | Crude benzene hydrofining method and device |
| CN115155460A (en) * | 2022-07-11 | 2022-10-11 | 福建永荣科技有限公司 | Benzene desulfurization adsorber for alkene method cyclohexanol process |
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