CN104004541B - A kind of preparation method of coal-based high arene underwater content stock oil - Google Patents
A kind of preparation method of coal-based high arene underwater content stock oil Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 7
- 239000003921 oil Substances 0.000 claims abstract description 157
- 238000000034 method Methods 0.000 claims abstract description 68
- 239000002994 raw material Substances 0.000 claims abstract description 49
- 239000011280 coal tar Substances 0.000 claims abstract description 35
- 238000001833 catalytic reforming Methods 0.000 claims abstract description 32
- 239000002283 diesel fuel Substances 0.000 claims abstract description 27
- 238000005194 fractionation Methods 0.000 claims abstract description 24
- 238000004821 distillation Methods 0.000 claims abstract description 23
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- 238000004517 catalytic hydrocracking Methods 0.000 claims description 26
- 238000006243 chemical reaction Methods 0.000 claims description 26
- 238000000926 separation method Methods 0.000 claims description 22
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- 239000003054 catalyst Substances 0.000 claims description 18
- 229910021536 Zeolite Inorganic materials 0.000 claims description 16
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- PWMGHDCLHPWGBX-UHFFFAOYSA-N [4-(carbamimidoylsulfanylmethyl)phenyl]methyl carbamimidothioate Chemical compound NC(=N)SCC1=CC=C(CSC(N)=N)C=C1 PWMGHDCLHPWGBX-UHFFFAOYSA-N 0.000 claims description 4
- 239000010953 base metal Substances 0.000 claims description 4
- 239000010941 cobalt Substances 0.000 claims description 4
- 229910017052 cobalt Inorganic materials 0.000 claims description 4
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- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 4
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- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims description 4
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- 239000010937 tungsten Substances 0.000 claims description 4
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- 238000009835 boiling Methods 0.000 claims description 2
- 229910052799 carbon Inorganic materials 0.000 claims description 2
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 2
- 239000000395 magnesium oxide Substances 0.000 claims description 2
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims description 2
- 229910044991 metal oxide Inorganic materials 0.000 claims description 2
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- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 2
- 239000001257 hydrogen Substances 0.000 description 32
- 229910052739 hydrogen Inorganic materials 0.000 description 32
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- Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
Abstract
The invention discloses a kind of preparation method of coal-based high arene underwater content stock oil, said method comprising the steps of: 1) raw materials pretreatment; 2) fractionation by distillation: DCL/Direct coal liquefaction generates oil, kerosene refines generation oil altogether or pretreated coal tar is divided into carbolic oil or naphtha fraction, diesel oil distillate and heavy oil fraction through air distillation or underpressure distillation, wherein, the cutting temperature of diesel oil distillate and heavy oil fraction is between 280 ~ 450 DEG C; Carbolic oil or naphtha fraction carry out phenol removal and obtain crude phenols and dephenolize oil, and obtain light ends oil after dephenolize oil and diesel oil distillate mixing, light ends oil carries out hydrofining; 3) hydrofining: light ends oil obtains hydrofining by hydrofining and generates oil; 4) product fractionation obtains the coal-based high arene underwater content stock oil producing aromatic hydrocarbons for catalytic reforming.The present invention can coal tar be not only raw material, can also DCL/Direct coal liquefaction generate oil or kerosene refine altogether generate oil as raw material, applicable raw materials scope is wide.
Description
Technical field
The invention belongs to coal chemical technology, particularly, the present invention relates to a kind of coal-derived oils deep processing method.
Background technology
Coal tar is the organic mixture based on aromatic hydrocarbon, it is an important byproduct in pyrolysis of coal/distillation process process, according to the difference of pyrolysis of coal pyrolysis temperature and process approach, coal tar can be divided into coalite tar (pyrolysis temperature 500 ~ 650 DEG C), coal-tar middle oil pyrolysis temperature (700 ~ 800 DEG C) and coal-tar heavy oil (pyrolysis temperature 950 ~ 1050 DEG C), and its composition difference is larger.
Coal-tar heavy oil derives from coke-oven plant, and annual production is stabilized in about 1,200 ten thousand tons, and actual amount of finish is less than 5,000,000 tons/year, serious waste of resources.Mainly contain following three kinds of modes: one is serve as low heat value industrial fuel oil to come into the market.Can only as low value-added primary products.Two is the raw materials as coal tar deep processing, can only therefrom extract the materials such as benzene, phenol, naphthalene, pitch.Be left to carry out burn processing as oil fuel, economic benefit is low.Three is take coal-tar heavy oil as raw material, adopts hydrofining or hydrocracking process technology, produces oil fuel.
In, coalite tar be mainly derived from middle low temperature pyrogenation produce the production such as blue charcoal, coal preparing natural gas.The annual blue charcoal in the whole nation is produced coalite tar in by-product and is reached 6,500,000 tons, is mainly distributed in Shan, Shanxi, border land of Meng San province.In addition, extensive coal preparing natural gas project will be built up successively, and expect coalite tar in coal preparing natural gas in 2015 and reach 6,000,000 tons, the year two thousand twenty reaches 2,000 ten thousand tons, is mainly distributed in the resourceful areas such as the brown coal such as Xinjiang, Inner Mongol, long-flame coal.In industrialized at present, the processing mode of coalite tar uses for reference existing refining of petroleum processing mode to produce oil fuel.
Compared with oil, coal tar has aromatic hydrocarbons and the high feature of naphthene content, for different coal tar, the content of aromatic hydrocarbons and naphthenic hydrocarbon is also different, greatly about the scope of 64%-90%, far away higher than the aromatic hydrocarbons in petroleum fractions and naphthene content, be applicable to the catalytic reforming raw material for the preparation of producing aromatic hydrocarbons.
And aromatic hydrocarbons chemical domestic needs vigorous (as BTX etc.), be mainly derived from the aromatics production process that oil is " catalytic reforming " technology of raw material at present, take oil as the restriction of Aromatics Production Technology by Domestic Resources and regional distribution of raw material, be difficult to the development of support downstream PTA and PET industry.Be that raw material prepares the petroleum naphtha of coal-based high arene underwater content as the raw material of catalytic reforming production aromatic hydrocarbons with coal tar, not only can solve domestic a large amount of aroamtic hydrocarbon raw material gap problem, the economic benefit of coal tar processing process can also be increased.
Chinese patent 201110006659.4 discloses a kind of method of widening catalytic reforming feedstock, this patent mixes as raw material using FCC stable gasoline and virgin naphtha by 50: 50 ~ 70: 30, through the removal of impurity of raw material metre filter, then remove the water carried in mixing petroleum naphtha through coalescer; Mixing petroleum naphtha and hydrogen mix to be heated to through process furnace and enter hydrogenator after temperature of reaction and contact with hydrogenation catalyst, carry out olefin saturated, desulfurization and denitrification reaction; Hydrogenation reaction effluent is separated and obtains hydrogen-rich gas and hydrogenated gasoline after condensing cooling, and hydrogen-rich gas recycles, and hydrogenated gasoline enters evaporator tower and carries out the refining petroleum naphtha that stripping fractionation is met catalytic reforming feedstock requirement; Mixing proportion can be carried out hydrotreatment more than the mixing petroleum naphtha of 50%FCC stable gasoline by present method, obtains the refining petroleum naphtha that foreign matter content all meets catalytic reforming feedstock requirement, solves the not enough problem of reformer feed, has widened the source of reformer feed.
Chinese patent 200510089847.2 discloses a kind of method of hydrotreating producing catalytic reforming raw material, and secondary processing of gasoline raw material is cut into light benzine cut, middle matter gasoline fraction and heavy gasoline fractions by this patent; Middle matter gasoline fraction enters the first reaction zone together with hydrogen, react under Hydrobon catalyst effect, reaction effluent enters second reaction zone after directly mixing with virgin naphtha without separation, react under the effect of Hydrobon catalyst, the reaction effluent generated carries out cooling, being separated, isolated hydrogen-rich gas recycles, and isolated liquid enters distillation dehydration tower, after imurity-removal, obtain petroleum naphtha.The method can process the secondary processing of gasoline that high sulfur-bearing is nitrogenous and olefin(e) centent is high under lower pressure, for catalytic reforming provides sulphur, nitrogen content to be all less than the acceptable material of 0.5 Μ G/G.
Chinese patent 200510089848.7 discloses a kind of method of producing catalytic reforming raw material, and secondary processing of gasoline raw material is cut into light benzine cut, middle matter gasoline fraction and heavy gasoline fractions by this patent; Middle matter gasoline fraction, optional virgin naphtha contact with the first Hydrobon catalyst together with hydrogen, carry out olefin saturation, reaction effluent directly contacts with the second Hydrobon catalyst without separation, carry out hydrogenating desulfurization and hydrodenitrification reaction, the reaction effluent generated carries out cooling, being separated, isolated hydrogen-rich gas recycles, and isolated liquid enters distillation dehydration tower, after imurity-removal, obtain petroleum naphtha.The method can process the secondary processing of gasoline that high sulfur-bearing is nitrogenous and olefin(e) centent is high under lower pressure, for catalytic reforming provides sulphur, nitrogen content to be all less than the acceptable material of 0.5 Μ G/G.
Chinese patent application 200910243462.5 discloses a kind of catalystic reforming method improving aromatics yield, and its step is as follows: feed naphtha, after heating unit, enters reaction unit; Products therefrom through overcooling laggard enter high-pressure separator; After described high-pressure separator, gained reformate enters stabilizer tower and processes; Overhead extraction dry gas, liquefied gas and a small amount of water; At the bottom of tower, the reformed oil of gained enters extraction system; Bottom described extraction system, extraction aromatic hydrocarbons enters diced system respectively with raffinating oil; Bottom diced system, extraction is heavily raffinated oil after heating unit, enters another reaction unit, and bottom is heavily raffinated oil as diesel oil kerosene or kerosene blend component by pipeline extraction simultaneously; Gained reaction product through overcooling laggard enter high-pressure separator.The advantage of raising aromatics yield catalystic reforming method of the present invention is: processing power, liquid yield, aromatics yield, hydrogen output improve greatly.
Above patent is all be that raw material is to prepare the method for catalytic reforming raw material with petroleum based oils.
Chinese patent application 201010218009.1 discloses a kind of production method and application of the coal-based naphtha with high potential aromatic content for catalytic reforming, the method comprises: a) hydrogenation step: mixed with hydrogen by the full cut liquefaction oil that DCL/Direct coal liquefaction is produced, expanded bed hydrotreating reactor is entered after mixing, contact that with hydrotreating catalyst hydrogenation reaction occurs, by flowing out the logistics of expanded bed hydrotreating reactor outlet after separation, fractionation, obtain light ends oil, middle matter cut and heavy distillate; And b) deep hydrofinishing step: after the light ends oil that step a) is obtained, the mixing of middle matter distillate, mix with hydrogen, enter fixed bed deep hydrofinishing reactor together, contact that with Hydrobon catalyst chemical reaction occurs, to the logistics of fixed bed deep hydrofinishing reactor outlet be flowed out after separation, fractionation, obtain the naphtha fraction of the high aromatic hydrocarbon potential content meeting catalytic reforming feed stock requirement, and extending catalyst work-ing life.This patent is that raw material adopts ebullated bed for the preparation of the method for the high aromatic hydrocarbons petroleum naphtha of catalytic reforming with liquefied coal coil.
Summary of the invention
The object of the invention is to, there is provided a kind of coal-derived oils deep processing method, the method can coal tar be not only raw material, can also DCL/Direct coal liquefaction generate oil or kerosene refine altogether generate oil as raw material, applicable raw materials scope is wide, can be used for the catalytic reforming raw material producing coal-based high aromatic hydrocarbon potential content.
For achieving the above object, present invention employs following technical scheme:
A preparation method for coal-based high arene underwater content stock oil, said method comprising the steps of:
1) raw materials pretreatment: when coal-derived oils raw material is DCL/Direct coal liquefaction generation oil or kerosene refines generation oil altogether, this step is omitted, and directly enters fractionation by distillation step;
When coal-derived oils raw material is coal tar, removes moisture wherein, solid impurity obtains pretreated coal tar;
2) fractionation by distillation: DCL/Direct coal liquefaction generates oil, kerosene refines generation oil altogether or pretreated coal tar is divided into carbolic oil or naphtha fraction, diesel oil distillate and heavy oil fraction through air distillation or underpressure distillation, wherein, the cutting temperature of diesel oil distillate and heavy oil fraction is between 280 ~ 450 DEG C;
Carbolic oil or naphtha fraction carry out phenol removal and obtain crude phenols and dephenolize oil, and obtain light ends oil after dephenolize oil and diesel oil distillate mixing, light ends oil carries out hydrofining;
3) hydrofining: light ends oil obtains hydrofining by hydrofining and generates oil;
4) product fractionation: when the cutting temperature of diesel oil distillate and heavy oil fraction is between 280 ~ 380 DEG C, hydrofining generates oil and enter separation column after cooling, gas-liquid separation, require to fractionate out the naphtha fraction being less than 145 DEG C, the cut being less than the naphtha fraction of 150 DEG C, the cut of 65 ~ 145 DEG C or 65 ~ 150 DEG C according to catalytic reforming raw material boiling range, above-mentioned fractionation cut is out the coal-based high arene underwater content stock oil producing aromatic hydrocarbons for catalytic reforming;
When the cutting temperature of diesel oil distillate and heavy oil fraction is between 380 ~ 450 DEG C, hydrofining generates oil and enter separation column after cooling, gas-liquid separation, be be less than the naphtha fraction of 145 DEG C or be less than the cut of the naphtha fraction of 150 DEG C or the cut of 65 ~ 145 DEG C or 65 ~ 150 DEG C according to the fractionation of variant production object, and tail oil, wherein, the naphtha fraction being less than 145 DEG C or the naphtha fraction being less than 150 DEG C or the cut of 65 ~ 145 DEG C or the cut of 65 ~ 150 DEG C are the coal-based high arene underwater content stock oil producing aromatic hydrocarbons for catalytic reforming.
Further, described tail oil adopts hydrocracking process to process, and gained hydrocracking generates oil and enter step 3 after cooling, gas-liquid separation) hydrofining.
Preferably, described step 2) in, employing alkali liquid washing method or solvent extration extract the phenolic compound in carbolic oil cut or naphtha fraction, obtain crude phenols and dephenolize oil.
Preferably, described step 3) in, hydrofining reactor is fixed-bed reactor, adopts single hop hydrogenation or multi-stek hydrogenation technique.
Preferably, described step 3) in, hydrogenation catalyst with one or more in unformed aluminum oxide, silicon oxide, titanium oxide, magnesium oxide, ZSM zeolite, zeolite L, y-type zeolite and Beta zeolite for carrier, active metal component comprises base metal component and noble metal components, wherein base metal component comprises one or more in nickel, cobalt, molybdenum and tungsten, and content in the catalyst counts 20wt% ~ 80wt% with non-noble metal oxide; Noble metal components comprises platinum and/or palladium, and content in the catalyst counts 0.1wt% ~ 20wt% with metal oxide containing precious metals.
Preferably, described step 3) in, Hydrobon catalyst pore volume>=0.4ml/g, specific surface area>=120m
2/ g, bulk density is 0.4 ~ 1.9Kg/m
3.
Preferably, described step 3) in, hydrofining reaction condition is: temperature of reaction is 200 ~ 440 DEG C, and reaction pressure is 6 ~ 17MPa, and volume space velocity is 0.5 ~ 4.0h
-1, hydrogen-oil ratio is 300 ~ 2000.
Preferably, in described hydrocracking process, hydrocracking reactor is fixed-bed reactor, adopts single hop hydrogenation or multi-stek hydrogenation technique.
Preferably, in described hydrocracking process, hydrogenation catalyst is with one or more in unformed aluminum oxide, silicon oxide, ZSM zeolite, zeolite L, y-type zeolite and Beta zeolite for carrier, and active metal component is one or more in group vib and group VIII metal element
Wherein, group vib metallic element is molybdenum and tungsten;
Group VIII metal element is cobalt and nickel.
Preferably, in described hydrocracking process, hydrocracking reaction condition is: temperature of reaction is 200 ~ 440 DEG C, and reaction pressure is 6 ~ 17MPa, and volume space velocity is 0.5 ~ 4.0h
-1, hydrogen-oil ratio is 300 ~ 2000.
In the present invention, for the coal tar that phenol content is higher, in carbolic oil or naphtha fraction oil, containing a considerable number of phenolic compound, if not dephenolize direct hydrogenation, the phenolic compound of high added value can be made to be converted into aromatic hydrocarbons to be entered in the finished product, both reduces product price, turn increases process hydrogen consumption.
For the coal tar that phenol content is lower, do not consider to propose phenol operation.
In the present invention, light ends oil, by hydrofining, removes detrimental impurity, saturation of olefins and the aromatic hydrocarbons such as the sulphur in stock oil, nitrogen, oxygen and metal.
Coal tar of the present invention be in coalite tar, middle coalite tar, coal-tar middle oil, coal-tar heavy oil any one or two or more coal tar with the mixing oil of arbitrary proportion.
In the present invention, when using alkali liquid washing method to carry phenol, alkali cleaning temperature is 30 ~ 60 DEG C, and the alkali cleaning time is 0.2 ~ 1.5min, and concentration of lye is 7% ~ 13%, and water/oil quality ratio is 0.6 ~ 1.2, adopts CO
2acidifying sodium phenolate; When using Recovery by Solvent Extraction Methold phenol, extraction agent is ethylene glycol or glycerol, and extraction temperature is normal temperature, and churning time is 10 ~ 40min, and dephenolize rate reaches as high as 96%.
Advantage of the present invention be mainly reflected in following some:
1. the present invention had both been applicable to coalite tar, middle coalite tar, coal-tar heavy oil, was also applicable to the mixing oil of any two above coal tar, and be also applicable to DCL/Direct coal liquefaction and generate oil and kerosene and refine altogether and generate oily, raw material is applied widely.
2. in method provided by the present invention, adopt rational processing process and suitable working depth, by the optimization of processing parameter, the light ends of different material oil can be made to produce the catalytic reforming raw material of high arene underwater content.
3. the present invention is that the high value added utilization of coal-derived oils provides novel method, has widened the source of the catalytic reforming raw material of high arene underwater content.
Accompanying drawing explanation
Below in conjunction with accompanying drawing, method provided by the present invention is further described,
Fig. 1 is that the present invention is not containing process flow sheet during tail oil hydrocracking;
Fig. 2 is the process flow sheet of the present invention when containing tail oil hydrocracking;
Eliminate the equipment of much necessity in figure, as pump, tank, process furnace, interchanger, valve etc., the shape and size of equipment and pipeline not by the restriction of accompanying drawing, but are determined as the case may be.
Reference numeral:
Digitized representation material in Fig. 1 and Fig. 2: 1, fresh hydrogen; 2, coal-derived oils raw material; 3, pretreated coal tar or DCL/Direct coal liquefaction generate oil or kerosene and refine altogether and generate oil; 4, carbolic oil or naphtha fraction; 5, diesel oil distillate; 6, heavy ends; 7, crude phenols; 8, dephenolize oil; 9, light ends oil; 10, hydrogen is mixed; 11, circulating hydrogen; 12, hydrofining generates oil; 13, gas-liquid separation liquid phase; 14, cut one; 15, cut two; 16, cut three; 17, cut four; 18, tail oil; 19, hydrogen is mixed; 20, circulating hydrogen; 21, tail oil hydrocracking generates oil; 22, gas-liquid separation liquid phase;
Letter and number combination in Fig. 1 and Fig. 2 represents unit, device or equipment: V1, pretreatment unit; T1, fractionation by distillation unit; C1, fresh hydrogen compressor; D1, dephenolize unit; R1, hydrofining unit; C2, circulating hydrogen compressor; V2, hydrofining generate oil-gas-liquid separating unit; T2, product fractionation unit; R2, Hydrocracking unit; C3, circulating hydrogen compressor; V3, hydrocracking generate oil-gas-liquid separating unit.
Embodiment
With the drawings and specific embodiments, the present invention is further detailed explanation below.
As shown in Figure 1, first coal-derived oils stock oil 2 carry out de-slag (solid impurity) process of dewatering in pretreatment unit V1, pretreated raw material 3 (pretreated coal tar, or, not pretreated DCL/Direct coal liquefaction generates oil or kerosene refines generation oil altogether) enter fractionation by distillation unit T1, carry out fractionation by distillation, be divided into carbolic oil or naphtha fraction 4, diesel oil distillate 5, heavy ends 6.Carbolic oil or naphtha fraction 4 extract after crude phenols 7 through alkali liquid washing method or solvent extration in dephenolize cells D 1, remaining dephenolize oil 8 and diesel oil distillate 5 mixed light ends oil 9 and the hydrogen 1 compressed through hydrogen gas compressor C1 or the circulating hydrogen 11 compressed through circulating hydrogen compressor C2 or hydrogen 1 and the mixed mixing hydrogen 10 of circulating hydrogen 11 enter hydrofining unit R 1 simultaneously and carry out hydrofining, generate oil 12 from R1 hydrofining out to generate through hydrofining and after oil-gas-liquid separating unit V2, to obtain gas-liquid separation mutually 13, gas-liquid separation 13 enters product fractionation unit T2 mutually, in T2, material is separated cut 1 or cut 2 15 or cut 3 16 or cut 4 17, above-mentioned cut one can for the cut being less than 65 DEG C, cut two can be the cut of 65 ~ 145 DEG C or the cut of 65 ~ 150 DEG C, cut three can be kerosene(oil)fraction, cut four can be diesel oil distillate, those skilled in the art can be according to actual needs, select different cut points, such as above-mentioned cut one and cut two are merged, obtain being less than the naphtha fraction of 145 DEG C or being less than the naphtha fraction of 150 DEG C, the naphtha fraction being wherein less than 145 DEG C or the naphtha fraction being less than 150 DEG C or the cut of 65 ~ 145 DEG C or the cut of 65 ~ 150 DEG C are the coal-based high arene underwater content stock oil producing aromatic hydrocarbons for catalytic reforming.
As shown in Figure 2, first coal-derived oils stock oil 2 carry out de-slag (solid impurity) process of dewatering in pretreatment unit V1, pretreated raw material 3 (pretreated coal tar, or, not pretreated DCL/Direct coal liquefaction generates oil or kerosene refines generation oil altogether) enter fractionation by distillation unit T1, carry out fractionation by distillation, be divided into carbolic oil or naphtha fraction 4, diesel oil distillate 5, heavy ends 6.Carbolic oil or naphtha fraction 4 extract after crude phenols 7 through alkali liquid washing method or solvent extration in dephenolize cells D 1, remaining dephenolize oil 8 and diesel oil distillate 5 mixed light ends oil 9 and the hydrogen 1 compressed through hydrogen gas compressor C1 or the circulating hydrogen 11 compressed through circulating hydrogen compressor C2 or hydrogen 1 and the mixed mixing hydrogen 10 of circulating hydrogen 11 enter hydrofining unit R 1 simultaneously and carry out hydrofining, generate oil 12 from R1 hydrofining out to generate through hydrofining and after oil-gas-liquid separating unit V2, to obtain gas-liquid separation mutually 13, gas-liquid separation 13 enters product fractionation unit T2 mutually, in T2, material is separated cut 1 or cut 2 15 or cut 3 16 or cut 4 17 or tail oil 18, above-mentioned cut one can for the cut being less than 65 DEG C, cut two can be the cut of 65 ~ 145 DEG C or the cut of 65 ~ 150 DEG C, cut three can be kerosene(oil)fraction, cut four can be diesel oil distillate, those skilled in the art can be according to actual needs, select different cut points, such as above-mentioned cut one and cut two are merged, obtain being less than the naphtha fraction of 145 DEG C or being less than the naphtha fraction of 150 DEG C, the naphtha fraction being wherein less than 145 DEG C or the naphtha fraction being less than 150 DEG C or the cut of 65 ~ 145 DEG C or the cut of 65 ~ 150 DEG C are the coal-based high arene underwater content stock oil producing aromatic hydrocarbons for catalytic reforming.Tail oil 18 and through hydrogen gas compressor C1 compress hydrogen 1 or through circulating hydrogen compressor C2 compress circulating hydrogen 11 through circulating hydrogen compressor C3 compress circulating hydrogen 20 or mixing hydrogen 10,19 go Hydrocracking unit R2 to carry out hydrocracking lighting reaction, obtain tail oil hydrocracking and generate oil 21, this oil generates oil-gas-liquid separating unit V3 through hydrocracking and is separated and obtains gas-liquid separation mutually 22, and gas-liquid separation 22 can generate oil with R1 hydrofining out and together enters product fractionation unit T2 and carry out fractionation by distillation mutually.
The beneficial effect of illustrating object of the present invention further below in conjunction with specific embodiment and having, but protection scope of the present invention is not limited to the following example.
Embodiment 1
Adopt the technical process of Fig. 1, generate oil for raw material with gelatin liquefaction, through distillation unit, be cut into the heavy distillate of < 230 DEG C of carbolic oil or naphtha fraction, 230 DEG C ~ 350 DEG C diesel oil distillates and > 350 DEG C.< 230 DEG C of carbolic oil or naphtha fraction mix with 230 DEG C ~ 350 DEG C diesel oil distillates after dephenolize unit adopts alkali liquid washing method to extract crude phenols product, and mixed light ends oil nature is in table 1.Light ends oil is through obtained 65 ~ 145 DEG C of cuts of deep hydrofinishing, i.e. the catalytic reforming raw material oil of high arene underwater content, main character is in table 3.Above-mentioned each technique unit technological condition is in table 2.Deep hydrofinishing employing inlet amount is the fixed bed hydrogenation testing apparatus of 100ml/h, adopts two reactors in series patterns.
Embodiment 2
Adopt the technical process of Fig. 2, with middle coalite tar for raw material, enter distillation unit through the de-pretreated purification coal tar of slag (solid impurity) of dehydration, be cut into the heavy distillate of < 230 DEG C of carbolic oil or naphtha fraction, 230 DEG C ~ 450 DEG C diesel oil distillates and > 450 DEG C.< 230 DEG C of carbolic oil or naphtha fraction mix with 230 DEG C ~ 450 DEG C diesel oil distillates after dephenolize unit adopts solvent extration to extract crude phenols product, mixed light ends oil nature is in table 1, light ends oil is refining obtained 65 ~ 150 DEG C of cuts after deep hydrofinishing, tail oil hydrocracking, the i.e. catalytic reforming raw material oil of high arene underwater content, main character is in table 3.Above-mentioned each technique unit technological condition is in table 2.
The present embodiment completes on the fixed bed hydrogenation testing apparatus being 100ml/h, and deep hydrofinishing adopts two reactors in series patterns; Tail oil hydrocracking is refining reaction device after the fixed bed of 100ml/h by the fixed bed hydrogenation cracking case of a 100ml/h and an inlet amount, adopts two reactors in series patterns.
Embodiment 3
Adopt the technical process of Fig. 1, take coal-tar heavy oil as raw material, enter distillation unit through the de-pretreated purification coal tar of slag (solid impurity) of dehydration, be cut into the heavy distillate of < 230 DEG C of carbolic oil or naphtha fraction, 230 DEG C ~ 350 DEG C diesel oil distillates and > 350 DEG C.< 230 DEG C of carbolic oil or naphtha fraction mix with 230 DEG C ~ 350 DEG C diesel oil distillates after dephenolize unit adopts solvent extration to extract crude phenols product, and mixed light ends oil nature is in table 1.Mixing light distillate can produce the naphtha fraction being less than 150 DEG C through deep hydrofinishing, i.e. the catalytic reforming raw material oil of high arene underwater content, and main character is in table 3.Above-mentioned each technique unit technological condition is in table 2.
Deep hydrofinishing adopts inlet amount to be the fixed-bed reactor of 100ml/h, adopts two reactors in series patterns.
The light ends oil nature of table 1 embodiment 1-3 different material
The each unit technological condition of table 2 embodiment 1-3
The main character of table 3 embodiment 1-3 height arene underwater content catalytic reforming raw material
As can be seen from the data of table 3, the high arene underwater content catalytic reforming raw material that the present invention obtains, arene underwater content is high, the stock oil producing triphen (benzene,toluene,xylene) preferably for catalytic reforming-Aromatics Extractive Project, its arene underwater content is higher than petroleum reforming raw oil, especially embodiment 3, when taking coal-tar heavy oil as raw material of the present invention, the high arene underwater content catalytic reforming raw material that the present invention obtains, arene underwater content is up to 85.8%, and this is that petroleum reformer feed institute is inaccessiable.
Claims (10)
1. a preparation method for coal-based high arene underwater content stock oil, said method comprising the steps of:
1) raw materials pretreatment: when coal-derived oils raw material is DCL/Direct coal liquefaction generation oil or kerosene refines generation oil altogether, this step is omitted, and directly enters fractionation by distillation step;
When coal-derived oils raw material is coal tar, removes moisture wherein, solid impurity obtains pretreated coal tar;
2) fractionation by distillation: DCL/Direct coal liquefaction generates oil, kerosene refines generation oil altogether or pretreated coal tar is divided into carbolic oil or naphtha fraction, diesel oil distillate and heavy oil fraction through air distillation or underpressure distillation, wherein, the cutting temperature of diesel oil distillate and heavy oil fraction is between 280 ~ 450 DEG C;
Carbolic oil or naphtha fraction carry out phenol removal and obtain crude phenols and dephenolize oil, and obtain light ends oil after dephenolize oil and diesel oil distillate mixing, light ends oil carries out hydrofining;
3) hydrofining: light ends oil obtains hydrofining by hydrofining and generates oil;
4) product fractionation: when the cutting temperature of diesel oil distillate and heavy oil fraction is between 280 ~ 380 DEG C, hydrofining generates oil and enter separation column after cooling, gas-liquid separation, require to fractionate out the naphtha fraction being less than 145 DEG C, the cut being less than the naphtha fraction of 150 DEG C, the cut of 65 ~ 145 DEG C or 65 ~ 150 DEG C according to catalytic reforming raw material boiling range, be the coal-based high arene underwater content stock oil producing aromatic hydrocarbons for catalytic reforming;
When the cutting temperature of diesel oil distillate and heavy oil fraction is between 380 ~ 450 DEG C, hydrofining generates oil and enter separation column after cooling, gas-liquid separation, be be less than the naphtha fraction of 145 DEG C or be less than the cut of the naphtha fraction of 150 DEG C or the cut of 65 ~ 145 DEG C or 65 ~ 150 DEG C according to the fractionation of variant production object, and tail oil, wherein, the naphtha fraction being less than 145 DEG C or the naphtha fraction being less than 150 DEG C or the cut of 65 ~ 145 DEG C or the cut of 65 ~ 150 DEG C are the coal-based high arene underwater content stock oil producing aromatic hydrocarbons for catalytic reforming.
2. method according to claim 1, is characterized in that, described step 4) in tail oil adopt hydrocracking process to process, gained hydrocracking generates oil through cooling, enters step 3 after gas-liquid separation) hydrofining.
3. method according to claim 1 and 2, is characterized in that, described step 2) in, employing alkali liquid washing method or solvent extration extract the phenolic compound in carbolic oil cut or naphtha fraction, obtain crude phenols and dephenolize oil.
4. method according to claim 1 and 2, is characterized in that, described step 3) in, hydrofining reactor is fixed-bed reactor, adopts single hop hydrogenation or multi-stek hydrogenation technique.
5. method according to claim 1 and 2, it is characterized in that, described step 3) in, hydrogenation catalyst with one or more in unformed aluminum oxide, silicon oxide, titanium oxide, magnesium oxide, ZSM zeolite, zeolite L, y-type zeolite and Beta zeolite for carrier, active metal component comprises base metal component and noble metal components, wherein base metal component comprises one or more in nickel, cobalt, molybdenum and tungsten, and content in the catalyst counts 20wt% ~ 80wt% with non-noble metal oxide; Noble metal components comprises platinum and/or palladium, and content in the catalyst counts 0.1wt% ~ 20wt% with metal oxide containing precious metals.
6. method according to claim 1 and 2, is characterized in that, described step 3) in, Hydrobon catalyst pore volume>=0.4ml/g, specific surface area>=120m
2/ g, bulk density is 0.4 ~ 1.9Kg/m
3.
7. method according to claim 1 and 2, is characterized in that, described step 3) in, hydrofining reaction condition is: temperature of reaction is 200 ~ 440 DEG C, and reaction pressure is 6 ~ 17MPa, and volume space velocity is 0.5 ~ 4.0h
-1, hydrogen-oil ratio is 300 ~ 2000.
8. method according to claim 2, is characterized in that, in described hydrocracking process, hydrocracking reactor is fixed-bed reactor, adopts single hop hydrogenation or multi-stek hydrogenation technique.
9. method according to claim 2, it is characterized in that, in described hydrocracking process, hydrogenation catalyst with one or more in unformed aluminum oxide, silicon oxide, ZSM zeolite, zeolite L, y-type zeolite and Beta zeolite for carrier, active metal component is one or more in group vib and group VIII metal element
Wherein, group vib metallic element is molybdenum and tungsten;
Group VIII metal element is cobalt and nickel.
10. method according to claim 2, is characterized in that, in described hydrocracking process, hydrocracking reaction condition is: temperature of reaction is 200 ~ 440 DEG C, and reaction pressure is 6 ~ 17MPa, and volume space velocity is 0.5 ~ 4.0h
-1, hydrogen-oil ratio is 300 ~ 2000.
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| CN105062558B (en) * | 2015-07-31 | 2017-01-11 | 神华集团有限责任公司 | gasoline and preparation method thereof |
| CN107365600B (en) * | 2016-05-13 | 2020-04-21 | 神华集团有限责任公司 | A method for producing catalytic reforming raw materials by hydrorefining of non-petrochemical naphtha and its reaction device |
| CN108865253B (en) * | 2018-06-12 | 2020-12-18 | 煤炭科学技术研究院有限公司 | Method for producing aromatic hydrocarbon rich by direct coal hydrogenation liquefaction |
| CN112708485B (en) * | 2020-12-27 | 2023-04-11 | 陕西延长石油（集团）有限责任公司 | Method for preparing high-calorific-value high-density jet fuel from kerosene mixed raw material |
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| CN101885982A (en) * | 2010-06-23 | 2010-11-17 | 煤炭科学研究总院 | Hydrogenation method for coal tar suspension bed of heterogeneous catalyst |
| CN102465033A (en) * | 2010-11-04 | 2012-05-23 | 中国石油化工股份有限公司 | Processing method of medium-low temperature coal tar |
| CN102899087A (en) * | 2012-09-19 | 2013-01-30 | 王小英 | Deep processing method for medium and low temperature coal tar |
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Effective date of registration: 20160329 Address after: 100013 Beijing, Hepingli Youth ditch East Road, No. 5, No. Patentee after: Co., Ltd of coal science and technology academy Address before: 100013 Beijing, Hepingli Youth ditch East Road, No. 5, No. Patentee before: General Research Institute of Coal Science |