CN104419461A - Coal tar slurry bed and fixed bed series connection hydrogenation process - Google Patents
Coal tar slurry bed and fixed bed series connection hydrogenation process Download PDFInfo
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- CN104419461A CN104419461A CN201310360713.4A CN201310360713A CN104419461A CN 104419461 A CN104419461 A CN 104419461A CN 201310360713 A CN201310360713 A CN 201310360713A CN 104419461 A CN104419461 A CN 104419461A
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G67/00—Treatment of hydrocarbon oils by at least one hydrotreatment process and at least one process for refining in the absence of hydrogen only
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G2300/00—Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
- C10G2300/20—Characteristics of the feedstock or the products
- C10G2300/201—Impurities
- C10G2300/202—Heteroatoms content, i.e. S, N, O, P
Abstract
The present invention provides a coal tar slurry bed and fixed bed series connection hydrogenation process, which comprises: (1) carrying out a purification treatment; (2) carrying out pressure reducing or normal pressure distillation on the purified coal tar, and cutting into the light oil distillate and the heavy oil distillate, wherein the cutting point of the light-heavy oil distillate is 220-370 DEG C; (3) mixing the light oil distillate and H2, uniformly mixing, conveying the obtained material into a fixed bed, and carrying out hydrorefining under the hydrorefining catalyst effect to prepare a hydrorefining product; and (4) mixing the heavy oil distillate, a hydrocracking catalyst and H2, uniformly mixing, sequentially conveying the obtained material into a first-stage slurry bed and a second-stage slurry bed to carry out a double-stage hydrocracking reaction, and carrying out a fractionation treatment on the prepared hydrocracking product, wherein the distillate with the boiling point of more than 540 DEG C is externally discharged, the distillate with the boiling point of less than 350 DEG C is recycled as part of the fed material of the fixed bed, and the remaining components return to the first-stage slurry bed inlet. With the method of the present invention, the sulfur content and the nitrogen content in naphtha and diesel fuel are reduced, and the cetane number in the diesel fuel is substantially improved.
Description
Technical field
The present invention relates to a kind of slurry bed system and fixed bed Unionfining technique of coal tar, belong to technical field of coal chemical industry.
Background technology
Liquid fuel occupies very consequence in the various energy.The transportation means such as various automobile, boats and ships, aircraft, engineering machinery use liquid fuel all in a large number.Liquid fuel is mainly derived from from underground mining oil out.And in recent years, along with the continuous intensification of exhaustion and China's energy dilemma day by day of world petroleum resource, find reasonable, economic substitute energy, change energy consumption structure, become the task of top priority that China faces.
In prior art, along with the fast development of China's iron and steel and coal chemical industry, the output of coal tar is increasing, and effective utilization of coal tar also becomes more and more important.And be raw material with coal tar, under the effect of catalyzer, carry out technology that hydrofining or hydrocracking prepare liquid fuel also just to receive much concern as the substitute products of petrochemical complex, it can not only supplement the deficiency of domestic petroleum resource by petroleum replacing chemical industry, and for guarantee energy strategy safety, there is reality and long-range strategic importance.
At present, coal tar hydrogenating technology can roughly be summarized as according to its technical characterstic: coal tar hydrorefining technology, delayed coking-hydrocracking process integration technology, the fixed bed hydrogenation cracking technology of coal tar and the slurry bed system hydrocracking technology of coal tar.Such as Chinese patent literature CN103059973A discloses a kind of slurry bed system and fixed bed coupling process of full fraction of coal tar hydrogenation, full fraction of coal tar that the method mainly comprises the steps: (1) oil is after the pre-treatment of dehydration, udst separation, mix with hydrocracking catalyst, enter slurry bed system Hydrocracking unit through preheating; (2) at slurry bed system Hydrocracking unit, described full fraction of coal tar oil carries out hydrocracking under hydrocracking catalyst effect, and this process is continuously feeding, and first hydrogenated products enter fractionation unit; (3) at fractionation unit, described just hydrogenated products through fractionation operation wherein light component enter fixed bed hydrogenation refined unit, middle runnings loops back paste state bed reactor together with catalyzer, still loops back step (1) after the heavy component coke that remove portion catalyzer and cracking process produce after filtration; (4) at fixed bed hydrogenation refined unit, the light component of described just hydrogenated products carries out hydrotreated lube base oil, desulfurization, holder folk prescription speech under Hydrobon catalyst effect, obtains hydrogenated products; (5) at product rectification cell, hydrogenated products enter rectifying tower, carry out cut cutting and obtain the finished product vapour, diesel oil.
First above-mentioned technology carries out hydrocracking to full fraction of coal tar after pretreatment at slurry bed system Hydrocracking unit, the first hydrogenated products obtained are again through fractionation, light component enters fixed bed hydrogenation refined unit and carries out hydrofining, middle runnings is circulated to paste state bed reactor and carries out hydrocracking, and heavy component processes Posterior circle after filtration and carries out pre-treatment to pretreatment unit.The petrol and diesel oil target product prepared through above-mentioned technology is the petrol and diesel oil meeting Standard.But because above-mentioned technology directly carries out slurry bed system hydrocracking to full fraction of coal tar, and not only containing heavy ends in full fraction of coal tar, also containing middle runnings and light ends, and light ends is when carrying out slurry bed system hydrocracking, light ends forms diluting effect to heavy ends, reduces reactant concn, and hydrogen consumption in slurry bed system hydrocracking process can be caused like this to increase, cause the wasting of resources, also can affect the yield that coal tar hydrogenating prepares liquid fuel simultaneously.
In prior art, also have and first full fraction of coal tar is carried out reducing pressure or after air distillation, cutting into light oil distillate and heavy oil fraction, then the report that shortening prepares liquid fuel is carried out respectively to light oil distillate and heavy oil fraction.Such as Chinese patent literature CN101864327A discloses a kind of coal tar hydrogenation modification method, and the method mainly comprises the steps: that first coal tar is cut into the light oil distillate of <205 DEG C and the heavy oil fraction of >205 DEG C through air distillation or underpressure distillation; Carry out one section of fixed bed hydrogenation to the light oil distillate of <205 DEG C again to refine, alkylated reaction is carried out to this hydrotreated product, obtains gasoline products; The heavy oil fraction of >205 DEG C to be mixed afterwards and hydrogen is mixed into two ends fixed bed hydrogenation reactor and carries out deep hydrofinishing by weight adding thinning oil for 1:1, after fractionation process, obtains diesel oil distillate.Although above-mentioned technology has first carried out decompression or air distillation to full fraction of coal tar, again respectively hydrofining is carried out to the light ends obtained and heavy ends, but in above-mentioned technology, when shortening is carried out to heavy distillate, thinning oil is adopted again first to dilute heavy distillate, again to the hydrofining that the heavy distillate after dilution adopts fixed bed to carry out, and the existence of thinning oil can cause hydrogen consumption in unifining process to increase equally, cause the wasting of resources, also can affect the quality that coal tar hydrogenating prepares liquid fuel simultaneously.
That is, in prior art when carrying out slurry bed system or fixed bed hydrogenation reaction to the heavy distillate in coal tar, all carry out hydrogenation reaction again after adopting light ends or thinning oil to dilute heavy ends, light ends is present in heavy ends, when jointly carrying out hydrogenation reaction with heavy ends, there is hydrogen consumption high, also cause coal tar hydrogenating to prepare the problems such as the yield of liquid fuel is low, the S of liquid fuel, N content are high, the cetane value content of diesel product is low simultaneously.But the present inventor but finds that the existence of light ends is also not definitely harmful, especially for the coal tar of complicated component, select the light ends of sufficient quantity and mixing of heavy ends, while not affecting hydrogen consumption, the total conversion rate improving coal tar can not only be played, more can improve the quality of hydrofining product in coal tar hydrogenation process process, and this point is prior art those skilled in the art does not recognize.
As everyone knows, in hydrogenation technique, hydrogen dividing potential drop is more high is more conducive to hydrofining, particularly to the sulphur being difficult to remove and nitrogen, if expect the product that N, S content is low, hydrogen dividing potential drop needed for its unifining process can be higher, further increase the hydrogen consumption of whole technique, and slurry bed system equipment of the prior art and fixed bed unit independently carry out hydrogenation process, and a large amount of hydrogen contained in the gas of each equipment exhausting are not reasonably utilized.
Summary of the invention
Technical problem to be solved by this invention is when carrying out shortening to coal tar in prior art, hydrogenation is carried out again after needing first to adopt light ends or thinner to dilute heavy ends, reactant concn can be reduced like this, hydrogen consumption in catalytic hydrogenation is caused to increase, and the yield of liquid fuel is low, the problem that product quality is low, and then by rational parameter adjustment, creatively select the cut point that light and heavy fractions is the suitableeest, thus provide a kind of slurry bed system and fixed bed serial hydrogenation technique of coal tar; Further, the problem high for present coal tar hydrogenation process hydrogen consumption, hydrogen from each equipment in isolated gas does not have Appropriate application, and then slurry bed system and the fixed bed serial hydrogenation technique of another coal tar are provided.
The technical scheme that the present invention takes for this reason is:
The slurry bed system of coal tar and a fixed bed serial hydrogenation technique, comprise the steps:
(1) carry out dewatering, the purifying treatment of de-mechanical impurity;
(2) coal tar after purifying treatment in described step (1) is carried out reducing pressure or air distillation, cut into light oil distillate and heavy oil fraction, the cut point of light and heavy fractions 220 ~ 370 DEG C;
(3) by the light oil distillate in described step (2) and H
2mixing, enters fixed bed after mixing, under the effect of Hydrobon catalyst, carries out hydrofining, prepare hydrofining product;
(4) by described step (2) heavy oil fraction and hydrocracking catalyst, H
2mixing, enters one-level slurry bed system successively after mixing, secondary slurry bed system carries out two-stage hydrocracking reaction, controls transformation efficiency between 35 ~ 85%, carries out fractionation process to the hydrocracked product prepared,
Separation is obtained >540 DEG C of cut to arrange outward, be separated and obtain entering fixed bed after <350 DEG C of cut mixes with the light oil distillate of described step (2) as a part of charging of fixed bed, all the other components return one-level slurry bed system entrance as a part of feed cycle of one-level slurry bed system.
In the slurry bed system of above-mentioned coal tar and fixed bed serial hydrogenation technique, in the slurry bed system and fixed bed serial hydrogenation technique of the described coal tar of steady running, the hydrogen entering described fixed bed comprise by the external world replenish fixed bed hydrogen make-up and from the isolated gas of two-stage slurry bed system; And the isolated gas of described fixed bed is back to described one-level slurry bed system and described secondary slurry bed system respectively as the feed gas of two-stage slurry bed system.
In the slurry bed system of above-mentioned coal tar and fixed bed serial hydrogenation technique, the isolated gas of two-stage slurry bed system mixes with described hydrogen make-up after recycle compressor supercharging.
In the slurry bed system of above-mentioned coal tar and fixed bed serial hydrogenation technique, the heavy oil fraction in described step (4) first after thermal pretreatment, then with hydrocracking catalyst, H
2mixing.
In the slurry bed system of above-mentioned coal tar and fixed bed serial hydrogenation technique, the temperature of described thermal pretreatment is 80 ~ 280 DEG C.
In the slurry bed system of above-mentioned coal tar and fixed bed serial hydrogenation technique, described hydrocracking catalyst is the nanometer materials containing one or more in hydrogenation active component Fe, Co, Ni, Mo, W.
In the slurry bed system of above-mentioned coal tar and fixed bed serial hydrogenation technique, described one-level slurry reactor temperature 350 ~ 550 DEG C, secondary slurry reactor temperature is 350 ~ 550 DEG C, and other reaction conditionss of two-stage paste state bed reactor are: pressure is 10.0 ~ 18.0MPa, volume space velocity is 0.5 ~ 2.0h
-1, hydrogen to oil volume ratio is 1200 ~ 5000.
In the slurry bed system of above-mentioned coal tar and fixed bed serial hydrogenation technique, described Hydrobon catalyst is any one or a few in Co-Mo system, Ni-Mo system, Co-W system, Ni-W system.
In the slurry bed system of above-mentioned middle coalite tar and fixed bed Unionfining technique, the condition of described fixed bed hydrogenation reaction is: temperature is 220 ~ 450 DEG C, pressure is 12.0 ~ 18.0MPa, volume space velocity is 0.5 ~ 2.0h
-1, hydrogen to oil volume ratio is 500 ~ 3000.
In the slurry bed system of above-mentioned coal tar and fixed bed serial hydrogenation technique, described coal tar is one or both in middle coalite tar or coal-tar heavy oil.
In the slurry bed system of above-mentioned coal tar and fixed bed serial hydrogenation technique, add in residual oil, heavy oil, high-sulfur oils, high asphalt content oil, high heavy metal content oil in the coal tar in described step (1) any one or a few.
The present invention compared with prior art tool has the following advantages:
(1), in the slurry bed system of coal tar of the present invention and fixed bed serial hydrogenation technique, first carry out purifying treatment to coal tar, the object of purifying treatment is the solid impurity, water etc. that contain in removing coal tar, and then the coal tar after purifying treatment is reduced pressure or air distillation, cut into light oil distillate and heavy oil fraction, the temperature range being cut point with 220-370 DEG C, because the light oil distillate of sufficient quantity can be contained in the heavy oil fraction on this cut point, and the existence of this part light oil distillate has collaborative promoter action to heavy oil fraction in follow-up two-stage slurry bed system hydrocracking, it can improve the quality of the hydrogenated products of this part heavy oil fraction greatly, after tested, the method of the invention reduces the sulphur content in petroleum naphtha and diesel oil, nitrogen content, and the cetane value substantially increased in diesel oil.
(2) in the slurry bed system of coal tar of the present invention and fixed bed serial hydrogenation technique, further light oil distillate and the cut of <350 DEG C that obtains after the hydrocracking of two-stage slurry bed system are mixed into fixed bed and carry out hydrofining, the transformation efficiency of coal-tar heavy oil of the present invention can be improved further.The liquid fuel adopting the two-stage slurry bed system hydrogenation technique of coal-tar heavy oil of the present invention to prepare has low, the product quality of hydrogen consumption and can be further enhanced.
(3) in the slurry bed system of coal tar of the present invention and fixed bed serial hydrogenation technique, the hydrogen entering described fixed bed comprise by the external world replenish fixed bed hydrogen make-up and from the isolated gas of two-stage slurry bed system; And the isolated gas of described fixed bed is back to described one-level slurry bed system and described secondary slurry bed system respectively as the feed gas of two-stage slurry bed system.Its reason is mainly owing to containing a large amount of hydrogen from paste state bed reactor with from fixed-bed reactor in isolated gas, and it can reuse through adaptive adjustment.
The gas that fixed bed enters slurry bed system mainly relies on the pressure reduction between stream oriented device automatically to carry out, and through practical proof, in the light and heavy fractions cut coverage of the application, when heavy oil fraction carries out hydrocracked, treated in two-stage paste state bed reactor, it directly meets hydrocracking process necessary requirement by the isolated gas of fixed bed as the feed gas of two-stage slurry bed system.
Enter the gas of fixed bed by two-stage slurry bed system and extraneous hydrogen make-up forms the feed gas of high pressure gas as fixed bed under the supercharging of a compressor, meet the demand of fixed bed hydrogenation process for refining to hydrogen partial pressure by the adjustment of extraneous hydrogen.
Whole technological process only needs use compressor, the hydrogenation process of all devices can be realized, take full advantage of the pressure reduction between fixed bed and slurry bed system device, reasonably make use of each device in the gas and prior art that each device separates goes out and configure separately the technique that compressor carries out hydrotreatment, not only reduce the quantity of compressor, reduce equipment cost, and reasonably make use of hydrogen, further mitigate the hydrogen consumption of whole technique accordingly.
(4) in the slurry bed system of coal tar of the present invention and fixed bed serial hydrogenation technique, to be entered in the gas of paste state bed reactor except a large amount of hydrogen by fixed-bed reactor, also containing partial impurities, in this gas, C1 ~ C4 content is high, cause the molecular-weight average of whole air inlet high, be conducive to slurry bed system and operate in turbulent area, slagging prevention precursor deposition in the reactor.
(5) in the slurry bed system of coal tar of the present invention and fixed bed serial hydrogenation technique, further, residual oil can also be added in coal tar, high-sulfur oils, high pitch prill is containing gauging, high heavy metal content oil, one or more in heavy oil form mixture, above-mentioned steps is adopted to carry out shortening to this mixture again, owing to arranging suitable cut point to this mixture, and can light oil distillate containing sufficient quantity in heavy oil fraction in mixture on this cut point, and the existence of this part light oil distillate has collaborative promoter action to the heavy oil fraction in mixture in follow-up secondary slurry bed system hydrocracking, it can improve the hydrogenation conversion of the heavy oil fraction in this part mixes greatly.Therefore, adopt the two-stage slurry bed system hydrogenation technique of coal tar of the present invention, not only can carry out shortening to coal tar, can also carry out shortening to the mixing oil that residual oil, high-sulfur oils, high pitch prill are formed containing gauging, high heavy metal content oil, heavy oil and coal tar, and the liquid fuel prepared has equally, and hydrogen consumption is low, the advantage of excellent product performance.
(6), in the slurry bed system of coal tar of the present invention and fixed bed serial hydrogenation technique, further, can also select to carry out thermal pretreatment to heavy oil fraction, then with hydrocracking catalyst, H
2mixing, can make heavy oil fraction and catalyzer, H like this
2what mix is more even, so that improve its hydrogenation catalyst efficiency further.
Accompanying drawing explanation
Fig. 1 is the slurry bed system of coal tar of the present invention and the schema of fixed bed serial hydrogenation technique.
Embodiment
Below in conjunction with embodiment, the present invention is further described in detail, but is not limited to this.
Embodiment 1
(1) in treating plant, coal tar is dewatered, the purifying treatment of de-mechanical impurity, the coal tar water content after dehydration is less than 0.5wt%;
(2) coal tar after purifying treatment in described step (1) is carried out underpressure distillation, cut into the light oil distillate being less than 230 DEG C and the heavy oil fraction being greater than 230 DEG C;
(3) by the light oil distillate in described step (2) and H
2mixing, enters fixed bed after mixing, under the effect of Hydrobon catalyst, carries out hydrofining, and carries out fractionation to hydrofining product and obtain petroleum naphtha and diesel oil.In this step, the condition of described fixed bed hydrogenation reaction is: temperature is 220 DEG C, pressure is 12.0MPa, volume space velocity is 0.5h
-1, hydrogen to oil volume ratio is 500; Hydrobon catalyst composed as follows: 8wt%NiO, 20wt%MoO
3, surplus is ZSM-5 molecular sieve.
(4) by described step (2) heavy oil fraction and hydrocracking catalyst, H
2mixing, enter one-level slurry bed system successively after mixing, secondary slurry bed system carries out two-stage hydrocracking reaction, control transformation efficiency 35%, fractionation process is carried out to the hydrocracked product prepared, separation is obtained >540 DEG C of cut to arrange outward, separation obtains <350 DEG C of cut, enter fixed bed after mixing with the light oil distillate of described step (2) as a part of charging of fixed bed, all the other components return one-level slurry bed system as a part of feed cycle of one-level slurry bed system; In this step, the reaction conditions of two-stage slurry bed system is: temperature of reaction 350 DEG C, and pressure is 10.0MPa, volume space velocity is 0.5h
-1, hydrogen to oil volume ratio is 1200, hydrocracking catalyst is oil solubility nanometer level material, and it consists of 20wt%MoO3,5wt%NiO, surplus is oil soluble γ-A1
2o
3carrier.
In the present embodiment, the total conversion rate of coal tar is 96.0%, diesel oil total recovery 76%.
Embodiment 2
(1) in treating plant, the mixture of coal tar and residual oil is dewatered, the purifying treatment of de-mechanical impurity, the coal tar water content after dehydration is less than 0.5wt%;
(2) coal tar after purifying treatment in described step (1) is carried out underpressure distillation, cut into the light oil distillate being less than 370 DEG C and the heavy oil fraction being greater than 370 DEG C;
(3) by the light oil distillate in described step (2) and H
2mixing, enters fixed bed after mixing, under the effect of Hydrobon catalyst, carries out hydrofining, and carries out fractionation to hydrofining product and obtain petroleum naphtha and diesel oil.In this step, the condition of described fixed bed hydrogenation reaction is: temperature is 260 DEG C, pressure is 18.0MPa, volume space velocity is 0.6h
-1, hydrogen to oil volume ratio is 1000; Hydrobon catalyst composed as follows: 9wt%CoO, 20wt%MoO
3, surplus is ZSM-5 molecular sieve.
(4) by described step (2) heavy oil fraction and hydrocracking catalyst, H
2mixing, enter one-level slurry bed system successively after mixing, secondary slurry bed system carries out two-stage hydrocracking reaction, control transformation efficiency 40%, fractionation process is carried out to the hydrocracked product prepared, separation is obtained >540 DEG C of cut to arrange outward, separation obtains <350 DEG C of cut, enter fixed bed after mixing with the light oil distillate of described step (2) as a part of charging of fixed bed, all the other components return one-level slurry bed system as a part of feed cycle of one-level slurry bed system; In this step, the reaction conditions of two-stage slurry bed system is: one-level slurry bed system pressure 12MPa, secondary slurry bed system pressure 11MPa, and other condition is: temperature of reaction 4000 DEG C, and volume space velocity is 1h
-1, hydrogen to oil volume ratio is 2000, hydrocracking catalyst is oil solubility nanometer level material, and it consists of 20wt%CoO, 8wt%WO3, surplus is oil soluble γ-Al
2o
3carrier.
In the present embodiment in whole hydrogenation technique, as shown in Figure 1, the hydrogen entering described fixed bed comprise by the external world replenish fixed bed hydrogen make-up and from the isolated gas of two-stage slurry bed system; And the isolated gas of described fixed bed is back to described one-level slurry bed system and described secondary slurry bed system respectively as the feed gas of two-stage slurry bed system.The gas that fixed bed enters slurry bed system mainly relies on the pressure reduction between stream oriented device automatically to carry out, and directly meets hydrocracking process necessary requirement by the isolated gas of fixed bed as the feed gas of two-stage slurry bed system.Enter the gas of fixed bed by two-stage slurry bed system and extraneous hydrogen make-up forms the feed gas of high pressure gas as fixed bed under the supercharging of a compressor, meet the demand of fixed bed hydrogenation process for refining to hydrogen partial pressure by the adjustment of extraneous hydrogen.
In the present embodiment, the total conversion rate of coal tar is 96.0%, diesel oil total recovery 78%, hydrogen consumption 5.7%.
Embodiment 3
(1) in treating plant, the mixture of coal tar, high-sulfur oils and high asphalt content oil is dewatered, the purifying treatment of de-mechanical impurity, the coal tar water content after dehydration is less than 0.5wt%;
(2) coal tar after purifying treatment in described step (1) is carried out underpressure distillation, cut into the light oil distillate being less than 240 DEG C and the heavy oil fraction being greater than 240 DEG C;
(3) by the light oil distillate in described step (2) and H
2mixing, enters fixed bed after mixing, under the effect of Hydrobon catalyst, carries out hydrofining, and carries out fractionation to hydrofining product and obtain petroleum naphtha and diesel oil.In this step, the condition of described fixed bed hydrogenation reaction is: temperature is 300 DEG C, pressure is 14.0MPa, volume space velocity is 0.8h
-1, hydrogen to oil volume ratio is 1500; Hydrobon catalyst composed as follows: 8wt%CoO, 25wt%WO
3, surplus is ZSM-5 molecular sieve.
(4) by described step (2) heavy oil fraction carry out at 80 DEG C after thermal pretreatment with hydrocracking catalyst, H
2mixing, enter one-level slurry bed system successively after mixing, secondary slurry bed system carries out two-stage hydrocracking reaction, control transformation efficiency 65%, fractionation process is carried out to the hydrocracked product prepared, separation is obtained >540 DEG C of cut to arrange outward, separation obtains <350 DEG C of cut, enter fixed bed after mixing with the light oil distillate of described step (2) as a part of charging of fixed bed, all the other components return one-level slurry bed system as a part of feed cycle of one-level slurry bed system; In this step, the reaction conditions of two-stage slurry bed system is: temperature of reaction 550 DEG C, and pressure is 18.0MPa, volume space velocity is 1.5h
-1, hydrogen to oil volume ratio is 2500, hydrocracking catalyst is oil solubility nanometer level material, and it consists of 20wt%Fe2O3,5wt%NiO, surplus is oil soluble γ-Al
2o
3carrier.
In the present embodiment, the total conversion rate of coal tar is 96.2%, diesel oil total recovery 77.4%.
Embodiment 4
(1) in treating plant, the mixture of coal tar, heavy oil and high heavy metal oil is dewatered, the purifying treatment of de-mechanical impurity, the coal tar water content after dehydration is less than 0.5wt%;
(2) coal tar after purifying treatment in described step (1) is carried out underpressure distillation, cut into the light oil distillate being less than 320 DEG C and the heavy oil fraction being greater than 320 DEG C;
(3) by the light oil distillate in described step (2) and H
2mixing, enters fixed bed after mixing, under the effect of Hydrobon catalyst, carries out hydrofining, and carries out fractionation to hydrofining product and obtain petroleum naphtha and diesel oil.In this step, the condition of described fixed bed hydrogenation reaction is: temperature is 350 DEG C, pressure is 18.0MPa, volume space velocity is 1.0h
-1, hydrogen to oil volume ratio is 2000; Hydrobon catalyst composed as follows: 10wt%NiO, 20wt%WO
3, surplus is ZSM-5 molecular sieve.
(4) by described step (2) heavy oil fraction carry out at 100 DEG C after thermal pretreatment with hydrocracking catalyst, H
2mixing, enter one-level slurry bed system successively after mixing, secondary slurry bed system carries out two-stage hydrocracking reaction, control transformation efficiency 50%, fractionation process is carried out to the hydrocracked product prepared, separation is obtained >540 DEG C of cut to arrange outward, separation obtains <350 DEG C of cut, enter fixed bed after mixing with the light oil distillate of described step (2) as a part of charging of fixed bed, all the other components return one-level slurry bed system as a part of feed cycle of one-level slurry bed system; In this step, the reaction conditions of two-stage slurry bed system is: one-level slurry bed system pressure 16MPa, secondary slurry bed system pressure 15MPa, and other condition is: temperature of reaction 510 DEG C, and volume space velocity is 2h
-1, hydrogen to oil volume ratio is 3000, hydrocracking catalyst is oil solubility nanometer level material, and it consists of 10wt%Fe2O3,15wt%WO3, surplus is natural zeolite molecular sieve carrier.
In the present embodiment in whole hydrogenation technique, as shown in Figure 1, the hydrogen entering described fixed bed comprise by the external world replenish fixed bed hydrogen make-up and from the isolated gas of two-stage slurry bed system; And the isolated gas of described fixed bed is back to described one-level slurry bed system and described secondary slurry bed system respectively as the feed gas of two-stage slurry bed system.The gas that fixed bed enters slurry bed system mainly relies on the pressure reduction between stream oriented device automatically to carry out, and directly meets hydrocracking process necessary requirement by the isolated gas of fixed bed as the feed gas of two-stage slurry bed system.Enter the gas of fixed bed by two-stage slurry bed system and extraneous hydrogen make-up forms the feed gas of high pressure gas as fixed bed under the supercharging of a compressor, meet the demand of fixed bed hydrogenation process for refining to hydrogen partial pressure by the adjustment of extraneous hydrogen.
In the present embodiment, the total conversion rate of coal tar is 97.0%, diesel oil total recovery 75.3%, hydrogen consumption 5.8%.。
Embodiment 5
(1) in treating plant, coal tar is dewatered, the purifying treatment of de-mechanical impurity, the coal tar water content after dehydration is less than 0.5wt%;
(2) coal tar after purifying treatment in described step (1) is carried out underpressure distillation, cut into the light oil distillate being less than 300 DEG C and the heavy oil fraction being greater than 300 DEG C;
(3) by the light oil distillate in described step (2) and H
2mixing, enters fixed bed after mixing, under the effect of Hydrobon catalyst, carries out hydrofining, and carries out fractionation to hydrofining product and obtain petroleum naphtha and diesel oil.In this step, the condition of described fixed bed hydrogenation reaction is: temperature is 400 DEG C, pressure is 18.0MPa, volume space velocity is 1.5h
-1, hydrogen to oil volume ratio is 2500; Hydrobon catalyst composed as follows: 4wt%NiO, 10wt%MoO
3, 5wt%CoO, 10wt%WO
3, surplus is ZSM-5 molecular sieve.
(4) by described step (2) heavy oil fraction carry out at 150 DEG C after thermal pretreatment with hydrocracking catalyst, H
2mixing, enter one-level slurry bed system successively after mixing, secondary slurry bed system carries out two-stage hydrocracking reaction, control transformation efficiency 55%, fractionation process is carried out to the hydrocracked product prepared, separation is obtained >540 DEG C of cut to arrange outward, separation obtains <350 DEG C of cut, enter fixed bed after mixing with the light oil distillate of described step (2) as a part of charging of fixed bed, all the other components return one-level slurry bed system as a part of feed cycle of one-level slurry bed system; In this step, the reaction conditions of two-stage slurry bed system is: one-level slurry bed system pressure 18MPa, secondary slurry bed system pressure 17MPa, and other condition is: temperature of reaction 450 DEG C, and volume space velocity is 1.8h
-1, hydrogen to oil volume ratio is 3500, hydrocracking catalyst is oil solubility nanometer level material, and it consists of 18wt%MoO3,5wt%CoO surplus is natural zeolite molecular sieve carrier.
In the present embodiment in whole hydrogenation technique, as shown in Figure 1, the hydrogen entering described fixed bed comprise by the external world replenish fixed bed hydrogen make-up and from the isolated gas of two-stage slurry bed system; And the isolated gas of described fixed bed is back to described one-level slurry bed system and described secondary slurry bed system respectively as the feed gas of two-stage slurry bed system.The gas that fixed bed enters slurry bed system mainly relies on the pressure reduction between stream oriented device automatically to carry out, and directly meets hydrocracking process necessary requirement by the isolated gas of fixed bed as the feed gas of two-stage slurry bed system.Enter the gas of fixed bed by two-stage slurry bed system and extraneous hydrogen make-up forms the feed gas of high pressure gas as fixed bed under the supercharging of a compressor, meet the demand of fixed bed hydrogenation process for refining to hydrogen partial pressure by the adjustment of extraneous hydrogen.
In the present embodiment, the total conversion rate of coal tar is 97.2%, diesel oil total recovery 78.2%, hydrogen consumption 6%.
Embodiment 6
(1) in treating plant, coal tar is dewatered, the purifying treatment of de-mechanical impurity, the coal tar water content after dehydration is less than 0.5wt%;
(2) coal tar after purifying treatment in described step (1) is carried out air distillation, cut into the light oil distillate being less than 280 DEG C and the heavy oil fraction being greater than 280 DEG C;
(3) by the light oil distillate in described step (2) and H
2mixing, enters fixed bed after mixing, under the effect of Hydrobon catalyst, carries out hydrofining, and carries out fractionation to hydrofining product and obtain petroleum naphtha and diesel oil.In this step, the condition of described fixed bed hydrogenation reaction is: temperature is 450 DEG C, pressure is 16.0MPa, volume space velocity is 2.0h
-1, hydrogen to oil volume ratio is 3000; Hydrobon catalyst composed as follows: 8wt%NiO, 10wt%WO
3, 10wt%CoO surplus is ZSM-5 molecular sieve.
(4) by described step (2) heavy oil fraction carry out at 250 DEG C after thermal pretreatment with hydrocracking catalyst, H
2mixing, enter one-level slurry bed system successively after mixing, secondary slurry bed system carries out two-stage hydrocracking reaction, control transformation efficiency 70%, fractionation process is carried out to the hydrocracked product prepared, separation is obtained >540 DEG C of cut to arrange outward, separation obtains <350 DEG C of cut, enter fixed bed after mixing with the light oil distillate of described step (2) as a part of charging of fixed bed, all the other components return one-level slurry bed system as a part of feed cycle of one-level slurry bed system; In this step, the reaction conditions of two-stage slurry bed system is: one-level slurry bed system pressure 15MPa, secondary slurry bed system pressure 14MPa, and other condition is: temperature of reaction 380 DEG C, and volume space velocity is 1.3h
-1, hydrogen to oil volume ratio is 4000, hydrocracking catalyst is oil solubility nanometer level material, and it consists of 30wt%FeS surplus is natural zeolite molecular sieve carrier.
In the present embodiment in whole hydrogenation technique, as shown in Figure 1, the hydrogen entering described fixed bed comprise by the external world replenish fixed bed hydrogen make-up and from the isolated gas of two-stage slurry bed system; And the isolated gas of described fixed bed is back to described one-level slurry bed system and described secondary slurry bed system respectively as the feed gas of two-stage slurry bed system.The gas that fixed bed enters slurry bed system mainly relies on the pressure reduction between stream oriented device automatically to carry out, and directly meets hydrocracking process necessary requirement by the isolated gas of fixed bed as the feed gas of two-stage slurry bed system.Enter the gas of fixed bed by two-stage slurry bed system and extraneous hydrogen make-up forms the feed gas of high pressure gas as fixed bed under the supercharging of a compressor, meet the demand of fixed bed hydrogenation process for refining to hydrogen partial pressure by the adjustment of extraneous hydrogen.
In the present embodiment, the total conversion rate of coal tar is 94.0%, diesel oil total recovery 78.4%, hydrogen consumption 5.9%.
Embodiment 7
(1) in treating plant, coal tar is dewatered, the purifying treatment of de-mechanical impurity, the coal tar water content after dehydration is less than 0.5wt%;
(2) coal tar after purifying treatment in described step (1) is carried out underpressure distillation, cut into the light oil distillate being less than 260 DEG C and the heavy oil fraction being greater than 260 DEG C;
(3) by the light oil distillate in described step (2) and H
2mixing, enters fixed bed after mixing, under the effect of Hydrobon catalyst, carries out hydrofining, and carries out fractionation to hydrofining product and obtain petroleum naphtha and diesel oil.In this step, the condition of described fixed bed hydrogenation reaction is: temperature is 400 DEG C, pressure is 18.0MPa, volume space velocity is 2h
-1, hydrogen to oil volume ratio is 2500; Hydrobon catalyst composed as follows: 8wt%NiO, 20wt%MoO
3, surplus is ZSM-5 molecular sieve.
(4) by described step (2) heavy oil fraction carry out at 280 DEG C after thermal pretreatment with hydrocracking catalyst, H
2mixing, enter one-level slurry bed system successively after mixing, secondary slurry bed system carries out two-stage hydrocracking reaction, control transformation efficiency 85%, fractionation process is carried out to the hydrocracked product prepared, separation is obtained >540 DEG C of cut to arrange outward, separation obtains <350 DEG C of cut, enter fixed bed after mixing with the light oil distillate of described step (2) as a part of charging of fixed bed, all the other components return one-level slurry bed system as a part of feed cycle of one-level slurry bed system; In this step, the reaction conditions of two-stage slurry bed system is: one-level slurry bed system pressure 15MPa, secondary slurry bed system pressure 14MPa, and other condition is: temperature of reaction 530 DEG C, and volume space velocity is 0.8h
-1, hydrogen to oil volume ratio is 5000, hydrocracking catalyst is oil solubility nanometer level material, and it consists of 20wt%MoO3,5wt%NiO, surplus is oil soluble γ-A1
2o
3carrier.
In the present embodiment in whole hydrogenation technique, as shown in Figure 1, the hydrogen entering described fixed bed comprise by the external world replenish fixed bed hydrogen make-up and from the isolated gas of two-stage slurry bed system; And the isolated gas of described fixed bed is back to described one-level slurry bed system and described secondary slurry bed system respectively as the feed gas of two-stage slurry bed system.The gas that fixed bed enters slurry bed system mainly relies on the pressure reduction between stream oriented device automatically to carry out, and directly meets hydrocracking process necessary requirement by the isolated gas of fixed bed as the feed gas of two-stage slurry bed system.Enter the gas of fixed bed by two-stage slurry bed system and extraneous hydrogen make-up forms the feed gas of high pressure gas as fixed bed under the supercharging of a compressor, meet the demand of fixed bed hydrogenation process for refining to hydrogen partial pressure by the adjustment of extraneous hydrogen.
In the present embodiment, the total conversion rate of coal tar is 95.0%, diesel oil total recovery 77.6%, hydrogen consumption 5.7%.
Embodiment 8
(1) in treating plant, coal tar is dewatered, the purifying treatment of de-mechanical impurity, the coal tar water content after dehydration is less than 0.5wt%;
(2) coal tar after purifying treatment in described step (1) is carried out underpressure distillation, cut into the light oil distillate being less than 350 DEG C and the heavy oil fraction being greater than 350 DEG C;
(3) by the light oil distillate in described step (2) and H
2mixing, enters fixed bed after mixing, under the effect of Hydrobon catalyst, carries out hydrofining, and carries out fractionation to hydrofining product and obtain petroleum naphtha and diesel oil.In this step, the condition of described fixed bed hydrogenation reaction is: temperature is 360 DEG C, pressure is 14.0MPa, volume space velocity is 1.0h
-1, hydrogen to oil volume ratio is 1200; Hydrobon catalyst composed as follows: 8wt%NiO, 20wt%MoO
3, surplus is ZSM-5 molecular sieve.
(4) by described step (2) heavy oil fraction and hydrocracking catalyst, H
2mixing, enter one-level slurry bed system successively after mixing, secondary slurry bed system carries out two-stage hydrocracking reaction, control transformation efficiency 35%, fractionation process is carried out to the hydrocracked product prepared, separation is obtained >540 DEG C of cut to arrange outward, separation obtains <350 DEG C of cut, enter fixed bed after mixing with the light oil distillate of described step (2) as a part of charging of fixed bed, all the other components return one-level slurry bed system as a part of feed cycle of one-level slurry bed system; In this step, the reaction conditions of two-stage slurry bed system is: temperature of reaction 455 DEG C, and pressure is 13.2MPa, volume space velocity is 0.6h
-1, hydrogen to oil volume ratio is 2500, hydrocracking catalyst is oil solubility nanometer level material, and it consists of 20wt%MoO3,5wt%NiO, surplus is oil soluble γ-Al
2o
3carrier.
In the present embodiment in whole hydrogenation technique, as shown in Figure 1, the hydrogen entering described fixed bed comprise by the external world replenish fixed bed hydrogen make-up and from the isolated gas of two-stage slurry bed system; And the isolated gas of described fixed bed is back to described one-level slurry bed system and described secondary slurry bed system respectively as the feed gas of two-stage slurry bed system.The pressure reduction that the gas that fixed bed enters slurry bed system mainly relies on stream oriented device to ask carries out automatically, directly meets hydrocracking process necessary requirement by the isolated gas of fixed bed as the feed gas of two-stage slurry bed system.Enter the gas of fixed bed by two-stage slurry bed system and extraneous hydrogen make-up forms the feed gas of high pressure gas as fixed bed under the supercharging of a compressor, meet the demand of fixed bed hydrogenation process for refining to hydrogen partial pressure by the adjustment of extraneous hydrogen.
In the present embodiment, the total conversion rate of coal tar is 96.2%, diesel oil total recovery 78%, total hydrogen consumption 5.7%.
In addition, present invention also offers coal tar used in above-mentioned all embodiments, residual oil, heavy oil, high-sulfur oils, high asphalt content oil and high heavy metal content oil properties, as shown in table 1, and further provide the petroleum naphtha and bavin oil properties that prepare, as shown in table 2.
Table 1 raw material oil properties
The petroleum naphtha that table 2 prepares and bavin oil properties
Comparative example 1
The present invention adopts the operational path provided in documents CN103059973A as comparative example of the present invention, and it for raw material, adopts following technique to prepare liquid fuel with the coal tar used in above-described embodiment:
Water in pre-treatment removing raw material and mechanical impurity, mix with hydrocracking catalyst and enter paste state bed reactor, hydrocracking catalyst is oil solubility nanometer level material, and it consists of 20wt%MoO3,5wt%NiO, surplus is oil soluble γ-Al
2o
3carrier, hydrocracking condition is as follows: preheating temperature 150 DEG C, temperature of reaction 455 DEG C, pressure is 13.2MPa, volume space velocity is 0.6h
-1, hydrogen to oil volume ratio is 2500, head product after hydrocracking enters separation column, lighting end enters back segment fixed-bed reactor and carries out hydrofining, this part cut accounts for 15wt%, middle runnings is about 65wt% and loops back paste state bed reactor continuation hydrocracking, raw material storage tank is entered after the coke that the heavy ends of about 20wt% produces in remove portion catalyzer and reaction process after filtration, the cyclic utilization rate of catalyzer is about 80%, and wherein light ends fixed bed hydrogenation refining reaction condition is as follows: temperature is 360 DEG C, pressure is 14.0MPa, volume space velocity is 1.0h
-1, hydrogen to oil volume ratio is 1200, Hydrobon catalyst consist of 8wt%NiO, 20wt%MoO
3, surplus is ZSM-5 molecular sieve.
The performance of the gasoline adopting above-mentioned technology to prepare is as follows: density 0.82g/cm
-3, sulphur content <50ppm, nitrogen content <50ppm, octane value 94, the performance of the diesel oil distillate prepared is as follows: density 0.81g/cm
-3, sulphur content <50ppm, nitrogen content <50ppm, cetane value 34.
Comparative example 2
The present invention adopts the operational path provided in documents CN103059973A as comparative example of the present invention, its with the full cut of tar for raw material adopts following technique prepare liquid fuel:
Water in pre-treatment removing raw material and mechanical impurity, mix with hydrocracking catalyst and enter paste state bed reactor, hydrocracking catalyst is 35%WO
3, 10%NiO, 3%P
2o
5, surplus is USY molecular sieve, hydrocracking condition is as follows: preheating temperature 150 DEG C, reaction pressure break 12MPa, temperature of reaction are 390 DEG C, volume space velocity 0.5h
-1, hydrogen to oil volume ratio is 1600, head product after hydrocracking enters separation column, lighting end enters back segment fixed-bed reactor and carries out hydrofining, this part cut accounts for 15wt%, middle runnings is about 65wt% and loops back paste state bed reactor continuation hydrocracking, raw material storage tank is entered after the coke that the heavy ends of about 20wt% produces in remove portion catalyzer and reaction process after filtration, the cyclic utilization rate of catalyzer is about 80%, wherein light ends fixed bed hydrogenation refining reaction condition is as follows: reaction pressure 8MPa, temperature of reaction 375 DEG C, volume space velocity 0.5h
-1, hydrogen to oil volume ratio 1600; Fixed bed refine after product obtain gasoline and diesel oil through fractionation;
The performance of the gasoline adopting above-mentioned technology to prepare is as follows: density 0.80g/cm
-3, sulphur content <55ppm, nitrogen content <55ppm, octane value 90, the performance of the diesel oil distillate prepared is as follows: density 0.70g/cm
-3, sulphur content <55ppm, nitrogen content <55ppm, cetane value 35.
From above-mentioned two comparative examples, the petroleum naphtha adopting the method for the invention to prepare, the sulphur content of diesel oil, nitrogen content reduce greatly, and diesel-fuel cetane number also improves greatly.
Obviously, above-described embodiment is only for clearly example being described, and the restriction not to embodiment.For those of ordinary skill in the field, can also make other changes in different forms on the basis of the above description.Here exhaustive without the need to also giving all embodiments, and thus the apparent change of extending out or variation be still among the protection domain of the invention claim.
Claims (11)
1. the slurry bed system of coal tar and a fixed bed serial hydrogenation technique, comprise the steps:
(1) carry out dewatering, the purifying treatment of de-mechanical impurity;
(2) coal tar after purifying treatment in described step (1) is carried out reducing pressure or air distillation, cut into light oil distillate and heavy oil fraction, the cut point of light and heavy fractions 220 ~ 370 DEG C;
(3) by the light oil distillate in described step (2) and H
2mixing, enters fixed bed after mixing, under the effect of Hydrobon catalyst, carries out hydrofining, prepare hydrofining product;
(4) by described step (2) heavy oil fraction and hydrocracking catalyst, H
2mixing, enters one-level slurry bed system successively after mixing, secondary slurry bed system carries out two-stage hydrocracking reaction, controls transformation efficiency between 35 ~ 85%, carries out fractionation process to the hydrocracked product prepared,
Separation is obtained > 540 DEG C of cuts to arrange outward, be separated and obtain entering fixed bed after < 350 DEG C of cuts mix with the light oil distillate of described step (2) as a part of charging of fixed bed, all the other components return one-level slurry bed system entrance as a part of feed cycle of one-level slurry bed system.
2. the slurry bed system of coal tar according to claim 1 and fixed bed serial hydrogenation technique, is characterized in that,
In the slurry bed system and fixed bed serial hydrogenation technique of the described coal tar of steady running, the hydrogen entering described fixed bed comprise by the external world replenish fixed bed hydrogen make-up and from the isolated gas of two-stage slurry bed system;
And the isolated gas of described fixed bed is back to described one-level slurry bed system and described secondary slurry bed system respectively as the feed gas of two-stage slurry bed system.
3. the slurry bed system of coal tar according to claim 2 and fixed bed serial hydrogenation technique, is characterized in that,
The isolated gas of two-stage slurry bed system mixes with described hydrogen make-up after recycle compressor supercharging.
4., according to slurry bed system and the fixed bed serial hydrogenation technique of the arbitrary described coal tar of claim 1 ~ 3, it is characterized in that,
Heavy oil fraction in described step (4) first after thermal pretreatment, then with hydrocracking catalyst, H
2mixing.
5. the slurry bed system of coal tar and fixed bed serial hydrogenation technique according to claim 4, it is characterized in that, the temperature of described thermal pretreatment is 80 ~ 280 DEG C.
6., according to slurry bed system and the fixed bed serial hydrogenation technique of the arbitrary described coal tar of claim 1 ~ 5, it is characterized in that,
Described hydrocracking catalyst is the nanometer materials containing one or more in hydrogenation active component Fe, Co, Ni, Mo, W.
7. the slurry bed system of coal tar and fixed bed serial hydrogenation technique according to claim 6, is characterized in that,
Described one-level slurry reactor temperature 350 ~ 550 DEG C, secondary slurry reactor temperature is 350 ~ 550 DEG C, and other reaction conditionss of two-stage paste state bed reactor are: pressure is 10.0 ~ 18.0MPa, volume space velocity is 0.5 ~ 2.0h
-1, hydrogen to oil volume ratio is 1200 ~ 5000.
8., according to slurry bed system and the fixed bed serial hydrogenation technique of the arbitrary described coal tar of claim 1 ~ 7, it is characterized in that,
Described Hydrobon catalyst is any one or a few in Co-Mo system, Ni-Mo system, Co-W system, Ni-W system.
9. according to claim 8 in the slurry bed system of coalite tar and fixed bed Unionfining technique, it is characterized in that,
The condition of described fixed bed hydrogenation reaction is: temperature is 220 ~ 450 DEG C, pressure is 12.0 ~ 18.0MPa, volume space velocity is 0.5 ~ 2.0h
-1, hydrogen to oil volume ratio is 500 ~ 3000.
10., according to slurry bed system and the fixed bed serial hydrogenation technique of the arbitrary described coal tar of claim 1 ~ 9, it is characterized in that,
Described coal tar is one or both in middle coalite tar or coal-tar heavy oil.
11. slurry bed system of coal tar and fixed bed serial hydrogenation techniques according to claim 10, is characterized in that,
Residual oil, heavy oil, high-sulfur oils, high asphalt content oil, any one or a few in high heavy metal content oil is added in the coal tar in described step (1).
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