CN103509599B - A kind of cocurrent flow type method of hydrotreating producing intermediate oil - Google Patents
A kind of cocurrent flow type method of hydrotreating producing intermediate oil Download PDFInfo
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Abstract
A kind of cocurrent flow type method of hydrotreating producing intermediate oil, fresh feed oil is introduced hydrofining reactor and hydrocracking reactor in the mode also flowed simultaneously, the fresh feed oil content wherein entering hydrocracking reactor is multiply, respectively from charging between the bed of hydrocracking reactor; The reaction effluent of hydrofining reactor enters hydrocracking reactor through being separated tail oil fraction, and the reaction effluent of hydrocracking reactor enters hydrofining reactor together with part material oil.Method provided by the invention can process heavy distillate, and maximum produces intermediate oil.
Description
Technical field
The invention belongs to a kind of method for hydrogen cracking obtaining low boiler cut hydrocarbon ils in the presence of hydrogen.
Background technology
Along with being deteriorated year by year and environmental requirement increasingly strict in world wide of crude quality, as the hydrocracking process of one of the Main Means of crude oil secondary processing, heavy oil lighting, because adaptability to raw materials is strong, production decision is flexible, liquid product yield is high, good product quality, produce in clean fuel process at sulfur-bearing and high-sulfur crude oil deep processing and play more and more important effect, its range of application is also increasingly extensive.
In recent years, market to all kinds of oil product especially to the sustainable growth of high-quality intermediate oil product consumption, the pressure of refinery's production high-quality middle runnings oil production is also increasing, and therefore, oil type hydrocracking technique plays more and more important effect in production clean fuel process.
Hydrocracking process generally can be divided into single dose single stage process, single hop tandem process and two-stage process.Adopt the single stage process of amorphous hydrocracking catalyst to be once that maximum produces the main processes of intermediate oil, but its deficiency to be initial reaction temperature higher, catalyst on-stream cycle time is shorter, and is difficult to process heavier inferior raw material.Although two-stage process device flexibility of operation is comparatively large, adaptability to raw material is strong, flow process relative complex, the investment of infrastructure investment, catalyzer and running cost all relatively high.One-stage serial technological process adopts the pattern of hydrofining, hydrocracking catalyst serial operation usually, usually active higher molecular sieve type catalyst is adopted in hydrocracking section, in raw material, organic nitrogen compound is to the disadvantageous effect of hydrocracking catalyst activity, need first to carry out hydrofining pre-treatment to raw material, the nitrogen impurity content in raw material is down to enough low level.Relative to amorphous hydrocracking catalyst, molecular sieve type hydrocracking catalyst activity is high, and initial reaction temperature is low, but intermediate oil yield is relatively low.
WO97/38066 discloses the inverted sequence series connection method in a kind of hydroprocessing reactor assembly.Fresh feed is delivered to hydrofining section by the method together with the effluent of hydrocracking reaction section, and the reaction product of hydrofining section is at purification and cooling section removing NH
3and H
2s also obtains hydrogen-rich gas and liquid phase stream after cooling, and hydrogen-rich gas returns hydrocracking reaction section, and liquid phase stream enters the unconverted oil and other lighting ends that distillation stage obtains, and gained unconverted oil returns hydrocracking reaction section.The method can further improve hydrocracked product quality.
US6296758 discloses a kind of method for hydrogen cracking improving intermediate oil yield.The method is on the basis of WO97/38066 method, and arrange a special Reaction Separation device, top is gas phase hydrogenation refining reaction section, and bottom is air lift segregation section.The method can realize unconverted oil circulation under operating pressure, thus realizes the economical operation under low per pass conversion, improves quality product.
CN1216967C discloses the two-stage hydrocracking technique that a kind of maximum produces intermediate oil.The method adopts " order stream " and the combination process route of " parallel-flow ".Adopt hydrotreatment and hydrocracking series connection at " order stream " hydrocracking section, obtain the light-end products of about 50%, only adopt amorphous hydrocracking catalyst to carry out the circulation cracking of tail oil at " parallel-flow " hydrocracking section.The method maximum can produce intermediate oil, and according to circumstances can adjust production decision flexibly, maximum diesel oil yield or rocket engine fuel.
Prior art adopts the pattern of hydrofining, hydrocracking catalyst serial operation usually.The present inventor finds, under this operator scheme, because raw material has carried out weighted BMO spaces through hydrofining section, while refining stage carries out desulfurization, denitrification reaction, also a small amount of lighting reaction can be there is, relative in this cracking zone charging of stock oil by containing part (usually 10% ~ 20%) middle runnings, stock oil after refining directly contacts the very high hydrocracking catalyst of cracking activity, easily there is more secondary cracking reaction in middle runnings, thus reduces the yield of intermediate oil.The present invention is in order to overcome this problem, and first refining stage outlet oil be separated through separation column before entering cracking case, middle runnings separated, and avoids the possibility that secondary cracking occurs on hydrocracking catalyst.Relative to the inverted sequence serial hydrocracking method of prior art, the invention provides the technical scheme that fresh feed oil enters the also stream of hydrofining section and hydrocracking section simultaneously, at the direct introducing portion fresh feed of hydrocracking section, the cracking activity of hydrocracking catalyst is suppressed by organic nitrogen compound in fresh feed, under preventing hydrocracking reaction Duan Wu ammonia environment, cracking activity is excessively strong, cause the secondary cracking of more intermediate oil, thus further increase the yield of intermediate oil.In addition, containing the fresh feed of organic nitrogen compound from charging between hydrocracking reactor each bed, cause hydrocracking reactor top bed poisoning of catalyst inactivation when avoiding nitrogen content higher, while raising intermediate oil yield, optimize hydrocracking reactor reaction atmosphere further.
This part fresh feed oil enters the technical scheme of hydrocracking section, also can prevent the too low concentration of hydrogen sulfide of hydrocracking reaction section from causing hydrocracking catalyst to reduce under high hydrogen partial pressure conditions, make the problem of the degradation such as the activity of hydrocracking catalyst, selectivity.In addition, the hydrogen-rich stream effluent of hydrocracking reactor enters into hydrofining reactor again, can save recycle hydrogen consumption.
The part by weight that described fresh feed oil enters hydrofining reactor and hydrocracking reactor is 20:1 ~ 1:1.The described fresh feed oil content entering hydrocracking reactor is 2-6 stock, respectively from charging between the bed of hydrocracking reactor; Overall for benchmark with the fresh feed oil entering hydrocracking reactor, by weight, the every stock material between hydrocracking reactor bed is 10% ~ 50%; Described tail oil fraction enters hydrocracking reactor from the top of hydrocracking reactor.
H in the atmosphere of described hydrocracking reactor
2s dividing potential drop is 0.01 ~ 0.30MPa, NH
3dividing potential drop is 0.001 ~ 0.05MPa.
The charging of described hydrofining reactor is: the reaction effluent of part fresh feed oil and whole hydrocracking reactor.Reaction conditions in described hydrofining reactor: temperature of reaction 300 ~ 450 DEG C, reaction pressure 3.0 ~ 20.0MPa, hydrogen to oil volume ratio 300 ~ 2000 is 0.1 ~ 5.0h to the volume space velocity of fresh feed oil
-1.
Described Hydrobon catalyst be load at amorphous alumina or/and the loaded catalyst of group vib base metal on sial or VIII base metal or its combination.Preferred Hydrobon catalyst is with γ-Al
2o
3for carrier, catalyst activity component is selected from one or more in Mo, W, Co, Ni of group vib and group VIII metal component.
The reaction effluent of hydrofining reactor successively through fractionation be separated, obtain light naphtha fraction (being less than 65 DEG C), heavy naphtha fraction (65 ~ 145 DEG C), intermediate oil (145 ~ 370 DEG C) and tail oil fraction (being greater than 370 DEG C).
The charging of described hydrocracking reactor is: all or part of tail oil, and part fresh feed oil.Reaction conditions in described hydrocracking reactor: temperature of reaction is 300 ~ 450 DEG C, reaction pressure 3.0 ~ 25.0MPa, hydrogen to oil volume ratio 300 ~ 2000, volume space velocity is 0.5 ~ 8.0h
-1(for chargings all in hydrocracking reactor).
Described hydrocracking catalyst is made up of a kind of carrier and load base metal on this carrier, and this carrier is made up of amorphous aluminum silicide and molecular sieve.Wherein, amorphous aluminum silicide is selected from one or more in silicon oxide, aluminum oxide or their combination.Overall for benchmark with hydrocracking catalyst, with oxide basis, hydrocracking catalyst consists of: aluminum oxide 30 % by weight ~ 72 % by weight, silica-alumina 10 % by weight ~ 52 % by weight, molecular sieve 1 % by weight ~ 15 % by weight, group vib metal 15 % by weight ~ 35 % by weight.Group VIII metal 2 % by weight ~ 8 % by weight.
One or more in faujusite, mordenite, zeolite L, omega zeolite, Beta zeolite of described molecular screening.Described group vib metal and group VIII metal component are selected from one or more in Mo, W, Co, Ni.
Advantage of the present invention is:
1, method provided by the invention can process heavy distillate, and maximum produces intermediate oil.Compared with conventional one-stage serial hydrocracking method, the present invention only has tail oil fraction to enter hydrocracking section, improves the selectivity of intermediate oil.Compared with the inverted sequence serial hydrocracking method of prior art, after fresh feed oil is introduced hydrocracking reactor in the mode of " and stream " by the present invention, the ammonia that organic nitrogen compound wherein and following reaction generate partly can suppress the cracking activity of hydrocracking catalyst, prevent in hydrocracking reactor system excessively strong without the cracking activity of hydrocracking catalyst under ammonia environment, cause the generation of more intermediate oil secondary cracking phenomenon, thus be conducive to the yield improving intermediate oil.
2, containing the fresh feed oil of organic nitrogen compound from charging between hydrocracking reactor each bed, hydrocracking reactor top bed poisoning of catalyst inactivation is caused when avoiding nitrogen content higher, while raising intermediate oil yield, optimize hydrocracking reactor reaction atmosphere further, and the selectivity of the intermediate oil of middle and lower part, cracking reaction district bed hydrocracking reaction can be improved.
3, compared with the inverted sequence serial hydrocracking method of prior art, the introducing of fresh feed oil adds the sulphur content in hydrocracking reaction system, improves H
2the dividing potential drop of S, can the activity and selectivity of available protecting sulphided state hydrocracking catalyst.
Summary of the invention
The object of the invention is on prior art basis, a kind of cocurrent flow type method of hydrotreating producing intermediate oil is provided.
Method provided by the invention comprises:
(1) after stock oil mixes with hydrogen, enter hydrofining reactor and hydrocracking reactor by a certain percentage, the stock oil wherein entering hydrocracking reactor is divided into multiply simultaneously, respectively from charging between the bed of hydrocracking reactor;
(2) reaction effluent of hydrofining reactor enters high-pressure separator, light pressure separator, separation column successively, is separated obtains light naphtha fraction, heavy naphtha fraction, intermediate oil and tail oil fraction by separation column;
(3) all or part of tail oil fraction enters hydrocracking reactor, and the reaction effluent of hydrocracking reactor enters hydrofining reactor together with part material oil.
Described stock oil is selected from one or more in straight run vacuum gas oil, wax tailings, deasphalted oil, and boiling range is 260-700 DEG C, and sulphur content is not more than 50000 μ g/g, and nitrogen content is not more than 5000 μ g/g.The sulphur content of preferred described stock oil is not more than 40000 μ g/g, and nitrogen content is not more than 2000 μ g/g.
Accompanying drawing explanation
Accompanying drawing is the schematic flow sheet of the cocurrent flow type method of hydrotreating of production intermediate oil provided by the present invention.
Embodiment
Below in conjunction with accompanying drawing, to method provided by the present invention, be further described, but not thereby limiting the invention.As shown in drawings, stock oil enters storage tank 1 through pipeline 10, new hydrogen enters after make-up hydrogen compressor 2 supercharging through pipeline 11 and mixes with stock oil, mixture enters process furnace 9 through pipeline 12, mixture after heating is divided into two-way: a route pipeline 17 enters hydrofining reactor 4, and another road part is mixed hydrogen oil content and do not entered hydrocracking reactor 3 by pipeline 13,14,15 and 16.Under Hydrobon catalyst effect, desulfurization, denitrogenation, olefin saturated and aromatic saturation reaction is there is at hydrofining reactor 4 Raw oil and hydrogen, reaction effluent enters high-pressure separator 5 through pipeline 18 after flowing through heat exchange, cooling and carries out gas-liquid separation, the hydrogen rich stream at high-pressure separator 5 top enters circulating hydrogen compressor 6 by pipeline 19, after circulating hydrogen compressor supercharging, point two-way, enters hydrofining reactor 4 and hydrocracking reactor 3 respectively along pipeline 22.Sour water bottom high-pressure separator 5 is discharged through pipeline 21, and high-pressure separator 5 lower liquid phase stream passes via line 20 enters light pressure separator 7, carries out further gas-liquid separation at this.The isolated gas of light pressure separator 7 is extracted out through pipeline 23; Sour water bottom light pressure separator 7 is discharged through pipeline 25; The liquid phase stream of light pressure separator 7 bottom enters separation column 8 through pipeline 24.Separation column 8 tower top separates lighter hydrocarbons and light naphtha fraction is extracted out through pipeline 26, and heavy naphtha fraction is extracted out through top side line 27, and intermediate oil is extracted out through bottom side line 28, and tail oil fraction at the bottom of tower is divided into two-way after extracting out.All or part of tail oil fraction is through pipeline 30 Posterior circle to hydrocracking reactor 3 entrance, and react under the effect at hydrocracking catalyst together with part fresh feed oil, the resultant of reaction of bottom enters hydrofining reactor 4.Alternatively by part tail oil fraction through pipeline 29 withdrawing device.
The following examples to method provided by the invention, will be further described, but not thereby limiting the invention.
Stock oil A used in embodiment is a kind of VGO, and its main character is as shown in table 1.
In embodiment, the trade names of hydrofining reactor filling hydrogenation protecting catalyst are RG-1, and the trade names of Hydrobon catalyst are RN-32V, and the trade names of hydrocracking reactor filling hydrocracking catalyst are RHC-131.Identical catalyzer and type of feed is adopted in comparative example.Above-mentioned catalyzer all has Sinopec catalyzer branch office to produce.
Embodiment 1
Be 14.5MPa in reaction pressure, hydrofining reactor temperature of reaction 380 DEG C, hydrocracking reactor temperature of reaction 368 DEG C, hydrofining reactor volume space velocity (to fresh feed) is 1.8h
-1, hydrocracking reactor volume space velocity (to the whole charging of hydrocracking reactor) is 1.3h
-1reaction conditions under, with method for hydrogen cracking provided by the invention, adopt raw material A to carry out test, the ratio that fresh feed oil enters hydrofining reactor and hydrocracking reactor is 10:1, and tail oil fraction all loops back hydrocracking reactor.Hydrocracking reactor arranges four beds, and every bed inlet fresh feed amount accounts for 25 % by weight, H in hydrocracking reactor reaction atmosphere of hydrocracking reactor fresh feed total amount
2s dividing potential drop is from top to bottom in increasing progressively Gradient distribution, and a bed outlet is 0.004MPa, and reactor exit is 0.016MPa to the maximum, NH in hydrocracking reactor reaction atmosphere
3dividing potential drop is from top to bottom in increasing progressively Gradient distribution, and a bed outlet is 0.0007MPa, and reactor outlet is 0.003MPa to the maximum.Test-results is as shown in table 2, and in fresh feed 100%, product boat coal, diesel yield are respectively 42.20% and 39.13%, and intermediate oil total recovery is 81.33%, and total liquid product yield is 97.95%.
Embodiment 2
Be 14.5MPa in reaction pressure, hydrofining reactor temperature of reaction 380 DEG C, hydrocracking reactor temperature of reaction 360 DEG C, hydrofining reactor volume space velocity (to fresh feed) is 1.8h
-1, hydrocracking reactor volume space velocity (to the whole charging of hydrocracking reactor) is 1.3h
-1reaction conditions under, with method for hydrogen cracking provided by the invention, adopt raw material A to carry out test, the ratio that fresh feed oil enters hydrofining reactor and hydrocracking reactor is 20:1, and tail oil fraction all loops back hydrocracking reactor.Hydrocracking reactor arranges four beds, and every bed inlet fresh feed oil mass accounts for 25 % by weight, H in hydrocracking reactor reaction atmosphere of hydrocracking reactor fresh feed oil total amount
2s dividing potential drop is from top to bottom in increasing progressively Gradient distribution, and a bed exports H
2s dividing potential drop is 0.0015MPa, and reactor outlet maximum value is 0.006MPa; NH in hydrocracking reactor
3dividing potential drop is from top to bottom in increasing progressively Gradient distribution, and a bed outlet is 0.0003MPa, and reactor outlet maximum value is 0.0012MPa.Test-results is as shown in table 3, and in fresh feed 100%, product boat coal, diesel yield are respectively 41.50% and 38.65%, and intermediate oil total recovery is 80.15%, and total liquid product yield is 97.60%.
Comparative example
Be 14.5MPa in reaction pressure, hydrofining section temperature of reaction 380 DEG C, hydrocracking section temperature of reaction 350 DEG C, hydrofining section volume space velocity (to fresh feed) is 1.8h
-1, hydrocracking section volume space velocity (to the whole charging of hydrocracking section) 1.3h
-1reaction conditions under, with conventional inverted sequence serial hydrocracking method, raw material A is adopted to carry out test, fresh feed oil all enters hydrofining reactor, react in hydrofining reactor together with the effluent of hydrocracking reactor, the reaction product of hydrofining reactor is separated and after fractionation, obtain hydrogen-rich gas and return hydrocracking reactor, the tail oil fraction that fractionation obtains all loops back hydrocracking reactor.H in hydrocracking reactor reaction atmosphere
2s dividing potential drop, NH
3dividing potential drop is 0.Test-results is as shown in table 4, and in fresh feed 100%, product boat coal, diesel yield are respectively 39.49% and 37.06%, and intermediate oil total recovery is 76.55%, and total liquid product yield is 96.30%.
Table 1 stock oil character
| Stock oil is numbered | A |
| Density (20 DEG C)/(g/cm 3) | 0.9035 |
| S content/% | 1.3 |
| N content/(μ g/g) | 1300 |
| Condensation point/DEG C | 33 |
| Refractive index/n D 70 | 1.4861 |
| Boiling range (D-1160)/DEG C | |
| Initial boiling point | 277 |
| 10% | 388 |
| 50% | 426 |
| 90% | 466 |
| Final boiling point | 532 |
Table 2
| Product | Petroleum naphtha | Boat coal | Diesel oil |
| Boiling range scope/DEG C | <145 | 145-230 | 230-370 |
| Quality product yield/% | 16.62 | 42.20 | 39.13 |
| Density (20 DEG C)/(g/cm 3) | 0.734 | 0.790 | 0.827 |
| Total sulfur/(μ g/g) | <1 | <10 | <10 |
| Total nitrogen/(μ g/g) | <0.5 | <1 | <1 |
| Arene underwater content/% | >45 | / | / |
| Smoke point/mm | / | >25 | / |
| Cetane value | / | / | >65 |
Table 3
| Product | Petroleum naphtha | Boat coal | Diesel oil |
| Boiling range scope/DEG C | <145 | 145-230 | 145-370 |
| Liquid product mass yield/% | 17.45 | 41.50 | 38.65 |
| Density (20 DEG C)/(g/cm 3) | 0.735 | 0.792 | 0.827 |
| Total sulfur/(μ g/g) | <1 | <10 | <10 |
| Total nitrogen/(μ g/g) | <0.5 | <1 | <1 |
| Arene underwater content/% | >45 | / | / |
| Smoke point/mm | / | >25 | / |
| Cetane value | / | / | >65 |
Table 4
| Product | Petroleum naphtha | Boat coal | Diesel oil |
| Boiling range scope/DEG C | <145 | 145-230 | 230-370 |
| Quality product yield/% | 19.75 | 39.49 | 37.06 |
| Density (20 DEG C)/(g/cm 3) | 0.732 | 0.792 | 0.826 |
| Total sulfur/(μ g/g) | <1 | <10 | <10 |
| Total nitrogen/(μ g/g) | <0.5 | <1 | <1 |
| Arene underwater content/% | >45 | / | / |
| Smoke point/mm | / | >25 | / |
| Cetane value | / | / | >65 |
Claims (11)
1. produce a cocurrent flow type method of hydrotreating for intermediate oil, comprising:
(1) after stock oil mixes with hydrogen, enter hydrofining reactor and hydrocracking reactor by a certain percentage, the stock oil wherein entering hydrocracking reactor is divided into multiply simultaneously, respectively from charging between the bed of hydrocracking reactor;
(2) reaction effluent of hydrofining reactor enters high-pressure separator, light pressure separator, separation column successively, is separated obtains light naphtha fraction, heavy naphtha fraction, intermediate oil and tail oil fraction by separation column;
(3) all or part of tail oil fraction enters hydrocracking reactor, and the reaction effluent of hydrocracking reactor enters hydrofining reactor together with part material oil;
H in the atmosphere of described hydrocracking reactor
2s dividing potential drop is 0.01 ~ 0.30MPa, NH
3dividing potential drop is 0.001 ~ 0.05MPa.
2. in accordance with the method for claim 1, it is characterized in that, described stock oil is selected from one or more in straight run vacuum gas oil, wax tailings, deasphalted oil, and boiling range is 260-700 DEG C, sulphur content is not more than 50000 μ g/g, and nitrogen content is not more than 5000 μ g/g.
3. in accordance with the method for claim 1, it is characterized in that, the sulphur content of described stock oil is not more than 40000 μ g/g, and nitrogen content is not more than 2000 μ g/g.
4. in accordance with the method for claim 1, it is characterized in that, the part by weight that described stock oil enters hydrofining reactor and hydrocracking reactor is: 20:1 ~ 1:1.
5. in accordance with the method for claim 1, it is characterized in that, described in enter hydrocracking reactor stock oil be divided into 2-6 stock, respectively from charging between the bed of hydrocracking reactor; Overall for benchmark with the stock oil entering hydrocracking reactor, by weight, the every stock material between hydrocracking reactor bed is 10% ~ 50%; Described tail oil fraction enters hydrocracking reactor from the top of hydrocracking reactor.
6. in accordance with the method for claim 1, it is characterized in that, reaction conditions in described hydrofining reactor: temperature of reaction 300 ~ 450 DEG C, reaction pressure 3.0 ~ 20.0MPa, hydrogen to oil volume ratio 300 ~ 2000 is 0.1 ~ 5.0h to the volume space velocity of fresh feed oil
-1.
7. in accordance with the method for claim 1, it is characterized in that, reaction conditions in described hydrocracking reactor: temperature of reaction is 300 ~ 450 DEG C, reaction pressure 3.0 ~ 25.0MPa, hydrogen to oil volume ratio 300 ~ 2000, volume space velocity is 0.5 ~ 8.0h
-1.
8. in accordance with the method for claim 1, it is characterized in that, described Hydrobon catalyst be load at amorphous alumina or/and the loaded catalyst of group vib base metal on sial or VIII base metal or its combination.
9. in accordance with the method for claim 1, it is characterized in that, described hydrocracking catalyst is made up of a kind of carrier and load base metal on this carrier, and this carrier is made up of amorphous aluminum silicide and molecular sieve.
10. in accordance with the method for claim 9, it is characterized in that, overall for benchmark with hydrocracking catalyst, with oxide basis, hydrocracking catalyst consists of: aluminum oxide 30 % by weight ~ 72 % by weight, silica-alumina 10 % by weight ~ 52 % by weight, molecular sieve 1 % by weight ~ 15 % by weight, group vib metal 15 % by weight ~ 35 % by weight, group VIII metal 2 % by weight ~ 8 % by weight.
11., according to the method described in claim 9 or 10, is characterized in that, one or more in faujusite, mordenite, zeolite L, omega zeolite, Beta zeolite of described molecular screening.
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| CN110643390B (en) * | 2019-08-22 | 2021-10-22 | 中科合成油工程有限公司 | Hydrogenation method of high-reactivity oil product |
| CN111871333B (en) * | 2020-07-16 | 2023-06-27 | 南京延长反应技术研究院有限公司 | Micro-interface reaction system and method for anthracene oil hydrogenation |
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| FR2812302B1 (en) * | 2000-07-31 | 2003-09-05 | Inst Francais Du Petrole | 2-STEP HYDROCRACKING PROCESS OF HYDROCARBON CHARGES |
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| US1966617A (en) * | 1930-10-09 | 1934-07-17 | Rca Corp | Scanning device |
| CN1766054A (en) * | 2004-10-29 | 2006-05-03 | 中国石油化工股份有限公司 | Two-stage hydrocracking method for increasing yield of middle distillate oil |
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