CN102807895A - Hydrocracking method for increasing production of middle distillates - Google Patents
Hydrocracking method for increasing production of middle distillates Download PDFInfo
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Abstract
The invention relates to a hydrocracking method for increasing production of middle distillates. The method comprises the following steps that: fresh feedstock oils are simultaneously introduced into a hydrofining reactor and a hydrocracking reactor in a co-current flow way; a reaction effluent from the hydrofining reactor is separated to obtain light naphtha fractions, heavy naphtha fractions, middle distillates and tail oil fractions; all or part of the tail oil fractions are introduced into the hydrocracking reactor, and a reaction effluent from the hydrocracking reactor and part of the feedstock oils are introduced into the hydrofining reactor together. According to the method provided by the invention, the heavy distillates can be treated, and the maximum production of the middle distillates can be realized. Only the tail oil fractions are introduced into the hydrocracking reactor, so that the selectivity of middle distillates is improved; and part of the feedstock oils is introduced into the hydrocracking reactor, so that the phenomenon that the cracking activity of a hydrocracking catalyst is too strong, and more middle distillates are cracked secondarily in an ammonia-free environment in a hydrocracking reactor system is avoided, and thus the yield of the middle distillates is effectively improved.
Description
Technical field
The invention belongs to a kind of at the method for hydrogen cracking that has acquisition low boiler cut hydrocarbon ils under the situation of hydrogen.
Background technology
Strict day by day along with environmental requirement in the variation year by year of crude quality and the world wide; As the hydrocracking process of one of main means of crude oil secondary processing, heavy oil lighting, because the raw material suitability is strong, production decision is flexible; Liquid product yield is high; Good product quality is being brought into play more and more important effect in sulfur-bearing and high-sulfur crude oil deep processing production clean fuel process, its range of application is also increasingly extensive.
In recent years; Market to all kinds of oil products especially to the sustainable growth of high-quality intermediate oil product consumption; The pressure of refinery's production high-quality middle runnings oil prodn is also increasing, and therefore middle oil type hydrocracking technology is being brought into play more and more important effect in producing the clean fuel process.
Hydrocracking process generally can be divided into single agent single hop technology, single hop tandem process and two-stage process.The single hop technology that adopts amorphous hydrocracking catalyst once was the main processes that maximum is produced intermediate oil, but that its deficiency is an initial reaction temperature is higher, and the catalyzer cycle of operation is shorter, and is difficult to process heavier inferior raw material.Though two-stage process device flexibility of operation is bigger, adaptability to raw material is strong, the flow process relative complex, and infrastructure investment, catalyzer investment and running cost are all higher relatively.The one-stage serial technological process adopts the pattern of unifining, hydrocracking catalyst serial operation usually; Usually adopt active higher molecular sieve type catalyst in the hydrogen cracking section; Organic nitrogen compound is to the active disadvantageous effect of hydrocracking catalyst in the raw material; Need earlier raw material to be carried out the unifining pre-treatment, the nitrogen impurity content in the raw material is reduced to enough low level.With respect to amorphous hydrocracking catalyst, the molecular sieve type hydrocracking catalyst is active high, and initial reaction temperature is low, but the intermediate oil yield is relatively low.
WO97/38066 discloses the inverted sequence series connection method in a kind of hydroprocessing reactor assembly.This method is delivered to the unifining section with fresh feed with the elute of hydrocracking reaction section, and the reaction product of unifining section is removed NH in purification and cooling section
3And H
2Obtain hydrogen-rich gas and liquid phase stream after S and the cooling, hydrogen-rich gas returns the hydrocracking reaction section, and liquid phase stream gets into the unconverted oil and other lighting ends that the fractionation section obtains, and the gained unconverted oil is returned the hydrocracking reaction section.This method can further improve the hydrogen cracking quality product.
US6296758 discloses a kind of method for hydrogen cracking that improves the intermediate oil yield.This method is provided with a special Reaction Separation device on the basis of WO97/38066 method, top is gas phase hydrogenation refining reaction section, and the bottom is that gas is carried segregation section.This method can realize the unconverted oil circulation under working pressure, thereby realizes the economical operation under the low per pass conversion, improves quality product.
CN1216967C discloses the two-stage hydrocracking technology that a kind of maximum is produced intermediate oil.This method adopts the combination process route of " sequential flow " and " parallel-flow ".Adopt hydrotreatment and hydrogen cracking series connection at " sequential flow " hydrogen cracking section, obtain about 50% light-end products, only adopt amorphous hydrocracking catalyst to carry out the circulation cracking of tail oil at " parallel-flow " hydrogen cracking section.But this method maximum is produced intermediate oil, and can according to circumstances adjust production decision flexibly, and maximum is produced diesel oil or rocket(engine)fuel.
Summary of the invention
The objective of the invention is provides a kind of method for hydrogen cracking of voluminous intermediate oil on the prior art basis.
Method provided by the invention comprises:
(1) raw oil gets into hydrofining reactor and hydrocracking reactor by a certain percentage simultaneously with after hydrogen mixes;
(2) reaction effluent of hydrofining reactor gets into HP separator, light pressure separator, separation column successively, is separated obtaining light naphtha fraction, heavy naphtha fraction, intermediate oil and tail oil cut by separation column;
(3) all or part of tail oil cut gets into hydrocracking reactor, and the reaction effluent of hydrocracking reactor gets into hydrofining reactor with part material oil.
(4) said hydrofining reactor filling Hydrobon catalyst; Hydrocracking reactor top filling Hydrobon catalyst; Bottom filling hydrocracking catalyst, the Hydrobon catalyst that loads in the hydrocracking reactor and with the ratio of hydrocracking catalyst be 1: 6～1: 1.
The catalyzer of the Hydrobon catalyst of hydrocracking reactor top filling and hydrofining reactor filling can be identical, also can difference; The hydrocracking catalyst of hydrocracking reactor bottom filling is the molecular sieve carried non-noble metal catalyzer of crystal formation.Hydrocracking reactor top filling Hydrobon catalyst, filling hydrocracking catalyst in bottom can improve the flexibility of cracking reaction district to raw material.
Said raw oil is selected from one or more in straight run vacuum gas oil, wax tailings, the deasphalted oil, and boiling range is 260-700 ℃, 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 said raw oil is not more than 40000 μ g/g, and nitrogen content is not more than 2000 μ g/g.
Prior art adopts the pattern of unifining, hydrocracking catalyst serial operation usually.Contriver of the present invention finds; Under this operator scheme, because raw material has carried out the hydrogenation pre-treatment through the unifining section, when refining section is carried out desulfurization, denitrification reaction; A spot of lighting reaction can take place; With respect to raw oil, will contain the middle runnings of part (usually 10% ~ 20%) in this cracking zone charging, the raw oil after making with extra care directly contacts the very high hydrocracking catalyst of cracking activity; More secondary cracking reaction takes place in middle runnings easily, thereby has reduced the yield of intermediate oil.The present invention is in order to overcome this problem, and refining section outlet oil at first separates through separation column before getting into cracking case, and middle runnings is separated, and has avoided on hydrocracking catalyst, taking place the possibility of secondary cracking.With respect to the inverted sequence serial hydrocracking method of prior art, the invention provides fresh feed oil and get into technical scheme unifining section and hydrogen cracking section and stream simultaneously; Directly introduce the part fresh feed in the hydrogen cracking section; The cracking activity that suppresses hydrocracking catalyst through organic nitrogen compound in the fresh feed; Prevent that cracking activity is strong excessively under the hydrocracking reaction Duan Zaiwu ammonia environment; Cause the secondary cracking of more intermediate oil, thereby further improved the yield of intermediate oil.In addition; This part fresh feed oil gets into the technical scheme of hydrogen cracking section; Can prevent that the low excessively concentration of hydrogen sulfide of hydrocracking reaction section from causing hydrocracking catalyst under high hydrogen partial pressure conditions, to reduce, make the problem of the degradation such as activity, selectivity of hydrocracking catalyst.In addition, the hydrogen-rich stream of hydrocracking reactor goes out thing and enters into hydrofining reactor again, but economized cycle hydrogen consumption.The ratio that said raw oil gets into hydrofining reactor and hydrocracking reactor is 20: 1～1: 2.H in the atmosphere of said hydrocracking reactor
2The S dividing potential drop is 0.01～0.30MPa, NH
3Dividing potential drop is 0.001～0.05MPa.
The charging of said hydrofining reactor is: the reaction effluent of part fresh feed oil and whole hydrocracking reactors.Reaction conditions in the said hydrofining reactor: 300～450 ℃ of temperature of reaction, reaction pressure 3.0～20.0MPa, hydrogen to oil volume ratio 300～2000, the volume space velocity oily to fresh feed is 0.1～5.0h
-1
Said Hydrobon catalyst is to load on amorphous alumina or/and the loaded catalyst of the group vib base metal on the sial or VIII family base metal or its combination.Preferred Hydrobon catalyst is with γ-Al
2O
3Be carrier, the catalyst activity component is selected from one or more among the Mo, W, Co, Ni of group vib and VIII family metal component.
The reaction effluent of hydrofining reactor successively through fractionation with separate, obtain light naphtha fraction (less than 65 ℃), heavy naphtha fraction (65～145 ℃), intermediate oil (145～370 ℃) and tail oil cut (greater than 370 ℃).
The charging of said hydrocracking reactor is: all or part of tail oil, and part fresh feed oil.Reaction conditions in the said hydrocracking reactor: temperature of reaction is 300～450 ℃, reaction pressure 3.0～25.0MPa, and hydrogen to oil volume ratio 300～2000, volume space velocity are 0.5～8.0h
-1(to all chargings in the hydrocracking reactor).
Said hydrocracking catalyst is made up of a kind of carrier and the base metal that loads 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.With hydrocracking catalyst integral body is benchmark; In oxide compound, hydrocracking catalyst consists of: aluminum oxide 30 weight %～72 weight %, silica-alumina 10 weight %～52 weight %; Molecular sieve 1 weight %～15 weight %, group vib metal 15 weight %～35 weight %.Group VIII metal 2 weight %～8 weight %.
Said molecular screening one or more in faujusite, mordenite, zeolite L, omega zeolite, Beta zeolite.Said group vib metal and VIII family metal component are selected from one or more among Mo, W, Co, the Ni.
Advantage of the present invention is:
1, method provided by the invention can be handled heavy distillate, and maximum is produced intermediate oil.Compare with conventional one-stage serial hydrocracking method, the present invention only has the tail oil cut to get into the hydrogen cracking section, has improved the selectivity of intermediate oil.Compare with the inverted sequence serial hydrocracking method of prior art; After the present invention introduces hydrocracking reactor with fresh feed oil with the mode of " and stream "; Organic nitrogen compound wherein reaches the cracking activity that the ammonia that generates with afterreaction can partly suppress hydrocracking catalyst; Prevent in the hydrocracking reactor system that the cracking activity of hydrocracking catalyst is strong excessively under the no ammonia environment, cause the generation of more intermediate oil secondary cracking phenomenon, thereby help improving the yield of intermediate oil.
2, compare with the inverted sequence serial hydrocracking method of prior art, the introducing of fresh feed oil has increased the sulphur content in the hydrocracking reaction system, improves H
2The dividing potential drop of S can effectively be protected the activity and the selectivity of sulphided state hydrocracking catalyst.
Description of drawings
Accompanying drawing is the schematic flow sheet of the method for hydrogen cracking of voluminous intermediate oil provided by the present invention.
Embodiment
Accompanying drawing is the schematic flow sheet that the present invention provides method, has omitted many equipment among the figure, like pump, interchanger, compressor etc., but for a person skilled in the art, is known.
Below in conjunction with accompanying drawing, to method provided by the present invention, further specify, but therefore do not limit the present invention.Shown in accompanying drawing; Raw oil gets into storage tank 1 through pipeline 9; New hydrogen mixes with raw oil after pipeline 10 gets into make-up hydrogen compressor 2 superchargings; Mixture gets into process furnace 12 through pipeline 11, and the mixture after the heating is divided into two-way: a route pipeline 13 gets into hydrofining reactor 4, and another route pipeline 14 gets into hydrocracking reactor 3.Desulfurization, denitrogenation take place in raw oil and hydrogen under the Hydrobon catalyst effect in hydrofining reactor 4, alkene is saturated and the aromatic hydrocarbons saturated reaction; Reaction effluent is flowed through heat exchange, cooling after pipeline 28 entering HP separators 5 carry out gas-liquid separation; The hydrogen rich stream at HP separator 5 tops gets into circulating hydrogen compressor 6 by pipeline 15, after the circulating hydrogen compressor supercharging, divides two curb pipelines 18 and pipeline 29 to get into hydrofining reactor 4 and hydrocracking reactor 3 respectively.The sour water of HP separator 5 bottoms is discharged through pipeline 17, and HP separator 5 bottom liquid phase streams get into light pressure separator 7 through pipeline 16, carry out further gas-liquid separation at this.Mortgage separator 7 isolated gases are extracted out through pipeline 19; The sour water of light pressure separator 7 bottoms is discharged through pipeline 21; The liquid phase stream of light pressure separator 7 bottoms gets into separation column through pipeline 20.Separation column 8 cats head are told lighter hydrocarbons and light naphtha fraction and are extracted out through pipeline 22, heavy naphtha fraction through top side line 23 extract out, intermediate oil through the bottom side line 24 extract out, the tail oil cut is extracted out through pipeline 25 at the bottom of the tower, after be divided into two-way.All or part of tail oil cut is circulated to hydrocracking reactor 3 inlets behind pipeline 27; React under the effect of Hydrobon catalyst and hydrocracking catalyst with part fresh feed oil, the resultant of reaction of bottom gets into hydrofining reactor 4.Alternatively with part tail oil cut through pipeline 26 withdrawing devices.
Following embodiment will further explain method provided by the invention, but therefore do not limit the present invention.
Used raw oil A is a kind of VGO among the embodiment, and its main character is as shown in table 1.
The trade names of hydrofining reactor filling hydrogenation protecting catalyst are RG-1 among the embodiment; The trade names of Hydrobon catalyst are RN-32V; The trade names of the Hydrobon catalyst of hydrocracking reactor filling are RN-32V, and the trade names of the hydrocracking catalyst of filling are RHC-131.Adopt identical catalyzer and type of feed in the Comparative Examples.Above-mentioned catalyzer is produced by Sinopec catalyzer branch office.
Embodiment 1
In reaction pressure is 14.5MPa, 380 ℃ of unifining section temperature of reaction, and 375 ℃ of hydrogen cracking section temperature of reaction, it is 1.8h that the unifining segment body amasss air speed (to fresh feed)
-1, it is 1.3h that the hydrogen cracking segment body amasss air speed (to the whole chargings of hydrogen cracking section)
-1Reaction conditions under, with method for hydrogen cracking provided by the invention, adopt raw material A to carry out test.Catalyzer RN-32V and the ratio between the RHC-131 that the hydrogen cracking section is adopted are 1: 4; The ratio that fresh feed oil gets into hydrofining reactor and hydrocracking reactor is 5: 1, and the tail oil cut all loops back hydrocracking reactor.H in the hydrocracking reactor reaction atmosphere
2The S dividing potential drop is 0.025MPa, NH
3Dividing potential drop is 0.006MPa.Test-results is as shown in table 2, and in fresh feed 100%, product boat coal, diesel yield are respectively 40.80% and 38.54%, and the intermediate oil total recovery is 79.34%, and total liquid product yield is 97.20%.
Embodiment 2
In reaction pressure is 14.5MPa, 375 ℃ of unifining section temperature of reaction, and 380 ℃ of hydrogen cracking section temperature of reaction, it is 1.8h that the unifining segment body amasss air speed (to fresh feed)
-1, it is 1.3h that the hydrogen cracking segment body amasss air speed (to the whole chargings of hydrogen cracking section)
-1Reaction conditions under, with method for hydrogen cracking provided by the invention, adopt raw material A to carry out test, catalyzer RN-32V and the ratio between the RHC-131 that the hydrogen cracking section is adopted are 1: 2; The ratio that fresh feed oil gets into hydrofining reactor and hydrocracking reactor is 1.5: 1, and the tail oil cut all loops back hydrocracking reactor.H in the hydrocracking reactor reaction atmosphere
2The S dividing potential drop is 0.06MPa, NH
3Dividing potential drop is 0.014MPa.Test-results is as shown in table 3, and in fresh feed 100%, product boat coal, diesel yield are respectively 40.92% and 38.82%, and the intermediate oil total recovery is 79.74%, and total liquid product yield is 97.25%.
Comparative Examples
In reaction pressure is 14.5MPa, 380 ℃ of unifining section temperature of reaction, and 350 ℃ of hydrogen cracking section temperature of reaction, it is 1.8h that the unifining segment body amasss air speed (to fresh feed)
-1, the hydrogen cracking segment body amasss air speed (to the whole chargings of hydrogen cracking section) 1.3h
-1Reaction conditions under; With the inverted sequence serial hydrocracking method, adopt raw material A to carry out test, fresh feed oil all gets into hydrofining reactor; Elute with hydrocracking reactor reacts in hydrofining reactor; After the reaction product separation and fractionation of hydrofining reactor, obtain hydrogen-rich gas and return hydrocracking reactor, the tail oil cut that fractionation obtains all loops back hydrocracking reactor.H in the 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 the intermediate oil total recovery is 76.55%, and total liquid product yield is 96.30%.
Table 1 raw oil character
| The raw oil numbering | A |
| Density (20 ℃)/(g/cm 3) | 0.9035 |
| S content/% | 1.3 |
| N content/(μ g/g) | 1300 |
| Condensation point/℃ | 33 |
| Refractive index/n D 70 | 1.4861 |
| Boiling range (D-1160)/℃ | |
| Over point | 277 |
| 10% | 388 |
| 50% | 426 |
| 90% | 466 |
| Final boiling point | 532 |
Table 2
| Product | Petroleum naphtha | The boat coal | Diesel oil |
| The boiling range scope/℃ | <145 | 145-230 | 230-370 |
| Quality product yield/% | 17.86 | 40.80 | 38.54 |
| Density (20 ℃)/(g/cm 3) | 0.734 | 0.791 | 0.825 |
| 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 | The boat coal | Diesel oil |
| The boiling range scope/℃ | <145 | 145-230 | 145-370 |
| Liquid product mass yield/% | 17.51 | 40.92 | 38.82 |
| Density (20 ℃)/(g/cm 3) | 0.735 | 0.793 | 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 |
Table 4
| Product | Petroleum naphtha | The boat coal | Diesel oil |
| The boiling range scope/℃ | <145 | 145-230 | 230-370 |
| Quality product yield/% | 19.75 | 39.49 | 37.06 |
| Density (20 ℃)/(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. the method for hydrogen cracking of a voluminous intermediate oil comprises:
(1) raw oil gets into hydrofining reactor and hydrocracking reactor by a certain percentage simultaneously with after hydrogen mixes;
(2) reaction effluent of hydrofining reactor gets into HP separator, light pressure separator, separation column successively, is separated obtaining light naphtha fraction, heavy naphtha fraction, intermediate oil and tail oil cut by separation column;
(3) all or part of tail oil cut gets into hydrocracking reactor, and the reaction effluent of hydrocracking reactor gets into hydrofining reactor with part material oil;
(4) said hydrofining reactor filling Hydrobon catalyst; Hydrocracking reactor top filling Hydrobon catalyst; Bottom filling hydrocracking catalyst, the Hydrobon catalyst that loads in the hydrocracking reactor and with the ratio of hydrocracking catalyst be 1: 6～1: 1.
2. according to the described method of claim 1; It is characterized in that said raw oil is selected from one or more in straight run vacuum gas oil, wax tailings, the deasphalted oil, boiling range is 260-700 ℃; Sulphur content is not more than 50000 μ g/g, and nitrogen content is not more than 5000 μ g/g.
3. according to the described method of claim 1, it is characterized in that the sulphur content of said raw oil is not more than 40000 μ g/g, nitrogen content is not more than 2000 μ g/g.
4. according to the described method of claim 1, it is characterized in that the ratio that said raw oil gets into hydrofining reactor and hydrocracking reactor is 20: 1～1: 2.
5. according to the described method of claim 1, it is characterized in that H in the atmosphere of said hydrocracking reactor
2The S dividing potential drop is 0.01～0.30MPa, NH
3Dividing potential drop is 0.001～0.05MPa.
6. according to the described method of claim 1; It is characterized in that reaction conditions in the said hydrofining reactor: 300～450 ℃ of temperature of reaction, reaction pressure 3.0～20.0MPa; Hydrogen to oil volume ratio 300～2000, the volume space velocity oily to fresh feed is 0.1～5.0h
-1
7. according to the described method of claim 1, it is characterized in that reaction conditions in the said hydrocracking reactor: temperature of reaction is 300～450 ℃, reaction pressure 3.0～25.0MPa, and hydrogen to oil volume ratio 300～2000, volume space velocity are 0.5～8.0h
-1
8. according to the described method of claim 1, it is characterized in that said Hydrobon catalyst is to load on amorphous alumina or/and the loaded catalyst of the group vib base metal on the sial or VIII family base metal or its combination.
9. according to the described method of claim 1, it is characterized in that said hydrocracking catalyst is made up of a kind of carrier and the base metal that loads on this carrier, this carrier is made up of amorphous aluminum silicide and molecular sieve.
10. according to the described method of claim 9; It is characterized in that, be benchmark with hydrocracking catalyst integral body, in oxide compound; Hydrocracking catalyst consists of: aluminum oxide 30 weight %～72 weight %; Silica-alumina 10 weight %～52 weight %, molecular sieve 1 weight %～15 weight %, group vib metal 15 weight %～35 weight %.Group VIII metal 2 weight %～8 weight %.
11., it is characterized in that said molecular screening one or more in faujusite, mordenite, zeolite L, omega zeolite, Beta zeolite according to claim 9 or 10 described methods.
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| CN111088072A (en) * | 2018-10-24 | 2020-05-01 | 中国石油化工股份有限公司 | Hydrocracking method for reducing heavy naphtha bromine index and increasing aviation kerosene smoke point |
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| CN1478868A (en) * | 2002-08-29 | 2004-03-03 | 中国石油化工股份有限公司 | Hydrogenation cracking method for maximally producing intermediate distillate |
| 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 |
| CN101760233A (en) * | 2008-12-24 | 2010-06-30 | 中国石油化工股份有限公司 | Method for hydrocracking of coked wax oil |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1478868A (en) * | 2002-08-29 | 2004-03-03 | 中国石油化工股份有限公司 | Hydrogenation cracking method for maximally producing intermediate distillate |
| 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 |
| CN101760233A (en) * | 2008-12-24 | 2010-06-30 | 中国石油化工股份有限公司 | Method for hydrocracking of coked wax oil |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111088072A (en) * | 2018-10-24 | 2020-05-01 | 中国石油化工股份有限公司 | Hydrocracking method for reducing heavy naphtha bromine index and increasing aviation kerosene smoke point |
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