CN102453537A - Method for maximum production of clean diesel oil by shale oil whole fraction hydrogenation - Google Patents
Method for maximum production of clean diesel oil by shale oil whole fraction hydrogenation Download PDFInfo
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Abstract
The invention discloses a method for maximum production of clean diesel oil by shale oil whole fraction hydrogenation. The method adopts a technology combined hydrofining and hydrocracking. The method comprises the following steps of mixing a whole fraction of shale oil and hydrogen, feeding the mixture into a hydrofining reaction section, carrying out heat exchange cooling of effluence obtained by the hydrofining, feeding the cooled effluence into a separator, carrying out gas-liquid separation, feeding the separated liquid into a product fractionating tower, carrying out cutting to obtain products of naphtha, diesel oil and the like, feeding unconverted oil in the bottom of the product fractionating tower into a hydrocracking reaction section for hydrocracking to obtain hydrocracked effluent, and circulating all the hydrocracked effluent as a hydrofinishing raw material. Compared with the prior art, the method realizes production of clean diesel oil meeting the European V standard by shale oil whole fraction hydrogenation, has a product yield of 85% and can obtain a low-sulfur high-quality naphtha by-product as an ethylene production raw material, and thus providing a beneficial technology approach for shale oil deep processing and alleviating the situation of short supply of petroleum-based diesel oil.
Description
Technical field
The present invention relates to a kind of hydrogenation of shale oil maximum and produce the method for clean diesel.Specifically, be raw material with the full cut of shale oil, produce high-quality light-weight fuel oil through the method for unifining-hydrogen cracking.
Background technology
The world petroleum resource shortage, the technology that makes various non-conventional oil resources processings produce light-weight fuel oil becomes focus, and wherein one of technology is to be producing clean fuel with the shale oil.
Shale oil is that resinous shale is after hot-work; The product that its organic decomposes generates; Similar natural oil; But contain more unsaturated hydro carbons and dredge, non-hydrocarbons organic cpds such as nitrogen, oxygen, and these unsaturated hydro carbons and non-hydrocarbons organic cpds are to cause that the oil product colloid increases, sediment forms and the major cause that causes stability variation, color blackening.So, no matter, still produce other products, all need remove non-hydrocarbon compound with the further processing oil fuel of shale oil, saturation of olefins guarantees quality product.
Hydrotreatment foot oil product carries out the process of catalytic reforming in the presence of catalyzer and hydrogen, through oil product is carried out desulfurization, denitrogenation, deoxidation, alkene is saturated, aromatic hydrocarbons is saturated and demetalization and diasphaltene impurity etc., improves oil quality.The hydrotreatment technology has wide, the advantages such as liquid yield is high, good product quality of the raw material range of processing, is the indispensable a kind of processing means of production high-quality oil product.
Handle the existing report of shale oil recovery light-weight fuel oil with the method for hydrogenation.Introduced the method that a kind of hydrogenation of shale oil is produced diesel oil like US4419218; This method is with conventional method of hydrotreating shale oil to be carried out pre-treatment; The generation oil that obtains carries out cracking without separating all directly as cracking stock with the ZSM-12 sieve catalyst, produces diesel oil.Its shortcoming is that the generation oil of hydrotreatment directly advances cracking unit without separating, and the oxygen nitrogen content is higher in the face shale oil, and this is very big to the influence of cracking catalyst performance, is easy to inactivation, can not the assurance device long-term operation.
US4344840 has introduced the method that a kind of hydrogenation of shale oil is produced rocket(engine)fuel and diesel oil, and this method is with ebullated bed reactor shale oil to be carried out demetalization, handles with the fixed bed hydrogenation treatment unit again, obtains qualified rocket(engine)fuel and diesel oil.Its shortcoming is that the hydrogen consumption is high, process cost is high, construction investment is high, and liquid bed technology is not mature enough.
CN101067089 discloses a kind of working method of shale oil, and this technology is to adopt hydrotreatment and the series connection of hydrogenation catalytic conversion of heavy oil, by shale oil recovery light-weight fuel oil and low-carbon alkene.Its shortcoming is that the residual oil and the coke ratio that produce are more, will inevitably shorten the running period of device.
Summary of the invention
In order to overcome the deficiency of prior art, the invention provides the method that a kind of shale oil hydrogenation of total effluent maximum is produced clean diesel.This method not only can make the production of shale oil hydrogenation of total effluent satisfy the clean diesel of Europe V standard; Product yield can reach 85%; The low-sulfur high-quality petroleum naphtha of by-product can be used as the system ethylene raw simultaneously; Thereby, alleviate the nervous present situation of petroleum base diesel oil supply and demand for the shale oil deep processing provides useful technological approaches.
Hydrogenation of shale oil maximum of the present invention is produced the method for the cleaning diesel oil that disappears; Comprise that full cut of shale oil and hydrogen are mixed into the hydrofining reaction section; Elute after refining gets into separator through the heat exchange cooling and carries out gas-liquid separation; The liquid separated logistics gets into the product separation column, cuts out products such as petroleum naphtha, diesel oil.Unconverted oil entering hydrocracking reaction section is carried out hydrogen cracking at the bottom of the separation column, and the hydrocracking reaction elute of gained all gets into the hydrofining reaction section.
Among the present invention, the shared cover separation system of the reaction effluent of unifining and hydrogen cracking can reduce facility investment like this.Hydrogen-rich gas by the separation system gained can be circulated to hydrocracking reactor as recycle hydrogen after purifying.Sewage is discharged reactive system.
Unconverted oil of the present invention is as the criterion with diesel oil, counts light oil than the component that diesel oil is lighter, and the cut that overweights diesel oil is counted unconverted oil.
Shale oil properties according to the invention (in massfraction): oxygen level is 0.5%～5.0%, and nitrogen content is 1.0%～2.0%, and sulphur content is 0.5%～1.0%, and density (20 ℃) is about 1.0g/cm3, also contains more unsaturated hydrocarbons and colloid.Confirmed hydrogenation combination technique process of the present invention according to the shale oil properties.
Described shale oil hydrogenation of total effluent purification techniques is to remove oxygen carrier and olefin impurities such as alcohol, ketone, fat.The hydrofining reaction section is used for the Deep Hydrotreating of fresh feed and soaking section elute, and the hydrofining reaction section can adopt a reactor drum, preferably includes two tandem reactors.When the hydrofining reaction section adopts two tandem reactors; The first reactor charge high voidage Hydrobon catalyst; The conventional Hydrobon catalyst of second reactor charge; Can only adorn a kind of Hydrobon catalyst or two kinds and multiple Hydrobon catalyst grading loading, its pore volume is 0.2～0.6ml/g, and specific surface area is 100～350m
2/ g.The composition of first reactor drum and the Hydrobon catalyst of second reactor charge can be identical; Be to be active metal component with group vib metal and/or group VIII metal; Be preferably in cobalt, molybdenum, nickel and the tungsten one or more; Carrier is inorganic refractory metal oxide compound, is generally aluminum oxide or siliceous aluminum oxide.Weight with catalyzer is benchmark, and in oxide compound, the content of reactive metal is 10%～40%.First reactor drum is different with the particle size and the shape of the Hydrobon catalyst of second reactor charge; Have different bed voidages: the Hydrobon catalyst of first reactor drum is shapes such as Raschig ring shape, porous spherical, Bird's Nest shape, and bed voidage is 0.45～0.85.When the hydrofining reaction section was used two tandem reactors, the hydrocracking reaction elute can get into first reactor drum, also can get into second reactor drum.
Demetalization, saturated, the aromatic hydrocarbons saturated reaction of alkene mainly take place in first reactor drum of described hydrofining reaction section; A small amount of desulfurization, denitrification reaction take place simultaneously; Therefore the catalyzer that uses has higher active metallic content, and the catalyzer that the guard reactor in the general hydrogenation process uses is protective material, and protectant active metallic content is lower; Temperature of reaction is lower, generally below 200 ℃; The complete saturated reaction of deep desulfuration, denitrogenation and alkene mainly takes place in second reactor drum.
Said hydrogen refining process condition optimization is following: hydrogen dividing potential drop 5～19MPa, and hydrogen to oil volume ratio 500～1500, first temperature of reactor are 200～280 ℃, volume space velocity is 0.5～5.0h
-1, second temperature of reactor is 300～450 ℃, volume space velocity is 0.1～2.0h
-1
Described hydrogen cracking is unconverted oil (last running) hydrogen cracking after the shale oil hydrogenation of total effluent is made with extra care.The hydrogen cracking section can only be adorned a kind of hydrocracking catalyst or two kinds and multiple filling hydrocracking catalyst at different stages; Also can be with Hydrobon catalyst and filling hydrocracking catalyst at different stages; Unconverted oil is carried out deep hydrogenation transform, hydrocracking catalyst can be selected the middle oil type hydrocracking catalyst of commodity for use.Hydrocracking catalyst commonly used is to be active metal component with group vib metal and/or group VIII metal, is preferably in cobalt, aluminium, nickel and the tungsten one or more, and carrier is aluminum oxide or amorphous aluminum silicide, and the cracking component is a molecular sieve.Because oxygen, nitrogen content are than higher in the full cut of shale oil; Oxide compound, the nitride composition more complicated in oil; So hydrocracking catalyst of the present invention is to be the hydrocracking catalyst of carrier with amorphous aluminum silicide and molecular sieve, this catalyzer has again that good naphthenic hydrocarbon selectivity rises ring, isomerization of paraffinic hydrocarbons, the appropriate hydrogen cracking of last running, aromatic hydrocarbons is saturated and heteroatoms removes performance improving the active while.Weight with catalyzer is benchmark, and the content of active metal oxide is 10%～35%, and molecular sieve content is 5%～40%.Its pore volume is 0.3～0.5ml/g, and specific surface area is 100～450m
2/ g.Molecular sieve is generally Modified Zeolite Y, and a kind of or mixture in the modified beta zeolite etc.
The processing condition of said hydrogen cracking are preferably following: hydrogen dividing potential drop 5～19MPa, 300～450 ℃ of temperature of reaction, hydrogen to oil volume ratio 500～1500, volume space velocity 0.2～4.0h during liquid
-1
The catalyzer that uses in the inventive method can be selected the commercial catalyst that suits as required, also can prepare by this area ordinary method.
The present invention has the following advantages:
1. a small amount of desulfurization, denitrification reaction owing to take place in first reactor drum of hydrofining reaction section among the present invention, thereby catalyst activity is higher, and this is just highly beneficial to alkene and aromatic hydrogenation saturated reaction; Under the pyroreaction condition, the sulphur nitrogen impurity that passes through in the saturated aromatic hydrocarbons of hydrogenation is easy to remove, and then has improved desulfurization, denitrification effect, reaches the purpose of deep refining in second reactor drum.
2. the present invention has dysgenic water so the separation system after refining can in time be discharged to hydrocracking catalyst owing to oxygen level in the shale oil is higher, has guaranteed the hydrocracking catalyst long-term operation; The hydrogen cracking elute all circulates as hydrorefined charging; Can improve unifining charging quality on the one hand, reduce refining reaction device green coke, guarantee long-term operation; Another side hydrogen cracking elute is with back purified method; Make the further hydrogenation of polynuclear compound that does not have enough time in the raw material to react saturated, promptly help lighting more, favourable to the quality that improves lightweight oil.
3. the present invention is directed to feed oxygen, characteristics that nitrogen content is high, select anti-nitrogen and water resistance good, the suitable hydrocracking catalyst that contains amorphous aluminum silicide and molecular sieve of cracking performance, guaranteed the long-term operation of device.And can produce the fine clean diesel.
4. present method is directly handled the full cut of shale oil, does not need raw material is carried out like pre-treatment such as cuttings, and the step that simplifies the operation reduces production costs.
5. the present invention does not have the sulphur clean diesel product except obtaining, and goes back by-product part high-quality petroleum naphtha, can be used as the system ethylene raw.Shale oil can be alleviated present oil supply as the raw material of producing clean diesel global anxiety occurs,, the development of following shale oil industry had great potential and application prospect for diesel production provides new method.
Description of drawings
Fig. 1 is a principle process synoptic diagram of the present invention.
Embodiment
As shown in the figure; Shale oil raw material 1 and hydrogen 2 are mixed into first reactor drum 3 of hydrofining reaction section, obtain second reactor drum 5 that unifining generates oily 4 entering hydrofining reaction sections, obtain unifining generation oily 6 and carry out gas-liquid separation through heat exchange cooling entering separator 7; The hydrogen-rich gas 8 that obtains, water 9 and liquid oil 10; Hydrogen-rich gas 8 gets into recycle compressor, can be used as recycle hydrogen and uses water 9 direct extraction systems; Liquid oil 10 gets into product separation column 11, obtains petroleum naphtha 12, diesel oil 13 and unconverted oil 14.Unconverted oil 14 entering hydrocracking reactors 15 carry out hydrogen cracking at the bottom of the separation column, and the hydrocracking reaction elute 16 of gained all gets into hydrofining reaction section first reactor drums 3.
To combine embodiment further to set forth technical scheme of the present invention below.
Embodiment 1～3.
The raw oil character of using among the embodiment is seen table 1.
The full cut character of table 1 shale oil (consisting of the quality percentage composition)
At first full cut of shale oil and hydrogen and hydrocracking reaction elute are mixed into hydrofining reactor; Obtaining unifining generation oil separates; Unconverted oil gets into hydrocracking reactor and carries out hydrogen cracking; The hydrogenation reaction effluent of gained all returns hydrofining reactor as hydrorefined charging, obtains unifining generation oil and carries out fractionation.
The macrobead hydrotreating catalyst R-FF-26 of the first reactor charge Fushun Petrochemical Research Institute of hydrofining reaction section development is shaped as the Raschig ring of diameter 10 * 10mm, and bed voidage is 0.60.The FF-36 hydrotreating catalyst of second reactor charge Fushun Petrochemical Research Institute development and production.The composition of two kinds of catalyzer is identical, is carrier with the aluminum oxide, is active ingredient with Mo-Ni, and its reactive metal counts 30% with oxide weight, the specific surface area>=160m of catalyzer
2/ g, pore volume are 0.35 ± 0.02mL/g.FF-36 catalyzer diameter is 1.2 ± 0.mm, the bar shaped of long 3～8mm, and bed voidage is 0.38.(conventional one section process for refining refers to that two kinds of catalyst loadings are in a reactor drum to adopt conventional one section process for refining A respectively; Operational condition is identical with the present invention's second reactor drum; Volume space velocity is total air speed of two tandem reactors of the refining section of the present invention) compare test, processing condition and correlation data such as table 2 with the refining section B of this technology.
Table 2 processing condition and generation oiliness confrontation ratio-unifining
Annotate: A representes single reactor, and B representes the double-reactor series connection.
Show that by the simultaneous test data use one-stage serial process for refining technology of the present invention, the desulfurization removing nitric effect obviously improves, and has good refining effect.
Table 3 processing condition and the matter-hydrogen cracking of generation oiliness
FC-14 is the hydrocracking catalyst of Fushun Petrochemical Research Institute's development and production.
The whole flow process product property of table 4 and yield-unifining/hydrogen cracking
Can find out that by the embodiment data through hydrogenation combination technique of the present invention, the shale oil hydrogenation of total effluent is converted into the high-quality clean fuel to greatest extent; Especially the clean diesel that can direct production satisfies Europe V standard; Product yield can reach 85%, and the low-sulfur high-quality petroleum naphtha of by-product can be used as the system ethylene raw, can prolong the work-ing life of catalyzer and the runtime of device simultaneously; Improve treatment capacity, reduce plant energy consumption and production cost.
Claims (10)
1. a hydrogenation of shale oil maximum is produced the method for clean diesel; It is characterized in that: full cut of shale oil and hydrogen are mixed into the hydrofining reaction section; Elute after refining gets into separator through the heat exchange cooling and carries out gas-liquid separation, and the liquid separated logistics gets into the product separation column, cuts out petroleum naphtha, diesel product; Unconverted oil entering hydrocracking reaction section is carried out hydrogen cracking at the bottom of the separation column, and the hydrocracking reaction elute of gained all gets into the hydrofining reaction section.
2. according to the described method of claim 1, it is characterized in that: the hydrogen-rich gas by the separation system gained is circulated to hydrocracking reactor as recycle hydrogen after purifying.
3. according to the described method of claim 1, it is characterized in that: the hydrofining reaction section adopts two tandem reactors.
4. according to the described method of claim 3, it is characterized in that: in two tandem reactors of hydrofining reaction section, the first reactor charge high voidage Hydrobon catalyst, the conventional Hydrobon catalyst of second reactor charge.
5. according to the described method of claim 4, it is characterized in that: the Hydrobon catalyst of first reactor drum is Raschig ring shape, porous spherical or Bird's Nest shape, and bed voidage is 0.45～0.85.
6. according to claim 4 or 5 described methods; It is characterized in that: first reactor drum is identical with the composition like the hydrogen catalyst for refining of second reactor charge; Be to be active metal component with group vib metal and/or group VIII metal, carrier is inorganic refractory metal oxide compound, is benchmark with the weight of catalyzer; In oxide compound, the content of reactive metal is 10%～40%.
7. according to the described method of claim 4, it is characterized in that the hydrogen refining process condition is: hydrogen dividing potential drop 5～19MPa, hydrogen to oil volume ratio 500～1500, first temperature of reactor are 200～280 ℃, volume space velocity is 0.5～5.0h
-1, second temperature of reactor is 300～450 ℃, volume space velocity is 0.1～2.0h
-1
8. according to the described method of claim 1, it is characterized in that: hydrocracking catalyst is selected middle oil type hydrocracking catalyst for use.
9. according to claim 1 or 8 described methods; It is characterized in that: hydrocracking catalyst is an active ingredient with in cobalt, molybdenum, nickel and the tungsten one or more; Carrier is aluminum oxide or amorphous aluminum silicide, and the cracking component is a molecular sieve, is benchmark with the weight of catalyzer; The content of active metal oxide is 10%～35%, and molecular sieve content is 5%～40%.
10. according to claim 1 or 8 described methods, it is characterized in that the processing condition of hydrogen cracking are: hydrogen dividing potential drop 5～19MPa, 300～450 ℃ of temperature of reaction, hydrogen to oil volume ratio 500～1500, volume space velocity 0.2～4.0h during liquid
-1
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Cited By (5)
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| CN103497782A (en) * | 2013-10-16 | 2014-01-08 | 黑龙江省能源环境研究院 | Method of producing low-sulfur low freezing point diesel by full-range shale oil |
| CN107983360A (en) * | 2017-11-24 | 2018-05-04 | 抚顺新瑞催化剂有限公司 | Shale oil catalytic Hydrogenation for fuel oil catalyst system and its application method |
| CN114437804A (en) * | 2020-10-19 | 2022-05-06 | 中国石油化工股份有限公司 | Hydrocracking method of high-nitrogen raw oil |
| CN114437798A (en) * | 2020-10-19 | 2022-05-06 | 中国石油化工股份有限公司 | Shale oil hydrocracking method |
| CN114437799A (en) * | 2020-10-19 | 2022-05-06 | 中国石油化工股份有限公司 | Hydrocracking method |
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