CN101724444A - Low-cost hydrogenation process method - Google Patents
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- CN101724444A CN101724444A CN200810228364A CN200810228364A CN101724444A CN 101724444 A CN101724444 A CN 101724444A CN 200810228364 A CN200810228364 A CN 200810228364A CN 200810228364 A CN200810228364 A CN 200810228364A CN 101724444 A CN101724444 A CN 101724444A
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Abstract
The invention discloses a low-cost hydrogenation process method, which comprises the following steps of: mixing base oil with hydrogen; allowing the mixture to pass through a catalyst bed under the condition of a hydrogenation process; and mixing and recycling partial hydrotreating products without setting a hydrogen circulating system, wherein the using amount of the hydrogen is 1 to 10 times that of the hydrogen which is dissolved by a reaction system under the condition of adding a reaction condition based on the chemical hydrogen consumption during the reaction. The low-cost hydrogenation process method is a hydrogenation process of gas, liquid and solid phases with a low hydrogen-oil ratio; due to the low hydrogen-oil ratio, the hydrogen circulating system in the conventional hydrogenation process can be removed to greatly reduce the equipment investment and the operation cost; the reaction can be ensured to perform successfully by properly maintaining a little gas-phase hydrogen; and proper hydrotreating product circulation can ensure that the operation is stably performed for a long-time circle.
Description
Technical field
The present invention relates to a kind of fixed bed three-phase hydrogenation method, this method does not need hydrogen recycle link and circulating hydrogen compressor.
Background technology
The fixed bed hydrogenation technological process normally in order to remove from the sulphur in the raw material of crude oil, nitrogen, oxygen, metal impurities, or reduces the size of raw molecule and the catalytic reaction process that carries out.Hydrogenation technique process itself, because want unsaturated components such as saturated aromatic hydrocarbons, alkene, and the hydrogenation that removes impurity, need to consume a certain amount of hydrogen, be called the chemistry consumption hydrogen of hydrogenation reaction here.Its chemical hydrogen consumption of the hydrogenation technique process of different material is different, can measure by experiment or calculate by experimental formula.It is generally acknowledged that in the hydrogenation technique process, need operate, main purpose is to improve speed of response and avoid catalyst deactivation under the condition of the amounts of hydrogen that consumes far above chemical hydrogen.In the hydrogenation technique, hydrogen usage is generally represented with the volume ratio of hydrogen under the standard state and stock oil, is called for short hydrogen-oil ratio.
When hydrogenation technique adopts bigger hydrogen-oil ratio, after finishing, hydrogenation reaction must have a large amount of hydrogen more than needed.These hydrogen more than needed are common all to mix back continuation as the hydrogen feed of reacting with new hydrogen by hydrogen cycle process after the circulating hydrogen compressor supercharging.
In the hydrogenation technique device, the investment of hydrogen recycle link accounts for the significant proportion of whole process cost.If the hydrogen flowing quantity in the hydrotreatment process can be reduced and saves hydrogen gas circulating system and circulating hydrogen compressor, can reduce the investment and the process cost of hydrogenation technique device greatly, and then reduce the cost of product, improve the market competitiveness of enterprise.
Chinese patent CN86108622 discloses a kind of hydrofining technology of reformed oil, and hydrogen to oil volume ratio is 200-1000: 1; Chinese patent CN93101935.4 discloses a kind of inferior feedstock oil a period of hydrocracking processing method, hydrogen to oil volume ratio 1300-1500: 1; Chinese patent CN94102955.7 discloses a kind of Rifining method for catalylic cracking gasoline by adding hydrogen, volume of hydrogen oil ratio 150-500: 1; Chinese patent CN96109792.2 discloses a kind of method of serial hydrogenation explained hereafter high-quality vaseline, hydrogen to oil volume ratio 300-1400: 1; Chinese patent CN96120125.8 discloses a kind of method of producing white oil by the direct hydrogenation of cycloalkyl straight run, hydrogen to oil volume ratio 500-1500: 1.The characteristics of these patents are to have higher hydrogen-oil ratio, therefore must hydrogen recycle link and circulating hydrogen compressor.
Summary of the invention
At the deficiencies in the prior art, the invention provides a kind of hydrogenation method that need not use the hydrogen recycle link, reduce the cost of investment and the process cost of hydrogenation technique.
Low-cost hydrogenation processing method process of the present invention is as follows, stock oil mixes with hydrogen, process beds under the hydrogenation technique condition, partial hydrogenation product and stock oil mixed cycle are used, hydrogen gas circulating system is not set, hydrogen usage is to increase 1～10 times of reactive system dissolved hydrogen amount under the reaction conditions on reaction process chemistry hydrogen consumption basis, preferably increases 1～5 times of dissolved hydrogen amount.
In the inventive method, technology contents such as concrete hydrogenation technique condition and selection of catalysts can be determined according to the conventional knowledge in this area according to feedstock property and quality product requirement.The dissolved hydrogen amount can measuring under the chemical hydrogen consumption of reaction process and the reaction conditions, can calculate according to the experimental formula that this area document provides, can estimate that also above-mentioned experimental formula and empirical value can be with reference to " hydroprocessing technique and engineering " book associated visceras of Sinopec press publication in 2004 according to the empirical value that this area document provides.Determination of test method chemistry hydrogen consumption and reactive system dissolved hydrogen amount are technological methods well known to those skilled in the art, as on testing apparatus, adopt the condition identical, when reaching suitable reaction result, measure chemical hydrogen consumption and system dissolves hydrogen amount with reaction process.
In the inventive method, the circulation of partial hydrogenation product mixes with reaction raw materials, with the quiet run of assurance hydrogenation reaction and the work-ing life of catalyzer, internal circulating load can be determined according to the particular case of reactive system, suitably add big cycle volume when for example exothermic heat of reaction is big, reactive chemistry hydrogen consumes and suitably adds big cycle volume etc. when high, in general the ratio of by volume internal circulating load and raw material oil mass is 0.1: 1～20: 1, be preferably 0.5: 1～5: 1, in general internal circulating load is favourable to reaction process greatly, but can cause unfavorable results such as power consumption increase, comprehensively various factors is finally determined.The hydrogenation products that recycles can directly recycle, and also can use through recirculation after the fractionating system.
In the inventive method,, the recycle hydrogen system need be set, can save hydrogen recycle link necessary in the conventional hydrotreatment process and circulating hydrogen compressor etc. though the amounts of hydrogen of using is excessive less a little more than the chemical hydrogen consumption of reaction.
In the inventive method, the raw material that the hydrogenation technique process is used can comprise gasoline, kerosene, diesel oil, VGO (vacuum distillate), CGO (wax tailings), LCO (catalytic cracking light cycle oil), residual oil, deasphalted oil, lubricated wet goods.According to the requirement of purpose product, hydrogenation technique can comprise hydrofining, hydrotreatment, hydro-upgrading, hydrocracking etc.
In the hydrogenation process of the present invention, because therefore the amounts of hydrogen of using, does not need hydrogen gas circulating system far below the hydrogen usage of prior art.
In the inventive method, other hydrogenation conditions can determine that by this area general knowledge in general, temperature of reaction is 150～450 ℃ according to raw material properties, quality product requirement etc., and reaction pressure is 1～17MPa, and volume space velocity is 0.5～10h during liquid
-1
In the hydrogenation process of the present invention, the amounts of hydrogen of use is for increasing the dissolved hydrogen amount of the system that is slightly more than on chemical hydrogen consumption basis, and this scheme can guarantee that slightly a small amount of gas phase hydrogen exists in the reactive system, guarantees that reactive system is in the gas, liquid, solid three-phase state.In the hydrogenation process of condition of the present invention, the required hydrogen of hydrogenation reaction is mainly derived from the hydrogen that is dissolved in the stock oil.Along with the carrying out of reaction, the hydrogen that is dissolved in the liquid phase constantly consumes, and the hydrogen in the gas phase constantly dissolves in the liquid phase, keeps having of gas phase hydrogen to be beneficial to the quantity that guarantees dissolved hydrogen in the liquid phase.In general hydrogenation process be to eliminate the process of raw material Semi-polarity material, since the polarity of hydrogen molecule a little less than, rule according to " similar mixing ", if be dissolved under the state that the hydrogen in the liquid phase do not reach capacity, the hydrogen that is dissolved in the stock oil is adsorbed on around the molecule of low-pole more, the hydrogen that needs hydrogen to carry out around the polar molecule of hydrogenation reaction is then less relatively, be adsorbed on low-pole molecule hydrogen on every side and also be not easy to be diffused into around the stronger molecule of polarity, so this state has influenced carrying out smoothly of hydrogenation reaction.Under the inventive method state, owing to there is gas phase hydrogen, when the hydrogen around the stronger molecule of polarity consumed along with the carrying out of reaction, the hydrogen in the gas phase can in time replenish into, and then guaranteed carrying out smoothly of hydrogenation reaction.In the tradition hydrogenation reaction, it is generally acknowledged that excessive hydrogen helps keeping activity of such catalysts stability far away, in the inventive method, though greatly reduce the reactive hydrogen oil ratio, the amounts of hydrogen of using is only slightly high than chemical hydrogen consumption, but because recycling of hydrogenation products still can keep activity of such catalysts stability.
Description of drawings
Fig. 1 is a processing method schematic flow sheet of the present invention.
The 1st, fresh feed, the 2nd, feedstock pump, the 3rd, fresh hydrogen, the 4th, turning oil, the 5th, parallel feeding comprises fresh feed, turning oil and new hydrogen, the 6th, hydrotreating reactor, the 7th, separator, the 8th, variable valve, the 9th, liquid product, the 10th, turning oil, the 11st, not fractionated product, the 12nd, separation column, the 13rd, final light-end products, the 14th, final heavy product.
Embodiment
Characteristics of the present invention are to reduce hydrogen-oil ratio greatly in fixed bed three-phase hydrotreatment process, thus necessary hydrogen recycle link and circulating hydrogen compressor in can the present conventional hydrotreatment process of cancellation.
Fixed bed three-phase hydrotreatment process of the present invention, material enters from reactor top, after the beds in the reactor of flowing through carries out the hydrotreatment reaction, discharges through the outlet of reactor lower part.
For ease of further specifying clear hydrogenation technique process of the present invention, here process of the present invention is described.As shown in Figure 1, fresh feed 1 mixes the back with fresh hydrogen 3 and turning oil 4 and forms logistics 5 after fresh feed pump 2 pressurizations, enter the reactor 6 that is filled with required hydrogenation catalyst then, enters separator 7 after the reaction.In separator 7, have a small amount of more than needed hydrogen and a large amount of impurity such as hydrogen sulfide, ammonia, lower carbon number hydrocarbons is emitted system through variable valve 8, liquid product is divided into the two-way logistics through exporting 9, and one the tunnel is that logistics 11, a tunnel as the finished product is as round-robin logistics 10.Logistics 10 loops back reactor upstream 4 and mixes with fresh feed.Logistics 11 enters separation column 12 as the finished product, is light product 13, heavy product 14 according to the fractionation of production purpose, and in fact, can be by the difference of reaction process and the different multiple products that fractionate out of product requirement.
Gasoline stocks is 230 ℃ of following hydrofining desulfurization, and catalyzer is the FDS-4A catalyzer of Fushun Petrochemical Research Institute's development and production.The chemical hydrogen consumption and the system dissolves hydrogen amount of elder generation's test determination reaction are carried out the inventive method process then.Reaction pressure is 3.0MPa, and volume space velocity is 4h during reaction raw materials fluid
-1Hydrogen to oil volume ratio adds 2 times of system dissolves hydrogen amount, circulation ratio (turning oil volume: the fresh feed volume) be 2: 1 by the reactive chemistry hydrogen-consuming volume.Reaction result is a desulfurization degree 99.7%, and is suitable substantially with the reaction effect that has now under the high hydrogen-oil ratio operational condition, and catalyst activity stability is suitable down with usual terms.
Comparative example 1
According to the operational condition of embodiment 1, the amounts of hydrogen that only is to use is the dissolved hydrogen amount of reactive system, and the reaction result desulfurization degree is 78.9%.
Comparative example 2
According to the operational condition of embodiment 1, the amounts of hydrogen that only is to use is the chemical hydrogen consumption of this reaction process, and the reaction result desulfurization degree is 90.3%.
Comparative example 3
According to the operational condition of embodiment 1, the amounts of hydrogen that only is to use is the popular response hydrogen to oil volume ratio, and promptly hydrogen to oil volume ratio is 400: 1, and excessive hydrogen uses the recycle hydrogen system, no hydrogenated products working cycle, and the reaction result desulfurization degree is 99.6%.
The boat coal is 290 ℃ of following hydrofining desulfurization, and catalyzer is the FH-40A catalyzer of Fushun Petrochemical Research Institute's development and production.The chemical hydrogen consumption and the system dissolves hydrogen amount of elder generation's test determination reaction are carried out the inventive method process then.Reaction pressure is 4.0MPa, and volume space velocity is 2h during reaction raw materials fluid
-1Hydrogen to oil volume ratio adds 1.5 times of system dissolves hydrogen amount, circulation ratio (turning oil volume: the fresh feed volume) be 0.3: 1 by the reactive chemistry hydrogen-consuming volume.Reaction result is a desulfurization degree 99.5%, and is suitable substantially with the reaction effect that has now under the high hydrogen-oil ratio operational condition, and catalyst activity stability is suitable down with usual terms.
With desulfurization and denitrogenation, catalyzer is the FHDS-6 catalyzer of Fushun Petrochemical Research Institute's development and production to diesel raw material 350 ℃ of following hydrofinings.The chemical hydrogen consumption and the system dissolves hydrogen amount of elder generation's test determination reaction are carried out the inventive method process then.Reaction pressure is 4.0MPa, and volume space velocity is 1.9h during reaction raw materials fluid
-1Hydrogen to oil volume ratio adds 0.8 times of system dissolves hydrogen amount, circulation ratio (turning oil volume: the fresh feed volume) be 2: 1 by the reactive chemistry hydrogen-consuming volume.Reaction result is a desulfurization degree 99.9%, and denitrification percent is 99.6%, and is suitable substantially with the reaction effect that has now under the high hydrogen-oil ratio operational condition, and catalyst activity stability is suitable down with usual terms.
Embodiment 4
With denitrogenation, catalyzer is 3996 catalyzer of Fushun Petrochemical Research Institute's development and production to vacuum gas oil VGO 379 ℃ of following hydrotreatments.The chemical hydrogen consumption and the system dissolves hydrogen amount of elder generation's test determination reaction are carried out the inventive method process then.Reaction pressure is 14.7MPa, and volume space velocity is 1h during reaction raw materials fluid
-1Hydrogen to oil volume ratio adds 3 times of system dissolves hydrogen amount, circulation ratio (turning oil volume: the fresh feed volume) be 3: 1 by the reactive chemistry hydrogen-consuming volume.Reaction result is a denitrification percent 99.4%, and is suitable substantially with the reaction effect that has now under the high hydrogen-oil ratio operational condition, and catalyst activity stability is suitable down with usual terms.
To remove sulphur and nitrogen, catalyzer is 3926 catalyzer of Fushun Petrochemical Research Institute's development and production to wax tailings CGO 398 ℃ of following hydrotreatments.The chemical hydrogen consumption and the system dissolves hydrogen amount of elder generation's test determination reaction are carried out the inventive method process then.Reaction pressure is 7.5MPa, and volume space velocity is 0.8h during reaction raw materials fluid
-1Hydrogen to oil volume ratio adds 2.3 times of system dissolves hydrogen amount, circulation ratio (turning oil volume: the fresh feed volume) be 5: 1 by the reactive chemistry hydrogen-consuming volume.Reaction result is a desulfurization degree 98.9%, and denitrification percent is 64.7%, and is suitable substantially with the reaction effect that has now under the high hydrogen-oil ratio operational condition, and catalyst activity stability is suitable down with usual terms.
To remove sulphur and nitrogen, catalyzer is the FHDS-6 catalyzer of Fushun Petrochemical Research Institute's development and production to catalytic cracking light cycle oil LCO 370 ℃ of following hydrofinings.The chemical hydrogen consumption and the system dissolves hydrogen amount of elder generation's test determination reaction are carried out the inventive method process then.Reaction pressure is 8.0MPa, and volume space velocity is 1.8h during reaction raw materials fluid
-1Hydrogen to oil volume ratio adds 2 times of system dissolves hydrogen amount, circulation ratio (turning oil volume: the fresh feed volume) be 1.9: 1 by the reactive chemistry hydrogen-consuming volume.Reaction result is a desulfurization degree 99.9%, and denitrification percent is 99.3%, and is suitable substantially with the reaction effect that has now under the high hydrogen-oil ratio operational condition, and catalyst activity stability is suitable down with usual terms.
Residual oil raw material is at 380 ℃ of following hydrogenation, and catalyzer is the FZC catalyst series of Fushun Petrochemical Research Institute's development and production.The chemical hydrogen consumption and the system dissolves hydrogen amount of elder generation's test determination reaction are carried out the inventive method process then.Reaction pressure is 15.65MPa, and volume space velocity is 0.2h during reaction raw materials fluid
-1Hydrogen to oil volume ratio adds 2 times of system dissolves hydrogen amount, circulation ratio (turning oil volume: the fresh feed volume) be 1: 1 by the reactive chemistry hydrogen-consuming volume.Reaction result is a desulfurization degree 87.1%, and denitrification percent 38.0% takes off carbon yield 55.3%, and total decreasing ratio of metallic nickel and vanadium is 69.1%, and is suitable substantially with the reaction effect that has now under the high hydrogen-oil ratio operational condition, and catalyst activity stability is suitable down with usual terms.
Embodiment 8
Deasphalted oil is at 385 ℃ of following hydrogenation, and catalyzer is the FZC catalyst series of Fushun Petrochemical Research Institute's development and production.The chemical hydrogen consumption and the system dissolves hydrogen amount of elder generation's test determination reaction are carried out the inventive method process then.Reaction pressure is 15.7MPa, and volume space velocity is 0.22h during reaction raw materials fluid
-1Hydrogen to oil volume ratio adds 3 times of system dissolves hydrogen amount, circulation ratio (turning oil volume: the fresh feed volume) be 3: 1 by the reactive chemistry hydrogen-consuming volume.Reaction result is a desulfurization degree 88.0%, and denitrification percent 65.4% takes off carbon yield 66.6%, and total decreasing ratio of metallic nickel and vanadium is 80.2%, and is suitable substantially with the reaction effect that has now under the high hydrogen-oil ratio operational condition, and catalyst activity stability is suitable down with usual terms.
Lube stock is at 280 ℃ of following hydrogenation, and catalyzer is the FV-10 catalyzer of Fushun Petrochemical Research Institute's development and production.The chemical hydrogen consumption and the system dissolves hydrogen amount of elder generation's test determination reaction are carried out the inventive method process then.Reaction pressure is 14.0MPa, and volume space velocity is 0.4h during reaction raw materials fluid
-1Hydrogen to oil volume ratio adds 2.5 times of system dissolves hydrogen amount, circulation ratio (turning oil volume: the fresh feed volume) be 3: 1 by the reactive chemistry hydrogen-consuming volume.Reaction result is product viscosity (40 ℃) 56.8mm
2/ s, 187 ℃ of flash-points (opening), color (Sai Shi number)+30, suitable substantially with the reaction effect that has now under the high hydrogen-oil ratio operational condition, catalyst activity stability is suitable down with usual terms.
Claims (8)
1. low-cost hydrogenation processing method, stock oil mixes with hydrogen, process beds under the hydrogenation technique condition, it is characterized in that: partial hydrogenation product and stock oil mixed cycle are used, hydrogen gas circulating system is not set, and hydrogen usage is to increase 1～10 times of reactive system dissolved hydrogen amount under the reaction conditions on reaction process chemistry hydrogen consumption basis.
2. in accordance with the method for claim 1, it is characterized in that hydrogen usage is to increase 1～5 times of reactive system dissolved hydrogen amount under the reaction conditions on reaction process chemistry hydrogen consumption basis.
3. in accordance with the method for claim 1, it is characterized in that the hydrogenation products by volume that recycles and the ratio of raw material oil mass are 0.1: 1～20: 1.
4. in accordance with the method for claim 3, it is characterized in that described internal circulating load ratio is 0.5: 1～5: 1.
5. in accordance with the method for claim 1, it is characterized in that the described hydrogenation products that recycles directly recycles, perhaps use through recirculation after the fractionating system.
6. in accordance with the method for claim 1, it is characterized in that described stock oil comprises gasoline, kerosene, diesel oil, vacuum distillate, wax tailings, catalytic cracking light cycle oil, residual oil, deasphalted oil or lubricating oil.
7. in accordance with the method for claim 1, it is characterized in that described hydrogenation conditions is: temperature of reaction is 150～450 ℃, and reaction pressure is 1～17MPa, and volume space velocity is 0.5～10h during liquid
-1
8. in accordance with the method for claim 1, it is characterized in that described hydrogenation technique comprises hydrofining, hydrotreatment, hydro-upgrading or hydrocracking.
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Cited By (4)
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| CN102465016A (en) * | 2010-11-05 | 2012-05-23 | 中国石油化工股份有限公司 | Combined hydrogenation process |
| CN102465019A (en) * | 2010-11-05 | 2012-05-23 | 中国石油化工股份有限公司 | Low-pressure combined hydrogenation technological method |
| WO2014044195A1 (en) * | 2012-09-21 | 2014-03-27 | 中国石油化工股份有限公司 | Reformate hydrotreatment method |
| US9862896B2 (en) | 2012-09-21 | 2018-01-09 | China Petroleum & Chemical Corporation | Hydrocarbon oil hydrotreating method |
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| CN101089134A (en) * | 2006-06-16 | 2007-12-19 | 中国石油化工股份有限公司 | Aviation kerosene fraction hydroupgrading process |
| CN101194001A (en) * | 2005-03-24 | 2008-06-04 | 过程动力学公司 | Control system method and apparatus for continuous liquid phase hydroprocessing |
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| US3870626A (en) * | 1973-02-27 | 1975-03-11 | Gulf Research Development Co | Method for reducing the mercaptan content of a middle distillate oil |
| CN1229838A (en) * | 1998-03-20 | 1999-09-29 | 中国石油化工集团公司 | Conversion process of hydrocarbon oil |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102465016A (en) * | 2010-11-05 | 2012-05-23 | 中国石油化工股份有限公司 | Combined hydrogenation process |
| CN102465019A (en) * | 2010-11-05 | 2012-05-23 | 中国石油化工股份有限公司 | Low-pressure combined hydrogenation technological method |
| CN102465019B (en) * | 2010-11-05 | 2014-08-20 | 中国石油化工股份有限公司 | Low-pressure combined hydrogenation technological method |
| CN102465016B (en) * | 2010-11-05 | 2014-08-20 | 中国石油化工股份有限公司 | Combined hydrogenation process |
| WO2014044195A1 (en) * | 2012-09-21 | 2014-03-27 | 中国石油化工股份有限公司 | Reformate hydrotreatment method |
| RU2609780C2 (en) * | 2012-09-21 | 2017-02-03 | Чайна Петролиум Энд Кемикл Корпорейшн | Reformate hydrotreatment method and apparatus |
| US9862896B2 (en) | 2012-09-21 | 2018-01-09 | China Petroleum & Chemical Corporation | Hydrocarbon oil hydrotreating method |
| US9879186B2 (en) | 2012-09-21 | 2018-01-30 | China Petroleum & Chemical Corporation | Reformate hydrotreatment method |
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Application publication date: 20100609 |