CN101787305B - Method of liquid phase circulation hydrotreatment and reaction system - Google Patents
Method of liquid phase circulation hydrotreatment and reaction system Download PDFInfo
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Abstract
The invention discloses a method of liquid phase circulation hydrotreatment. A part of liquid product after hydrotreatment circulates and is mixed with raw material to form liquid phase material, the hydrogen is mixed in the liquid phase material, the mixing volume of the hydrogen is increased by below 20 times of the dissolved hydrogen volume of a reaction system under the reaction condition based on the chemical hydrogen consumption in the reaction process, the liquid phase material mixed with the hydrogen enters the upper part of a reactor, the upper part of the reactor is provided with a gas phase space and an exhaust system which is communicated with the gas phase space, the pressure and the liquid level in the reactor are controlled by controlling the displacement of the exhaust system, the liquid phase material dissolved with the hydrogen enters a hydrogenation catalyst bed at the lower part of the reactor for hydrotreatment reaction, a part of the liquid phase reaction product is discharged from the reaction system, and the other part circulates and is mixed with the raw material. The method can ensure good reaction effect and leads the liquid phase circulation hydrotreatment to be stably controlled and operated.
Description
Technical field
The present invention relates to a kind of method of liquid phase circulation hydrotreatment and reactive system, particularly increase dissolved hydrogen by the liquid product circulation and carry out liquid-phase hydrogenatin treatment process and reactive system.
Background technology
The Powelery Solids Emission that sulphur content in the reduction diesel oil and aromaticity content can reduce exhaust gas from diesel vehicle reduces topsoil.China's solar oil specification standards are namely carried out with reference to EUROIII Emission Standard and are namely required sulphur namely to require sulphur less than 50 μ g/g less than 350 μ g/g and the execution of Europe IV standard.Be the production of reply New emission standard diesel oil, need on the one hand to solve a gordian technique difficult problem that newly-built hydrogenation unit carries out deep hydrodesulfurizationof of diesel oil, improves cetane value, improves oil quality; Need to carry out comprehensive conceptual design for the enterprise practical situation on the one hand in addition, implement risk and overlapping investment and obtain preferably economic benefit to reduce.At present Petrochemical Enterprises diesel quality upgrading mostly faces diesel oil hydrogenation scarce capacity, hydrogen resource not and the problems such as the hydrogenation degree of depth is unreasonable, and in the situation that the ultra-low-sulphur diesel production technology is updated, enterprise more and more tends to adopt modification scheme.Modification scheme is normally considered from following several respects: increase reactor volume (raising loaded catalyst); Select active better catalyzer; Improve hydrocarbon occurrence and hydrogen cleaning in the reactor; Develop new Technology etc.
In the fixed bed hydrogenation technological process of routine, in order to remove sulphur, nitrogen, oxygen, the metal impurities in the raw material or to reduce the size of feedstock, need to carry out catalytic hydrogenation reaction.For the temperature of reaction of controlling beds with avoid the catalyst carbon deposit inactivation, usually adopt larger hydrogen to oil volume ratio, after finishing, hydrogenation reaction must have a large amount of hydrogen more than needed.These hydrogen more than needed mix the hydrogen feed that continues as reaction with new hydrogen usually after the circulating hydrogen compressor supercharging.This technological process also can be defined as gas phase circulation hydrogenation technique.The ratio that the investment of this technological cycle hydrogen compressor accounts for whole hydrogenation unit cost is higher, hydrogen heat-exchange system energy consumption is larger, if the hydrogen flowing quantity in the hydrotreatment process can be reduced and saves hydrogen gas circulating system and circulating hydrogen compressor, can be for enterprise reduces investment outlay, for Clean Fuel Production reduces cost.
Chinese patent CN86108622 discloses a kind of hydrofining technology of reformed oil, and hydrogen to oil volume ratio is 200: 1-1000: 1; Chinese patent CN93101935.4 discloses a kind of inferior feedstock oil a period of hydrocracking processing method, hydrogen to oil volume ratio 1300: 1-1500: 1; Chinese patent CN94102955.7 discloses a kind of Rifining method for catalylic cracking gasoline by adding hydrogen, volume of hydrogen oil ratio 150: 1-500: 1; Chinese patent CN96109792.2 discloses a kind of method of serial hydrogenation explained hereafter high-quality vaseline, hydrogen to oil volume ratio 300: 1-1400: 1; Chinese patent CN96120125.8 discloses a kind of method of producing white oil by cycloalkyl straight run direct hydrogenation, hydrogen to oil volume ratio 500: 1-1500: 1.The characteristics of these patents are to have higher hydrogen-oil ratio, therefore must hydrogen recycle link and circulating hydrogen compressor.
US Patent No. 6213835, US6428686 etc. disclose a kind of hydrogenation technique of in advance molten hydrogen, by amount of liquid or the air pressure in the amounts of hydrogen control reactor in the control liquid feeding.But it does not solve the H that will produce fully in the hydrofining reaction process
2S, NH
3Deng the problem that detrimental impurity removes, cause it constantly in reactor, to accumulate, greatly reduce reaction efficiency, also can't effectively process sulphur, raw material that nitrogen content is higher.In addition, the reactive system of liquid phase circulation hydrogenation technique and control method are significant to the stable operation of liquid phase circulation hydrogenation.In the disclosed liquid-phase hydrogenatin reactive system of CN200680018017.3, adopt pressure and liquid level in the amount control reactor that mixes hydrogen in the liquid phase, its deficiency is in control process, the amounts of hydrogen that may occur replenishing is less than the situation of reacting required amounts of hydrogen, when more such as the small molecule hydrocarbon that produces under the abnormal condition, liquid level descends in the reactor, this moment, the reaction of Controlling System was the mixed hydrogen amount that reduces in the liquid phase feed, if reduce too much, then amounts of hydrogen may be not enough to keep normal hydrogenation reaction, to the stable disadvantageous effect of bringing of reaction.
Summary of the invention
For the deficiencies in the prior art, the invention provides a kind of method of liquid phase circulation hydrotreatment and reactive system, adopt suitable process form and reactive system, so that the liquid phase circulation hydrotreatment can be stablized control and operation, and obtain desirable reaction effect.
Method of liquid phase circulation hydrotreatment of the present invention comprises following content: the part circulation through the liquid product of hydrotreatment is mixed into liquid phase material with raw material, hydrogen is sneaked into liquid phase material, the hydrogen mixed volume is by increasing below 20 times of reactive system dissolved hydrogen amount under the reaction conditions on reaction process chemical hydrogen consumption amount basis, be preferably 1~10 times, the liquid phase material that has mixed hydrogen enters reactor top, reactor top arranges a gas-phase space, the exhaust system that communicates with this gas-phase space is set, by pressure and the liquid level in the free air delivery control reactor of control exhaust system, the hydrogenation catalyst bed that the liquid phase material that has dissolved hydrogen enters reactor lower part carries out the hydrotreatment reaction, liquid-phase reaction product is partly discharged reactive system, and the part circulation mixes with raw material.
In the method for liquid phase circulation hydrotreatment of the present invention, the pressure in the reactor and the control mode of tank level control system are: when reactor pressure rising or liquid level decline, increase the free air delivery of reactor; When reactor pressure reduction or liquid level rising, reduce the free air delivery of reactor.Liquid level control in the reactor can also adopt the lifting rate of reactor to control, and perhaps adopts free air delivery and lifting rate to control simultaneously.
In the method for liquid phase circulation hydrotreatment of the present invention, the liquid product of circulation and the volume ratio of raw material (recycle ratio) are 0.1: 1~20: 1, are preferably 0.5: 1~5: 1.
In the method for liquid phase circulation hydrotreatment of the present invention, the reactor lower part beds uses suitable hydrogenation catalyst according to reaction needed, such as Hydrobon catalyst, catalyst for hydro-upgrading, hydrotreating catalyst, hydrocracking catalyst etc., various catalyzer can be selected commercial catalyst, also can prepare according to prior art.
In the method for liquid phase circulation hydrotreatment of the present invention, liquid phase material can require specifically to be determined by those skilled in the art according to feedstock property, quality product by the reaction conditions of beds, be generally: temperature of reaction is 150~450 ℃, reaction pressure is 1~17MPa, and volume space velocity is 0.5~15h during liquid
-1
In the method for liquid phase circulation hydrotreatment of the present invention, can as required two or more reactors in series (effluent of a reactor enters next reactor) or (material enters respectively different reactors) in parallel be used.
In the method for liquid phase circulation hydrotreatment of the present invention, at least one air lift tower tray is set in the gas-phase space on reactor top, pass into hydrogen below the air lift tower tray, hydrogen and liquid phase material contact air lift at the air lift tower tray and go out hydrogen sulfide and ammonia in the liquid phase material, hydrogen further is dissolved in the liquid phase material simultaneously, the beds that liquid phase material after the air lift enters reactor lower part carries out the hydrotreatment reaction, and the gas that contains hydrogen sulfide and ammonia after the air lift is discharged reactor from reactor head.
The air lift tower tray on reactor top can arrange 1~8, is preferably 2~5.The air lift tower tray can be various suitable structures, and such as bubble-cap type tower tray, float-valve type tower tray, sieve-board type tower tray etc., the concrete structure of tower tray is well known to those skilled in the art.The hydrogen that air lift is used is introduced reactor from the following optional position of a bottom tower tray, air lift with the amount of hydrogen by gas-liquid volume ratio count 0.1: 1~50: 1, be preferably 1: 1~20: 1.
Liquid phase circulation hydrotreatment reactive system of the present invention comprises reactor, reactor top arranges a gas-phase space, exhaust system is set to communicate with reactor upper gaseous phase space, reactor lower part is the hydrogenation catalyst bed, reactor arranges pressure monitor system and level monitoring system, pressure and the liquid level of the free air delivery control reactor of logical control exhaust system.
In the liquid phase circulation hydrotreatment reactive system of the present invention, can also adopt simultaneously control to discharge the interior liquid level of amount of liquid control reactor of reactor.
In the liquid phase circulation hydrotreatment reactive system of the present invention, at least one air lift tower tray is set preferably in the reactor upper gaseous phase space, the equipment that passes into hydrogen is set below the air lift tower tray.
In the method for liquid phase circulation hydrotreatment of the present invention, the amounts of hydrogen of using is for increasing the dissolved hydrogen amount of the system that is slightly more than on chemical hydrogen consumption amount basis, reactive moieties does not arrange hydrogen gas circulating system, relying on a large amount of circulation times of liquid-phase product to carry into the dissolved hydrogen of reactive system provides fresh feed to carry out the needed hydrogen of hydrogenation reaction, because recycling of hydrogenation products still can keep the activity stability of catalyzer.Its advantage is to eliminate H in the wetting Effects of Factors of catalyzer and the recycle hydrogen
2S and NH
3Impact; Because the specific heat capacity of turning oil is large, thereby greatly reduce the temperature rise of reactor, improve the utilising efficiency of catalyzer, and can reduce the side reaction such as cracking.
Method of liquid phase circulation hydrotreatment of the present invention adopts suitable flow process and red-tape operati mode; require to determine suitable mixed hydrogen amount according to feedstock property and reaction; pressure and liquid level by control free air delivery control reactor; the mixed hydrogen amount in the liquid phase material that guaranteed enough is used for follow-up hydrogenation reaction; the situation that the amounts of hydrogen deficiency can not occur can protect the stable of hydrogenation reaction to carry out.
In the method for liquid phase circulation hydrotreatment of the present invention, by adopting suitable structure of reactor and reactive system, effectively reduced in the hydrogenation products impurity such as hydrogen sulfide and ammonia to the disadvantageous effect of hydrogenation reaction, greatly improved the carrying out of catalyzed reaction, while can adapt to the processing treatment of various high impurity content raw materials, has improved the adaptability of technological process.
Description of drawings
Fig. 1 is processing method schematic flow sheet of the present invention.
Wherein: the 1-hydrogen make-up, the 2-compressor, the 3-feedstock pump, the 4-recycle pump, the 5-reactor, the 6-high score, 7-hydrogen, the 8-product, 9-discharges gas.
Fig. 2 is another schematic flow sheet of processing method of the present invention.
Wherein: the 1-hydrogen make-up, the 2-compressor, the 3-feedstock pump, the 4-recycle pump, the 5-reactor, the 6-high score, 7-hydrogen, the 8-product, 9-discharges gas, 10-reactor top discharging gas.
Embodiment
In the processing method of the present invention, according to processing condition, determine to sneak into the amounts of hydrogen in the raw material, amounts of hydrogen is higher than the reaction hydrogen-consuming volume, set suitable parameter by processing requirement, control amount of liquid (being liquid level) and pressure in the reactor by control reactor free air delivery and lifting rate.
A kind of detailed process of the present invention is as follows, stock oil and quantitative hydrogen under the hydrogenation technique condition through beds, partial hydrogenation product and stock oil mixed cycle are used, hydrogen gas circulating system is not set, hydrogen usage is higher than the reaction hydrogen-consuming volume, be controlled to be a certain amount ofly by reaction requirements, be generally 1~10 times of under reaction process chemical hydrogen consumption amount basis increase reaction conditions reactive system dissolved hydrogen amount.On reactor top or reactor rear portion control free air delivery and lifting rate control amount of liquid and pressure in the reactor.
In the inventive method, the technology contents such as selection of concrete hydrogenation technique condition and catalyzer can according to feedstock property and quality product requirement, be determined according to the conventional knowledge in this area.The dissolved hydrogen amount can measuring under the chemical hydrogen consumption amount of reaction process and the reaction conditions, can calculate according to the experimental formula that this area document provides, can estimate according to the empirical value that this area document provides 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.Determination of test method chemical hydrogen consumption amount 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 with reaction process, when reaching suitable reaction result, measure chemical hydrogen consumption amount and system dissolves hydrogen amount.
In the inventive method, the partial hydrogenation product circulation 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 larger, reactive chemistry hydrogen consumes and suitably adds big cycle volume etc. when high, in general the ratio of internal circulating load and raw material oil mass is 0.1: 1~20: 1 by volume, be preferably 0.5: 1~5: 1, in general internal circulating load is favourable to reaction process greatly, but can cause the unfavorable results such as power consumption increase, comprehensively various factors is finally determined.The hydrogenation products that recycles can use by direct circulation, also can use through recirculation after the fractionating system.
In the inventive method, although the amounts of hydrogen of using is excessive less a little more than the chemical hydrogen consumption amount of reaction, the recycle hydrogen system need be set, can save hydrogen recycle link necessary in the conventional hydrotreatment process and circulating hydrogen compressor etc.
In the inventive method, the raw material that hydrogenation process uses 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 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 0.5~15h during liquid
-1
In the hydrogenation process of the present invention, the amounts of hydrogen of using is for increasing the dissolved hydrogen amount of the system that is slightly more than on chemical hydrogen consumption amount basis, reactive moieties does not arrange hydrogen gas circulating system, relying on a large amount of circulation times of liquid-phase product to carry into the dissolved hydrogen of reactive system provides fresh feed to carry out the needed hydrogen of hydrogenation reaction, because recycling of hydrogenation products still can keep the activity stability of catalyzer.Reactor adopts close structural response device with trickle-bed reactor, controls amount of liquid and pressure in the reactor by controlling reactor free air delivery and lifting rate.Its advantage is to eliminate H in the wetting Effects of Factors of catalyzer and the recycle hydrogen
2S and NH
3Impact; Because the specific heat capacity of turning oil is large, thereby greatly reduce the temperature rise of reactor, improve the utilising efficiency of catalyzer, and can reduce the side reaction such as cracking.
Characteristics of the present invention are to require to determine to sneak into amounts of hydrogen in the charging according to reaction, and amounts of hydrogen is higher than the reaction hydrogen-consuming volume, control amount of liquid and pressure in the reactor by control reactor free air delivery and lifting rate.
For ease of further specifying clear hydrogenation process of the present invention, here process of the present invention is described.As shown in Figure 1, fresh feed with the hydrogen make-up 1 of compressed machine with form logistics after the turning oil that recycle pump 4 is come mixes, then enters the reactor 5 that is filled with required hydrogenation catalyst after fresh feed pump 3 pressurization, enter high score 6 after the reaction.In high score 6, the discharging gas 9 such as a small amount of hydrogen more than needed and a large amount of impurity such as hydrogen sulfide, ammonia, lower carbon number hydrocarbons are emitted system under the effect of hydrogen 7 air lifts, liquid product is divided into the two-way logistics, and one the tunnel is as the finished product 8, and one the tunnel is to mix with fresh feed as the logistics that circulates.This flow process is to control amount of liquid and pressure in the reactor by control reactor 5 to high score 6 free air deliveries and lifting rate.
For another shown in Figure 2, fresh feed after fresh feed pump 3 pressurization with the hydrogen make-up 1 of compressed machine with after the turning oil that recycle pump 4 is come mixes, form logistics, then enter the reactor 5 that is filled with required hydrogenation catalyst, in hydrogen 7 air lifts, the top of reactor 5 can be discharged the discharging gas 10 such as a small amount of hydrogen more than needed and a large amount of impurity such as hydrogen sulfide, ammonia, lower carbon number hydrocarbons and be emitted reactive system.Reaction product enters high score 6, and in high score 6, the discharging gas 9 such as partial vulcanization hydrogen, ammonia, lower carbon number hydrocarbons are emitted system, and liquid product is divided into the two-way logistics, and one the tunnel is as the finished product 8, and one the tunnel is to mix with fresh feed as the logistics that circulates.This flow process is to control amount of liquid and pressure in the reactor by control reactor 5 free air deliveries and lifting rate.In the embodiment, also high score 6 can be set among Fig. 2, reacted liquid phase material direct circulation.
Press the operating process of Fig. 1, the oil hydrofining desulfurization of normal two wires, catalyzer is the FH-UDS catalyzer of Fushun Petrochemical Research Institute's development and production.The chemical hydrogen consumption amount of elder generation's test determination reaction (be 0.27wt% to fresh feed) and Systems Theory dissolved hydrogen amount (being 0.18wt%) are then carried out the inventive method process.Reaction pressure is 6.4MPa, and volume space velocity is 6h during reaction raw materials fluid
-1Mixed hydrogen amount is 0.19wt% (mixed hydrogen amount/inlet amount) in the fixing control oil, and be constant basis, circulation ratio (turning oil volume: the fresh feed volume) be 2: 1, control amount of liquid and pressure in the reactor by control reactor free air delivery and lifting rate.Reaction result treated oil sulphur content is 5 μ g/g, and is substantially suitable with the reaction effect that has now under the high hydrogen-oil ratio operational condition, suitable under catalyst activity stability and the usual terms.This programme illustrates as long as when the mixed hydrogen (constant basis) in the oil reached theoretical dissolution hydrogen, can directly obtain sulphur content less than the ultra-low-sulphur diesel of 10 μ g/g.
Comparative example 1
Operational condition according to embodiment 1, adopt interior pressure and the liquid level of mixed hydrogen amount control reactor of control charging, because the mixed hydrogen amount of design only is slightly more than reactive chemistry hydrogen consumption, in control process, pressure or liquid level are unstable and when reducing mixed hydrogen amount, the amounts of hydrogen of sneaking into is not enough to keep reaction needed, and the sulphur content fluctuation in the reaction product obviously generally changes in 5~550 μ g/g scopes.
Press shown in Fig. 2 flow process, reactor top arranges 2 air lift tower trays, and the air lift hydrogen to oil volume ratio is 5: 1.With desulfurization and denitrogenation, catalyzer is the FHUDS-2 catalyzer of Fushun Petrochemical Research Institute's development and production to the Medium diesel oil raw material 365 ℃ of lower hydrofinings.The chemical hydrogen consumption amount of elder generation's test determination reaction (be 0.58wt% to fresh feed) and system dissolves hydrogen amount (being 0.18wt%) are then carried out the inventive method process.Reaction pressure is 5.5MPa, and volume space velocity is 3.2h during reaction raw materials fluid
-1Mixed hydrogen amount adds 0.8 times of system dissolves hydrogen amount by the reactive chemistry hydrogen-consuming volume, and (the turning oil volume: the fresh feed volume) be 4: 1, namely mixed hydrogen amount is 0.72wt% (mixed hydrogen amount/inlet amount) to circulation ratio in the fixing control oil, and is constant basis.Reaction result treated oil sulphur content is 9 μ g/g.Substantially suitable with the reaction effect under the existing high hydrogen-oil ratio operational condition, suitable under catalyst activity stability and the usual terms.
Comparative example 2
According to working method and the condition of embodiment 2, just reactor top is without the air lift tower tray, and reaction result treated oil sulphur content is about 750 μ g/g, can find out that it is very obvious adopting the technique effect of reactive system of the present invention.
Press shown in Fig. 2 flow process, and do not use wherein occurred frequently 6, reactor top arranges 3 air lift tower trays, and the air lift hydrogen to oil volume ratio is 1: 1.With denitrogenation, catalyzer is 3996 catalyzer of Fushun Petrochemical Research Institute's development and production to vacuum gas oil VGO 380 ℃ of lower hydrotreatments.Then chemical hydrogen consumption amount and the system dissolves hydrogen amount of elder generation's test determination reaction carry out the inventive method process.Reaction pressure is 14.7MPa, and volume space velocity is 1h during reaction raw materials fluid
-1Amounts of hydrogen adds 3 times of system dissolves hydrogen amount by the reactive chemistry hydrogen-consuming volume, and (the turning oil volume: the fresh feed volume) be 3: 1, namely mixed hydrogen amount is 1.72wt% (mixed hydrogen amount/inlet amount) to circulation ratio in the fixing control oil, and is constant basis.Reaction result is denitrification percent 99.0%, and is substantially suitable with the reaction effect that has now under the high hydrogen-oil ratio operational condition, suitable under catalyst activity stability and the usual terms.
Claims (10)
1. method of liquid phase circulation hydrotreatment, part circulation through the liquid product of hydrotreatment is mixed into liquid phase material with raw material, hydrogen is sneaked into liquid phase material, it is characterized in that: the hydrogen mixed volume is by increasing below 20 times of reactive system dissolved hydrogen amount under the reaction conditions on reaction process chemical hydrogen consumption amount basis, the liquid phase material that has mixed hydrogen enters reactor top, reactor top arranges a gas-phase space, the exhaust system that communicates with this gas-phase space is set, by pressure and the liquid level in the free air delivery control reactor of control exhaust system, the hydrogenation catalyst bed that the liquid phase material that has dissolved hydrogen enters reactor lower part carries out the hydrotreatment reaction, liquid-phase reaction product is partly discharged reactive system, and the part circulation mixes with raw material.
2. it is characterized in that in accordance with the method for claim 1: the hydrogen mixed volume is by 1~10 times of reactive system dissolved hydrogen amount under reaction process chemical hydrogen consumption amount basis increase reaction conditions.
3. it is characterized in that in accordance with the method for claim 1: the liquid level control in the reactor adopts free air delivery and lifting rate to control simultaneously.
4. it is characterized in that in accordance with the method for claim 1: the liquid product of circulation and the volume ratio of raw material are 0.1: 1~20: 1.
5. in accordance with the method for claim 1, it is characterized in that: liquid phase material by the reaction conditions of beds is: temperature of reaction is 150~450 ℃, and reaction pressure is 1~17MPa, and volume space velocity is 0.5~15h during liquid
-1
6. in accordance with the method for claim 1, it is characterized in that: at least one air lift tower tray is set in the gas-phase space on reactor top, pass into hydrogen below the air lift tower tray, hydrogen and liquid phase material contact air lift at the air lift tower tray and go out hydrogen sulfide and ammonia in the liquid phase material, hydrogen further is dissolved in the liquid phase material simultaneously, the beds that liquid phase material after the air lift enters reactor lower part carries out the hydrotreatment reaction, and the gas that contains hydrogen sulfide and ammonia after the air lift is discharged reactor from reactor head.
7. in accordance with the method for claim 6, it is characterized in that: the air lift tower tray on reactor top arranges 1~8, the hydrogen that air lift is used is introduced reactor from the following optional position of a bottom tower tray, air lift with the amount of hydrogen by gas-liquid volume ratio count 0.1: 1~50: 1.
8. liquid phase circulation hydrotreatment reactive system, comprise reactor, reactor top arranges a gas-phase space, exhaust system is set to communicate with reactor upper gaseous phase space, reactor lower part is the hydrogenation catalyst bed, reactor arranges pressure monitor system and level monitoring system, it is characterized in that: pressure and the liquid level of controlling reactor by the free air delivery of control exhaust system.
9. according to reactive system claimed in claim 8, it is characterized in that: adopt simultaneously control to discharge the interior liquid level of amount of liquid control reactor of reactor.
10. according to reactive system claimed in claim 8, it is characterized in that: at least one air lift tower tray is set in the reactor upper gaseous phase space, the equipment that passes into hydrogen is set below the air lift tower tray.
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CN102443411B (en) * | 2010-10-13 | 2013-12-04 | 中国石油化工股份有限公司 | Process method for prolonging operation period of hydrogenation device |
CN102443410B (en) * | 2010-10-13 | 2013-12-04 | 中国石油化工股份有限公司 | Method for prolonging operation period of hydrogenation device |
US8926826B2 (en) | 2011-04-28 | 2015-01-06 | E I Du Pont De Nemours And Company | Liquid-full hydroprocessing to improve sulfur removal using one or more liquid recycle streams |
RU2596828C1 (en) | 2012-09-21 | 2016-09-10 | Чайна Петролиум Энд Кемикл Корпорейшн | Hydrocarbon oil hydrotreating method and device |
CN103965959A (en) * | 2013-01-30 | 2014-08-06 | 中国石油天然气股份有限公司 | Liquid phase hydrogenation reaction method for multi-stage hydrogen dissolving |
CN104099127A (en) * | 2013-04-03 | 2014-10-15 | 中国石油天然气股份有限公司 | Distillate oil hydrotreating process |
CN104178206A (en) * | 2013-05-22 | 2014-12-03 | 中石化洛阳工程有限公司 | Liquid-solid two-phase hydrogenation process and device thereof |
CN105524657B (en) * | 2014-09-29 | 2017-03-29 | 中国石油化工股份有限公司 | A kind of fraction oil boiling bed hydrogenation method |
CN106311093A (en) * | 2015-07-01 | 2017-01-11 | 中国石化扬子石油化工有限公司 | Reactor used for reformate hydrogenation deolefination |
CN109126672A (en) * | 2018-09-18 | 2019-01-04 | 汤美侠 | A kind of Chemical Manufacture liquid phase hydrogenation reactor |
CN114515549A (en) * | 2020-11-18 | 2022-05-20 | 中国石油化工股份有限公司 | Pre-hydrogenation reaction system, pre-hydrogenation reaction method and application |
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