CN105733662A - Liquid phase hydrogenation reactor and process - Google Patents
Liquid phase hydrogenation reactor and process Download PDFInfo
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- CN105733662A CN105733662A CN201410758712.XA CN201410758712A CN105733662A CN 105733662 A CN105733662 A CN 105733662A CN 201410758712 A CN201410758712 A CN 201410758712A CN 105733662 A CN105733662 A CN 105733662A
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Abstract
The invention discloses a liquid phase hydrogenation reactor. The liquid phase hydrogenation reactor comprises a tube-shell type reactor, a heat exchanger and a hydrogen dissolution mixer. The tube-shell type reactor comprises an inner tube and a shell pass. The inner tube is filled with a hydrogenation catalyst and used for performing liquid phase hydrogenation of raw material oil after hydrogen dissolution and the hydrogenation catalyst and for discharging a hydrogenation product. The shell pass is disposed outside the inner tube, and is used for exchanging heat generated in the hydrogenation through adopting fed circulating hydrogen as a cold compound. The invention also discloses a liquid phase hydrogenation process.
Description
Technical field
The present invention relates to a kind of hydrogenation method and reactor, specifically, relate to a kind of liquid-phase hydrogenation processing method and reactor, be mainly used in technical field of petrochemical industry.
Background technology
The sustainable development of current World Economics and the increasingly stringent of environmental regulation, it is necessary to produce a large amount of light clean fuel, these are desirable that improves existing oil Refining Technologies.At present, the hydrogenation technique being main purpose with desulfurization and upgrading is applied widely in Clean Fuel Production.
Hydrogen addition technology is to improve one of conventional technology of oil quality, it is common that in order to remove the magazines such as sulfur in raw material, nitrogen, oxygen, metal, or the catalytic reaction process reducing the size of raw molecule and carrying out.In this process, the hydrogen of actual participation reaction only has the hydrogen of chemical hydrogen consumption, but in tradition trickle bed hydrogenation technique, it is necessary to amounts of hydrogen be far longer than chemical hydrogen consumption.Main cause has two.One is hydrogenation reaction is a strong exothermal reaction, in order to control reaction temperature, it is necessary to substantial amounts of hydrogen and raw oil take away reaction heat by beds；Two is in gas-liquid-solid phase reaction, and the hydrogen dividing potential drop remaining higher is conducive to hydrogenation reaction, it is suppressed that coke generates, and extends catalyst life.Do not participate in the hydrogen of reaction by separator and liquid phase separation and after removing impurity, be re-delivered in reactor after being improved pressure by circulating hydrogen compressor and participate in reacting.Circulating hydrogen compressor is as the key equipment of hydrogenation process, and investment and operating cost are higher, if it is possible to reduced by hydrogen flowing quantity, it is possible to be greatly saved investment for enterprise, also reduces cost for fuels cleaning Technique Popularizing.
In liquid-phase hydrogenatin technique, hydrogen and the premixing of raw oil elder generation, make hydrogen be dissolved in raw oil, enter back into reactor and react, in reaction, required hydrogen is entirely from the hydrogen dissolved.It is smaller that liquid-phase hydrogenatin technique has reactor, and cost of investment is low, and reaction temperature such as is easily controlled at the advantage.But there is also following problem, one is to meet amounts of hydrogen required in hydrogenation process, it is necessary to use substantial amounts of recycle oil or the extra solvent that adds to dissolve hydrogen, cause hydrogenation efficiency to reduce；Two is to control reaction temperature, it is necessary to injects cold hydrogen or cold oil to beds, takes away reaction heat.
US Patent No. 20060144756A1 discloses a kind of two-phase hydrogenation and controls system approach and device.In continuous print liquid-phase hydrogenatin process, eliminating recycle hydrogen, the hydrogen required for hydrogenation reaction comes from the hydrogen of liquid phase dissolved, it is not necessary to extra hydrogen.But it needs to use the bigger solvent of hydrogen solubility or diluent to dissolve hydrogen, affects follow-up hydrogenation efficiency.
Publication number is the U.S. patent Nos of US6213835 and US6428686, publication number is a kind of hydrogenation technique dissolving hydrogen in advance disclosed in the Chinese invention patent of CN200680018017.3, controls the amount of liquid in reactor or air pressure by controlling the amounts of hydrogen in liquid feedstock.But the problem of the objectionable impurities eliminations such as H2S, NH3 of generation that it is not solved by hydrogenation process, cause that it constantly accumulates in reactor, greatly reducing reaction efficiency, also cannot effectively process sulfur, raw material that nitrogen content is higher, above-mentioned patent is also without the concrete structure of open reactor.
Publication number is in the Chinese invention patent of CN1488711, discloses a kind of hydrogenation of residual oil suspended bed method for transformation, the heat exchange response system provided in the method, including interior pipe and shell side, but, do not add hydrogenation catalyst at this interior pipe, meanwhile, shell side does not adopt circulating hydrogen carry out heat exchange.
Publication number is in the Chinese invention patent of CN102049220, disclose a kind of strengthening boiling bed hydrogenation reactor, the method carries out hydrogenation reaction by hydrogenation material and catalyst, but liquid-phase hydrogenatin device is not provided in the method, it is impossible to carry out heat exchange by circulating hydrogen.
Summary of the invention
It is an object of the invention to provide a kind of liquid phase hydrogenation reactor and process thereof, to overcome the hydrogen existed in prior art to cannot be carried out cycle heat exchange, the hydrogenation reaction efficiency caused is low, and hydrogen demand amount is big, and the problem that the equipment investment caused increases.
For reaching above-mentioned purpose, the invention provides a kind of liquid phase hydrogenation reactor, including:
Shell-and-tube reactor, this reactor includes:
Interior pipe: fill hydrogenation catalyst in it, for the raw oil after the molten hydrogen of input is carried out liquid-phase hydrogenatin reaction with described hydrogenation catalyst, and exports hydrogenation reaction product；
Shell side, is arranged at the outside of said inner tube, as solidifiable substance, described hydrogenation reaction liberated heat is carried out heat exchange for the circulating hydrogen by inputting；
Heat exchanger, is connected to described shell side, for the described circulating hydrogen after the heat exchange of described shell side and described raw oil are carried out heat exchange again；
Molten hydrogen blender, it is connected to said inner tube, described shell side and described heat exchanger, this molten hydrogen blender is for receiving the described raw oil after described heat exchanger heat exchange and described circulating hydrogen, and the hydrogen newly supplemented, carry out abundant molten hydrogen to after saturated, raw oil after the said inner tube molten hydrogen of output, and carry out described hydrogenation reaction heat exchange to the described shell side described circulating hydrogen of output, to realize the circulation of hydrogen.
Above-mentioned liquid phase hydrogenation reactor, also includes:
Knockout drum, is connected to said inner tube, receives described hydrogenation reaction product, and described product is carried out gas-liquid separation, respectively output gaseous product and hydrogenated products.
Above-mentioned liquid phase hydrogenation reactor, also includes:
Hydrogen gas compressor, is connected to described heat exchanger and described shell side, for described circulating hydrogen is increased pressure.
Above-mentioned liquid phase hydrogenation reactor, the active component of described hydrogenation catalyst includes: W and Ni, and in oxide weight, the content of W is 0.5～32%, and the content of Ni is 2～32%.
Above-mentioned liquid phase hydrogenation reactor, described gaseous product includes: H2S and NH3。
Above-mentioned liquid phase hydrogenation reactor, described molten hydrogen blender is microbubble generator, is completely dissolved in described raw oil by described circulating hydrogen.
Above-mentioned liquid phase hydrogenation reactor, the reaction temperature of described hydrogenation reaction is: 330-380 degree, and reaction pressure is: 5-9MPa, and volume space velocity is: 0.5-2h-1, hydrogen consumption is 0.1～2wt%.
The present invention also provides for a kind of liquid-phase hydrogenation processing method, adopts liquid phase hydrogenation reactor described above, and described reactor includes: shell-and-tube reactor, heat exchanger and molten hydrogen blender, described method, including:
Reactions steps: for by filling hydrogenation catalyst in the interior pipe of described shell-and-tube reactor, carrying out liquid-phase hydrogenatin reaction with the raw oil after the molten hydrogen of input, and export hydrogenation reaction product；And by being arranged in the shell side of the described shell-and-tube reactor outside said inner tube the circulating hydrogen inputted as solidifiable substance, described hydrogenation reaction liberated heat is carried out heat exchange；
Heat exchange step: for the described circulating hydrogen after the heat exchange of described shell side and described raw oil are carried out heat exchange again；
Molten hydrogen blend step: for being received the described raw oil after described heat exchanger heat exchange and described circulating hydrogen by described molten hydrogen blender, and the hydrogen newly supplemented, carry out abundant molten hydrogen to after saturated, raw oil after the said inner tube molten hydrogen of output, and carry out described hydrogenation reaction heat exchange to the described shell side described circulating hydrogen of output, to realize the circulation of hydrogen.
Above-mentioned liquid-phase hydrogenation processing method, adopts hydrogen outside heat removing mode in described liquid-phase hydrogenation processing method.
Above-mentioned liquid-phase hydrogenation processing method, the reaction temperature of described hydrogenation reaction is: 330-380 degree, and reaction pressure is: 5-9MPa, and volume space velocity is: 0.5-2h-1, hydrogen consumption is 0.1～2wt%.
Compared with prior art, being liquid phase reacting material with what solid catalyst contacted in the present invention, reactor volume reduces, and reaction efficiency improves；Hydrogen outside heat removing, flow process is simple；Hydrogen heat-obtaining heat release forms recycle heat, and hydrogen utilization ratio is high, energy-optimised utilization；Byproduct of reaction H2S and NH3 discharges response system in time, improves hydrogenation reaction efficiency further.
Accompanying drawing explanation
Fig. 1 is liquid phase hydrogenation reactor structural representation of the present invention；
Fig. 2 is liquid-phase hydrogenation processing method schematic flow sheet of the present invention.
Wherein, accompanying drawing labelling:
Hydrogen after 1 raw oil 2 heat release；
The raw oil after the molten hydrogen of hydrogen 4 superfluous after 3 molten hydrogen；
Hydrogen 6 hydrogenation reaction product after 5 heat absorptions；
7 hydrogen newly supplemented；The gaseous by-products such as 8H2S, NH3；
9 hydrogenated products
11 liquid phase hydrogenation reactor 12 heat exchangers
13 molten hydrogen blender 14 knockout drums
15 hydrogen gas compressors
Detailed description of the invention
Introduce the realization of the present invention below by way of specific embodiment and had the advantage that, but accordingly the practical range of the present invention should do not constituted any restriction.All within the spirit and principles in the present invention, any amendment of making, equivalent replacement, improvement etc., should be included within protection scope of the present invention.
A kind of liquid-phase hydrogenation processing method of the present invention and reactor can be used for the deep desulfuration of poor ignition quality fuel component, denitrogenation, Porous deproteinized bone, produce cleaning diesel oil, can also be used for the hydrofinishings such as Petroleum, aerial kerosene, lubricating oil, paraffin and produce high-quality oil product, and produce high-quality cleaning boat coal, diesel oil technical process for wax oil raw material mild hydrocracking.
A kind of liquid phase hydrogenating method provided by the invention and reactor, adopt shell-and-tube liquid phase hydrogenation reactor, hydrogen enters the shell side of reactor as cold medium, take hydrogenation reaction liberated heat away, hydrogen after heat-obtaining enters heat exchanger, with raw oil heat exchange, heating raw oil, exothermic hydrogen enters molten hydrogen blender with the new hydrogen supplemented together with absorbing the raw oil of heat, after making the abundant molten hydrogen of raw oil extremely saturated, excessive hydrogen goes successively to the shell side heat-obtaining of reactor, forms the circulation of hydrogen.Raw oil after molten hydrogen enters reactor tube side, contacts with catalyst, carries out liquid-phase hydrogenatin reaction.Product enters knockout drum, and top portion separates out H2S and NH3, and bottom obtains product.
Fig. 1 is the structural representation of liquid phase hydrogenation reactor of the present invention, as it is shown in figure 1, one liquid phase hydrogenation reactor of the present invention, including: shell-and-tube reactor 11, heat exchanger 12, molten hydrogen blender 13, knockout drum 14 and hydrogen gas compressor 15；
Wherein, shell-and-tube reactor 11 includes: interior pipe 111 and shell side 112, fills hydrogenation catalyst in interior pipe 111, for the raw oil 4 after the molten hydrogen of input is carried out liquid-phase hydrogenatin reaction with hydrogenation catalyst, and exports hydrogenation reaction product 6；Shell side 112 is arranged at the outside of interior pipe 111, as solidifiable substance, hydrogenation reaction liberated heat is carried out heat exchange for the circulating hydrogen by inputting；Wherein, interior pipe 111 claims tube side, fills hydrogenation catalyst, for reaction zone；Interior pipe 111 is outside claims shell side 112, for heat transfer zone.
Heat exchanger 12, is connected to shell side 112, and for the circulating hydrogen after the heat exchange of shell side 112 and raw oil 1 are carried out heat exchange again, this circulating hydrogen is the hydrogen 5 after heat absorption；
Molten hydrogen blender 13, it is connected to interior pipe 111, shell side 112 and heat exchanger 12, this molten hydrogen blender 13 is for receiving the raw oil 1 after heat exchanger 12 heat exchange and circulating hydrogen, this circulating hydrogen is the hydrogen 2 after heat release, and the new hydrogen 7 supplemented, and carries out abundant molten hydrogen to after saturated, inside pipe 111 exports the raw oil 4 after molten hydrogen, and export circulating hydrogen to shell side 112 and carry out hydrogenation reaction heat exchange, the hydrogen 3 that this circulating hydrogen is superfluous after being molten hydrogen, to realize the circulation of hydrogen.
Knockout drum 14, is connected to interior pipe 111, receives hydrogenation reaction product 6, product is carried out gas-liquid separation, respectively output gaseous product and hydrogenated products.Wherein, gaseous product includes H2S and NH3Gas phase side-product 8, gaseous product flows out from the upper outlet of knockout drum 14, and hydrogenated products 9 flow out from the outlet at bottom of knockout drum 14.
Hydrogen gas compressor 15, is connected to heat exchanger 12 and shell side 112, for circulating hydrogen is increased pressure.
Wherein, the active component of hydrogenation catalyst includes: W and Ni, and in oxide weight, the content of W is 0.5～32%, and the content of Ni is 2～32%.
In the specific embodiment of the invention, molten hydrogen blender is microbubble generator, is completely dissolved in by circulating hydrogen in raw oil 1, makes raw oil 1 become the supersaturated solution of hydrogen, but the present invention can also adopt other kinds of molten hydrogen blender, and the present invention is not limited to this.
In the specific embodiment of the invention, the reaction temperature of hydrogenation reaction is: 330-380 degree, and reaction pressure is: 5-9MPa, and volume space velocity is: 0.5-2h-1, hydrogen consumption is 0.1～2wt%.But the present invention also can adopt the above-mentioned parameter of other scopes, and the present invention is not limited to this.
In the specific embodiment of the invention, being liquid phase reacting material with what solid-phase catalyst contacted, be absent from substantial amounts of hydrogen so that reactor volume reduces, and is absent from the gas phase problem to liquid phase and solid-state diffusion in the present invention, reaction efficiency improves.
In the specific embodiment of the invention, adopting hydrogen outside heat removing, it is not necessary to inject cold hydrogen or cold oil to beds, be also absent from the problem that follow-up heat-obtaining medium separates in the present invention, flow process is simple, and hydrogen circulation amount reduces, and utilization rate is high.
In the specific embodiment of the invention, after hydrogen autoreactor takes heat away in the present invention, heating raw oil 1, release heat, form recycle heat, energy utilization efficiency improves.
In the specific embodiment of the invention, in the present invention, hydrogenation reaction product enters knockout drum, and top portion separates out H2S and NH3, and byproduct of reaction is got rid of response system in time, improves hydrogenation reaction efficiency further.But the present invention is not limited to this.
Fig. 2 is the schematic flow sheet of liquid phase hydrogenating method of the present invention, as in figure 2 it is shown, the present invention also provides for a kind of liquid-phase hydrogenation processing method, adopt liquid phase hydrogenation reactor described above, reactor includes: shell-and-tube reactor 11, heat exchanger 12 and molten hydrogen blender 13, the method, including:
Reactions steps S1: for by filling hydrogenation catalyst in the interior pipe 111 of shell-and-tube reactor 11, carrying out liquid-phase hydrogenatin reaction with the raw oil 1 after the molten hydrogen of input, and export hydrogenation reaction product；And by being arranged in the shell side 112 of the shell-and-tube reactor 11 outside interior pipe 111 circulating hydrogen inputted as solidifiable substance, hydrogenation reaction liberated heat is carried out heat exchange；
Heat exchange step S2: for the circulating hydrogen after the heat exchange of shell side 112 and raw oil 1 are carried out heat exchange again；
Molten hydrogen blend step S3: for being received the raw oil 1 after heat exchanger 12 heat exchange and circulating hydrogen by molten hydrogen blender 13, and the hydrogen newly supplemented, carry out abundant molten hydrogen to after saturated, inside pipe 111 exports the raw oil 1 after molten hydrogen, and export circulating hydrogen to shell side 112 and carry out hydrogenation reaction heat exchange, to realize the circulation of hydrogen.
Wherein, the reaction temperature of hydrogenation reaction is: 330-380 degree, and reaction pressure is: 5-9MPa, and volume space velocity is: 0.5-2h-1, hydrogen consumption is 0.1～2wt%.
Below by way of specific embodiment, the effect that is embodied as of liquid-phase hydrogenation processing method of the present invention is described in detail:
Experiment adopts the flow process shown in Fig. 2, adopts feedstock property in Table one (raw oil 1 character).
Table 1 raw oil 1 character
| Density (20 DEG C), g/cm3 | 0.8503 |
| Boiling range, DEG C | 165/365 |
| Sulfur, μ g/g | 10520 |
| Nitrogen, μ g/g | 133 |
| Cetane number | 53.2 |
| Existent gum, mg/100ml | 290 |
| Polycyclic aromatic hydrocarbon, wt% | 8.9 |
Adopt the reactor that the present invention relates to shown in Fig. 1 and a kind of hydrogenation technique flow process being suitable for thereof, raw oil 1 character is as described in Table 1, catalyst adopts the PHF-102 catalyst researched and developed voluntarily, the active component of hydrogenation catalyst PHF-102 includes: W and Ni, in oxide weight, the content of W is 0.5～32%, and the content of Ni is 2～32%.
Reaction condition and product property are as shown in table 2.As can be seen from Table 2,400 DEG C are risen to temperature 330 DEG C, sulfur content is dropped to 9.7 μ g/g, 8.6 μ g/g, 8.5 μ g/g respectively by 10520 μ g/g, nitrogen content is dropped to 2.0 below μ g/g by 133 μ g/g, Cetane number is risen to more than 55 by 53.2, product property is necessarily improved, and this illustrates that this reactor involved in the present invention can be used in liquid-phase hydrogenatin process.
Table 2 embodiment one process conditions and product property
* note: circulation volume ratio=recycle oil/fresh feed
In sum, liquid phase hydrogenation reactor of the present invention and process thereof, to take circulating hydrogen mode, after hydrogen autoreactor takes heat away, heat raw oil, release heat, form recycle heat, energy utilization efficiency improves；Reactor volume of the present invention reduces, and reaction efficiency is greatly improved；Further, the present invention adopts hydrogen outside heat removing, it is not necessary to injecting cold hydrogen or cold oil to beds, be also absent from the problem that follow-up heat-obtaining medium separates, flow process is simple, and hydrogen circulation amount reduces, and utilization rate is high.
Certainly; the present invention also can have other various embodiments; when without departing substantially from present invention spirit and essence thereof; those of ordinary skill in the art are when can make various corresponding change and deformation according to the present invention, but these change accordingly and deformation all should belong to the scope of the claims appended by the present invention.
Claims (10)
1. a liquid phase hydrogenation reactor, it is characterised in that including:
Shell-and-tube reactor, this reactor includes:
Interior pipe: fill hydrogenation catalyst in it, for the raw oil after the molten hydrogen of input is carried out liquid-phase hydrogenatin reaction with described hydrogenation catalyst, and exports hydrogenation reaction product；
Shell side, is arranged at the outside of said inner tube, as solidifiable substance, described hydrogenation reaction liberated heat is carried out heat exchange for the circulating hydrogen by inputting；
Heat exchanger, is connected to described shell side, for the described circulating hydrogen after the heat exchange of described shell side and described raw oil are carried out heat exchange again；
Molten hydrogen blender, it is connected to said inner tube, described shell side and described heat exchanger, this molten hydrogen blender is for receiving the described raw oil after described heat exchanger heat exchange and described circulating hydrogen, and the hydrogen newly supplemented, carry out abundant molten hydrogen to after saturated, raw oil after the said inner tube molten hydrogen of output, and carry out described hydrogenation reaction heat exchange to the described shell side described circulating hydrogen of output, to realize the circulation of hydrogen.
2. liquid phase hydrogenation reactor according to claim 1, it is characterised in that also include:
Knockout drum, is connected to said inner tube, receives described hydrogenation reaction product, and described product is carried out gas-liquid separation, respectively output gaseous product and hydrogenated products.
3. liquid phase hydrogenation reactor according to claim 2, it is characterised in that also include:
Hydrogen gas compressor, is connected to described heat exchanger and described shell side, for described circulating hydrogen is increased pressure.
4. liquid phase hydrogenation reactor according to claim 1, it is characterised in that the active component of described hydrogenation catalyst includes: W and Ni, and in oxide weight, the content of W is 0.5～32%, and the content of Ni is 2～32%.
5. liquid phase hydrogenation reactor according to claim 2, it is characterised in that described gaseous product includes: H2S and NH3。
6. liquid phase hydrogenation reactor according to claim 1, it is characterised in that described molten hydrogen blender is microbubble generator, is completely dissolved in described raw oil by described circulating hydrogen.
7. liquid phase hydrogenation reactor according to claim 1, it is characterised in that the reaction temperature of described hydrogenation reaction is: 330-380 degree, and reaction pressure is: 5-9MPa, and volume space velocity is: 0.5-2h-1, hydrogen consumption is 0.1～2wt%.
8. a liquid-phase hydrogenation processing method, adopts liquid phase hydrogenation reactor as according to any one of claim 1-7, and described reactor includes: shell-and-tube reactor, heat exchanger and molten hydrogen blender, it is characterised in that described method, including:
Reactions steps: for by filling hydrogenation catalyst in the interior pipe of described shell-and-tube reactor, with the raw oil after the molten hydrogen of input
Carry out liquid-phase hydrogenatin reaction, and export hydrogenation reaction product；And by being arranged in the shell side of the described shell-and-tube reactor outside said inner tube the circulating hydrogen inputted as solidifiable substance, described hydrogenation reaction liberated heat is carried out heat exchange；
Heat exchange step: for the described circulating hydrogen after the heat exchange of described shell side and described raw oil are carried out heat exchange again；
Molten hydrogen blend step: for being received the described raw oil after described heat exchanger heat exchange and described circulating hydrogen by described molten hydrogen blender, and the hydrogen newly supplemented, carry out abundant molten hydrogen to after saturated, raw oil after the said inner tube molten hydrogen of output, and carry out described hydrogenation reaction heat exchange to the described shell side described circulating hydrogen of output, to realize the circulation of hydrogen.
9. liquid-phase hydrogenation processing method described in claim 8, it is characterised in that adopt hydrogen outside heat removing mode in described liquid-phase hydrogenation processing method.
10. liquid-phase hydrogenation processing method according to claim 8, it is characterised in that the reaction temperature of described hydrogenation reaction is: 330-380 degree, and reaction pressure is: 5-9MPa, and volume space velocity is: 0.5-2h-1, hydrogen consumption is 0.1～2wt%.
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| CN107365599A (en) * | 2017-07-28 | 2017-11-21 | 大庆亿鑫化工股份有限公司 | A kind of food-grade normal hexane low-voltage hydrogenation production technology |
| CN108018070A (en) * | 2016-10-28 | 2018-05-11 | 中国石油化工股份有限公司 | A kind of heavy oil feedstock fixed bed hydrogenation system |
| CN111359542A (en) * | 2019-03-15 | 2020-07-03 | 南京延长反应技术研究院有限公司 | Micro-interface reinforced diesel hydrofining reaction system and method |
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| CN108018070A (en) * | 2016-10-28 | 2018-05-11 | 中国石油化工股份有限公司 | A kind of heavy oil feedstock fixed bed hydrogenation system |
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| CN111686651A (en) * | 2019-03-15 | 2020-09-22 | 南京延长反应技术研究院有限公司 | Micro-interface reinforced suspension bed hydrogenation reaction system and method |
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