CN103789006A - A two-phase hydrogenation reactor and a two-phase hydrogenation method - Google Patents
A two-phase hydrogenation reactor and a two-phase hydrogenation method Download PDFInfo
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Abstract
The invention provides a two-phase hydrogenation reactor and a two-phase hydrogenation method. Each space surrounded by the upper parts of each gas-liquid distributor, a corresponding liquid-phase collecting tray and a corresponding downcomer is a gas-phase chamber. Hydrogen is introduced into the gas-phase chambers from outside of the reactor. The liquid phase in the upper part of the reactor is collected by the liquid-phase collecting trays and flows onto gas-liquid distributing trays through the downcomers. The gas phase and the liquid phase are subjected to violent mass transfer by the gas-liquid distributors so that the hydrogen can be dissolved in the liquid phase well. The gas phase and the liquid phase in gas and liquid materials are separated after passing through the gas-liquid distributing trays. The liquid phase where the hydrogen is dissolved goes downward into catalyst bed layers to perform hydrogenation. The gas phase converges under the gas-liquid distributors and is discharged from the reactor. The two-phase hydrogenation reactor and the two-phase hydrogenation method can further enhance reaction effects of two-phase hydrogenation.
Description
Technical field
The present invention relates to a kind of two-phase hydrogenation reactor and two-phase hydrogenation method, relate in particular to a kind of two-phase hydrogenation reactor and two-phase hydrogenation method of diesel raw material two-phase hydrogenation production fine-quality diesel oil product, belong to petrochemical industry.
Background technology
Along with the continuous enhancing of people's environmental consciousness, environmental law Laws & Regulations requires stricter to engine exhaust emission, and various standard of fuel require the content of S, N also harsher.Simultaneously due to the continuous increase of Oil extraction amount and the continuous minimizing of conventional crude reserves, crude oil in poor quality trend is more and more serious, how S, the also corresponding increase of N content of the middle runnings that the secondary processing such as the intermediate oil that crude oil straight run distillation obtains and coking, catalytic cracking obtain, be processed into the middle runnings higher foreign matter content such as sulphur, nitrogen and meet the major issue that the product Shi Ge refinery of environmental requirement faces.
Hydrogenation process is the most economical effective scheme that removes middle runnings impurity.Existing most of hydrogenation unit all adopts higher hydrogen-oil ratio and hydrogen dividing potential drop, to guarantee the catalyst runs life-span, promotes the reactions such as hydrogenating desulfurization, denitrogenation, aromatic saturation and cracking.But the higher hydrogen gas circulating system of pressure needs high investment cost and running cost, has indirectly increased oil manufacture cost.
Along with the deepen continuously understanding of technician to hydrogen addition technology, a kind of two-phase hydrogenation technology is developed.In raw material and thinning oil, dissolve supersaturation hydrogen, directly enter reactor and carry out hydrogenation reaction, cancel recycle hydrogen system, reduce costs.Owing to having cancelled recycle hydrogen system, so this technique has certain limitation to the adaptability of raw material.This technology is mainly two-phase in reaction process, i.e. liquid phase (stock oil and thinning oil) and solid phase (catalyzer) claims in this patent that this technique is two-phase hydrogenation technology.
The key of two-phase hydrogenation technology is the meltage of hydrogen in oil, the meltage of hydrogen is more, hydrogenation effect is better, if the amounts of hydrogen deficiency of dissolving, there is hot polymerization reaction because there is no hydrogen in the latter half of branch of reactor, a large amount of carbon deposits on catalyzer, even cause reactor bed pressure drop to raise, so two-phase hydrogenation technology all adopts a large amount of turning oil to carry reaction hydrogen.Be generally and reduce turning oil consumption, reduce energy consumption, the reactor of two-phase hydrogenation technology is generally less, and molten hydrogen storage equipment is set between reactor, to promote the hydrogenation reaction degree of depth.
US6881326 has introduced a kind of two-phase hydrogenation preconditioning technique.Its technological process is that fresh feed oil, turning oil and hydrogen are dissolved in hydrogen in oil through a mixed hydrogen production device, and the oil that dissolves hydrogen enters less reactor and contacts and carry out hydrogenation reaction with catalyzer, deviates from the impurity in oil.After reaction, a logistics part is circulated to mixed hydrogen production device, and a part is discharged from device as product.This method is dissolved in required hydrogen in oil before adopting raw material and turning oil to enter reactor in advance, can omit recycle hydrogen system.The method reactor is generally less, needs to set up molten hydrogen storage equipment between reactor, and needs a large amount of turning oil to carry hydrogen.
Summary of the invention
For the deficiencies in the prior art, the invention provides a kind of two-phase hydrogenation reactor and application, can realize hydrogen at catalyst bed interlayer and dissolve, promote hydrogenation reaction.
In two-phase hydrogenation reactor of the present invention, at least one beds is set, adopts the operating method of upper feeding bottom discharge, on the top of at least one beds, molten hydrogen storage equipment is set; Molten hydrogen storage equipment comprises liquid phase catch tray, falls liquid passage and gas-liquid partition tray, and liquid phase catch tray is arranged on gas-liquid partition tray top, and hydrogen make-up entrance is set between liquid phase catch tray and gas-liquid partition tray; Gas-liquid allotter is set on gas-liquid partition tray, falls between liquid passage and gas-liquid partition tray and have gap, the upper end in gap is lower than the upper end gas-liquid entrance of gas-liquid allotter on gas-liquid partition tray; Between gas-liquid partition tray and the beds of bottom, gas-liquid separation space is set, and the relief outlet of excess hydrogen is set.
In two-phase hydrogenation reactor of the present invention, liquid phase catch tray and fall liquid passage and be connected, Main Function is to collect the liquid phase that reactor top flows down, and then guides on gas-liquid partition tray by falling liquid passage; Liquid phase catch tray can also prevent that supplementary hydrogen from upwards flowing into upper catalyst bed layer simultaneously.
In two-phase hydrogenation reactor of the present invention, fall liquid passage at least one, fall liquid passage can be arranged on reactor wall one side, also can be arranged in the middle of reactor.The total actual internal area that falls liquid passage is 1.0～2.0 times of reactor feed pipe actual internal area, preferably 1.0～1.2 times.Fall at the bottom of liquid passage along and gas-liquid partition tray face between actual internal area be 1.0～2.0 times of reactor feed pipe actual internal area, preferably 1.1～1.5 times.
In two-phase hydrogenation reactor of the present invention, gas-liquid allotter is set on gas-liquid partition tray, the gas-liquid mixed mass transfer parts that gas-liquid allotter is well known to those skilled in the art.Gas-liquid allotter can be conventional various forms, as (mixed type have suction function and overflow effect) such as suction type gas-liquid allotter, overflow type gas-liquid allotter, mixed type gas-liquid allotters simultaneously.Liquid level when suction occurs for suction type gas-liquid allotter and mixed type gas-liquid allotter is higher than falling edge at the bottom of liquid passage, and the liquid level when overflow of overflow type gas-liquid allotter liquid phase is higher than falling edge at the bottom of liquid passage.For the suction type gas-liquid allotter with blister configuration, at the bottom of gas-liquid allotter bubble-cap, along being to fall at the bottom of liquid passage along apart from 1.2～2.5 times of gas-liquid partition tray face height apart from gas-liquid partition tray face height, be preferably 1.5～2.0 times.Concrete height makes the appropriate adjustments according to the structure of bubble-cap.
In two-phase hydrogenation reactor of the present invention, hydrogen make-up entrance and excess hydrogen relief outlet can be arranged on the wall of reactor, also can adopt other suitable mode, for example, adopt through the hydrogen make-up pipeline of beds with through the excess hydrogen escape route of beds.
Two-phase hydrogenation technology of the present invention, adopts two-phase hydrogenation reactor of the present invention, is greater than any distillate of 120 ℃ as raw material take boiling range, under hydroconversion condition, carries out two-phase hydrogenation reaction, and reaction liquid phase effluent part loops back reactor.
Two-phase hydrogenation process conditions of the present invention is: 100 ~ 400 ℃ of temperature of reaction, preferably 260 ~ 380 ℃; Reaction pressure 1.5 ~ 8.0MPa, preferably 2.0 ~ 6.0MPa; Volume space velocity 0.6 ~ 5.0h
-1, preferably 1.0 ~ 2.5h
-1; Turning oil and fresh feed volume mixture volume ratio are 0.5:1 ~ 6.0:1, preferably 1:1 ~ 3:1; The supplementary amounts of hydrogen of the molten hydrogen storage equipment of catalyst bed interlayer is generally pressed gas-liquid volume ratio 2:1 ~ 100:1, preferably 5:1 ~ 50:1.
The hydrotreating catalyst that the hydrogenation catalyst using in two-phase hydrogenation technique of the present invention is this area routine, wherein the active metal component of catalyzer can be nickel, cobalt, molybdenum or tungsten etc. one or more, catalyzer carries out sulfidizing before use, and active metal component is converted into sulphided state.Catalyzer composition can comprise by weight percentage: nickel or cobalt are that 0.5% ~ 10%(calculates by its oxide compound), molybdenum or tungsten are that 1% ~ 35%(calculates by its oxide compound), carrier can be aluminum oxide, silicon oxide, aluminium oxide-silicon oxide, titanium oxide etc. one or more.Catalyzer is extrudate or spherical.The bulk density of catalyzer is 0.5 ~ 1.1g/cm
3, granules of catalyst diameter (spherical diameter or bar shaped diameter) is 0.04 ~ 1.0mm, specific surface area is 80 ~ 350m
2/ g.Beds adopts fixed bed form.
Gas-liquid allotter of the present invention top and liquid phase catch tray, to fall the space that liquid passage surrounds be phase chamber, hydrogen make-up is introduced phase chamber outward by reactor, the liquid phase on reactor top is collected by liquid phase catch tray, flow on gas-liquid partition tray by falling liquid passage, gas phase is mixed mass transfer with liquid phase through gas-liquid allotter fierceness, hydrogen is dissolved in liquid phase well, gas-liquid mixed material is by after gas-liquid partition tray, gas-liquid separation, the liquid phase of having dissolved hydrogen enters beds downwards and carries out hydrogenation reaction, and gas phase is collected and drawn reactor below gas-liquid partition tray.
Specifically, tool of the present invention has the following advantages:
1, molten hydrogen storage equipment volume is small and exquisite, is arranged between beds and reactor inlet, takies reactor volume little, and molten hydrogen efficiency is high; The introducing of hydrogen make-up and the discharge of excess hydrogen, guaranteed that reaction system carries out in liquid phase, and to two-phase hydrogenation, reaction does not exert an influence.
The problem that 2, can solve the outer molten hydrogen of existing two-phase hydrogenation Technology Need device, also can realize the maximization of two-phase hydrogenation reactor.
3, the present invention can realize at existing fixed bed hydrogenation reactor, and gas-liquid partition tray is existing mature technology, only need install liquid phase collecting board additional and fall liquid passage, and improvement expenses is very low.
4, reactor of the present invention is by adopting suitable molten hydrogen storage equipment, when dissolved hydrogen air lift supplies hydrogenation reaction, can take the impurity parts such as the hydrogen sulfide in liquid phase material out of reactor, reduce the restraining effect of hydrogen sulfide to hydrogenation reaction, under identical condition, improve hydrogenation reaction effect.
Accompanying drawing explanation
Fig. 1 is a kind of two-phase hydrogenation reactor of the present invention and molten hydrogen storage equipment and the main schematic diagram of looking of application.
Wherein: 1-reactor, liquid passage falls in 2-, 3-gas-liquid allotter, 4-beds, 5-liquid phase catch tray, 6-hydrogen intake, 7-hydrogen outlet, 8-gas-liquid partition tray.
Embodiment
Below in conjunction with accompanying drawing, a kind of molten hydrogen storage equipment of two-phase hydrogenation reactor of the present invention and application are further described.
As shown in Figure 1, raw material and turning oil enter in reactor 1, flow into liquid phase catch tray 5 downwards, flow into gas-liquid partition tray 8 cards by falling liquid passage 2, hydrogen is introduced phase chamber outward by reactor, gas phase is mixed mass transfer with liquid phase by gas-liquid allotter 3 fiercenesses on gas-liquid partition tray 8, hydrogen is dissolved in liquid phase well, gas-liquid material is by after gas-liquid partition tray 8, gas-liquid separation, the liquid phase of having dissolved hydrogen enters beds 4 downwards and carries out hydrogenation reaction, and gas phase is collected and drawn reactor below gas-liquid partition tray 8.
For further illustrating the solution of the present invention, enumerate following examples:
Embodiment 1
Reactor adopts structure as shown in Figure 1.Two-phase hydrogenation reactor adopts two beds, reactor inlet and catalyst bed interlayer arrange molten hydrogen storage equipment, liquid channel setting falls in close reactor wall one side, the total actual internal area that falls liquid passage is 1.0 times of reactor feed pipe actual internal area, fall at the bottom of liquid passage along and gas-liquid partition tray face between actual internal area be 1.2 times of reactor feed pipe actual internal area.On gas-liquid partition tray, arrange and there is the suction type gas-liquid allotter of blister configuration, at the bottom of gas-liquid allotter bubble-cap along being to fall at the bottom of liquid passage along 2.0 times apart from gas-liquid partition tray face height apart from gas-liquid partition tray face height.
Test is used feedstock property in table 1.Two-phase hydrogenation reactor adopts identical catalyzer, and catalyst property is in table 2.Two-phase hydrogenation device reaction condition and generation oil nature are in table 3.
Comparative example
The same embodiment of raw material of two-phase hydrogenation device, the operating method that adopts turning oil and raw material to mix molten hydrogen outside reactor.
Table 1 stock oil character
| Oil property | Two-phase hydrogenation device raw material |
| Density (20 ℃)/gcm -3 | 0.8378 |
| Boiling range scope/℃ | 159～348 |
| Sulphur/μ gg -1 | 5798 |
| Nitrogen/μ gg -1 | 123 |
Table 2 catalyzer physico-chemical property
| Project | Data |
| Catalyst activity component | Mo、Ni、W |
| Active component content (in oxide weight), % | 29 |
| Carrier | Aluminum oxide |
| Shape | Trifolium |
| Diameter | 3.1 |
| Pore volume/mLg -1 | 0.41 |
| Specific surface area/m2g -1 | 235 |
Table 3 hydrofining technology condition
| Processing condition | Embodiment | Comparative example |
| Reaction pressure/MPa | 4.0 | 4.0 |
| Temperature of reaction/℃ | 360 | 360 |
| Two-phase hydrogenation charge ratio | 2:1* | 2:1* |
| Hydrogen to oil volume ratio | ? | ? |
| Volume space velocity/h -1(fresh feed relatively) | 1.5 | 1.5 |
| Generate oil nature: | ? | ? |
| ?S，μg/g | 14.9 | 28.6 |
| ?N，μg/g | 4.7 | 11.7 |
| Boiling range scope, ℃ | 152～343 | 154～345 |
* two-phase hydrogenation reactor is discharged the volume ratio of liquid phase internal circulating load and the fresh feed of two-phase hydrogenation device.
Claims (10)
1. a two-phase hydrogenation reactor, arranges at least one beds in two-phase hydrogenation reactor, adopt the operating method of upper feeding bottom discharge, it is characterized in that: on the top of at least one beds, molten hydrogen storage equipment is set; Molten hydrogen storage equipment comprises liquid phase catch tray, falls liquid passage and gas-liquid partition tray, and liquid phase catch tray is arranged on gas-liquid partition tray top, and hydrogen make-up entrance is set between liquid phase catch tray and gas-liquid partition tray; Gas-liquid allotter is set on gas-liquid partition tray, falls between liquid passage and gas-liquid partition tray and have gap, the upper end in gap is lower than the upper end gas-liquid entrance of gas-liquid allotter on gas-liquid partition tray; Between gas-liquid partition tray and the beds of bottom, gas-liquid separation space is set, and the relief outlet of excess hydrogen is set.
2. reactor according to claim 1, is characterized in that: liquid phase catch tray and fall liquid passage and be connected, liquid phase catch tray is collected the liquid phase that reactor top flows down, and then guides on gas-liquid partition tray by falling liquid passage.
3. reactor according to claim 1, is characterized in that: fall liquid passage at least one, fall liquid channel setting and pressing close to reactor wall one side, or be arranged in the middle of reactor; The total actual internal area that falls liquid passage is 1.0～2.0 times of reactor feed pipe actual internal area, preferably 1.0～1.2 times.
4. according to the reactor described in claim 1 or 3, it is characterized in that: fall at the bottom of liquid passage along and gas-liquid partition tray face between actual internal area be 1.0～2.0 times of reactor feed pipe actual internal area, preferably 1.1～1.5 times.
5. reactor according to claim 1, is characterized in that: gas-liquid allotter is set on gas-liquid partition tray, and gas-liquid allotter is suction type gas-liquid allotter, overflow type gas-liquid allotter or mixed type gas-liquid allotter; Liquid level when suction occurs for suction type gas-liquid allotter and mixed type gas-liquid allotter is higher than falling edge at the bottom of liquid passage, and the liquid level when overflow of overflow type gas-liquid allotter liquid phase is higher than falling edge at the bottom of liquid passage.
6. reactor according to claim 1, it is characterized in that: the gas-liquid allotter arranging on gas-liquid partition tray is the suction type gas-liquid allotter with blister configuration, at the bottom of gas-liquid allotter bubble-cap, along being to fall at the bottom of liquid passage along apart from 1.2～2.5 times of gas-liquid partition tray face height apart from gas-liquid partition tray face height, be preferably 1.5～2.0 times.
7. reactor according to claim 1, is characterized in that: hydrogen make-up entrance and excess hydrogen relief outlet are arranged on the wall of reactor.
8. a two-phase hydrogenation method, it is characterized in that right to use requires the two-phase hydrogenation reactor described in 1 to 7 arbitrary claim, be greater than any distillate of 120 ℃ as raw material, under hydroconversion condition take boiling range, carry out two-phase hydrogenation reaction, reaction liquid phase effluent part loops back reactor.
9. method according to claim 8, is characterized in that: the temperature of reaction of two-phase hydrogenation method is 100 ~ 400 ℃, is preferably 260 ~ 380 ℃; Reaction pressure is 1.5 ~ 8.0MPa, is preferably 2.0 ~ 6.0MPa; Volume space velocity is 0.6 ~ 5.0h
-1, be preferably 1.0 ~ 2.5h
-1; Turning oil and fresh feed volume mixture volume ratio are 0.5:1 ~ 6.0:1, preferably 1:1 ~ 3:1; The supplementary amounts of hydrogen of the molten hydrogen storage equipment of catalyst bed interlayer is pressed gas-liquid volume ratio 2:1 ~ 100:1, preferably 5:1 ~ 50:1.
10. method according to claim 8, it is characterized in that: the hydrogenation catalyst using in two-phase hydrogenation method is hydrotreating catalyst, wherein the active metal component of catalyzer is one or more in nickel, cobalt, molybdenum or tungsten, catalyzer carries out sulfidizing before use, and active metal component is converted into sulphided state; Catalyzer composition comprises by weight percentage: the oxide compound of nickel or cobalt is 0.5% ~ 10%, and the oxide compound of molybdenum or tungsten is 1% ~ 35%.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109985573A (en) * | 2017-12-29 | 2019-07-09 | 中国石油化工股份有限公司 | A kind of hydrogenator improving even in liquid phase degree |
| CN111068589A (en) * | 2018-10-22 | 2020-04-28 | 中国石油化工股份有限公司 | Liquid-phase hydrogenation system and liquid-phase hydrogenation method |
| CN115591483A (en) * | 2022-12-15 | 2023-01-13 | 东营市俊源石油技术开发有限公司（Cn） | Food-grade white oil hydrogenation preparation device |
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| CN109985573A (en) * | 2017-12-29 | 2019-07-09 | 中国石油化工股份有限公司 | A kind of hydrogenator improving even in liquid phase degree |
| CN109985573B (en) * | 2017-12-29 | 2021-08-31 | 中国石油化工股份有限公司 | Hydrogenation reactor for improving liquid phase uniformity |
| CN111068589A (en) * | 2018-10-22 | 2020-04-28 | 中国石油化工股份有限公司 | Liquid-phase hydrogenation system and liquid-phase hydrogenation method |
| CN115591483A (en) * | 2022-12-15 | 2023-01-13 | 东营市俊源石油技术开发有限公司（Cn） | Food-grade white oil hydrogenation preparation device |
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