CN104178206A - Liquid-solid two-phase hydrogenation process and device thereof - Google Patents
Liquid-solid two-phase hydrogenation process and device thereof Download PDFInfo
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- CN104178206A CN104178206A CN201310206879.0A CN201310206879A CN104178206A CN 104178206 A CN104178206 A CN 104178206A CN 201310206879 A CN201310206879 A CN 201310206879A CN 104178206 A CN104178206 A CN 104178206A
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Abstract
The invention discloses a liquid-solid two-phase hydrogenation process and a device thereof. Hydrogen, fresh raw oil and circulating oil are mixed into a mixture in a first mixing dissolver, and the mixture flows into the a first reactor; gas is separated at the top of the first reactor; the liquid reacts with a catalyst through contact; part of a reaction effluent is used as circulating oil I, and the other part of the reaction effluent enters a second reactor, and is subjected to stripping by a steam stripping medium, mixed with hydrogen and discharged; the liquid with dissolved hydrogen contacts with a catalyst for reaction; the reaction effluent is subjected to gas-liquid separation; and part of a liquid product is used as the product, and the other part is used as circulating oil II. The process reduces the investment and operation cost.
Description
Technical field
The present invention relates to hydrocarbon oil hydrogenation technology, particularly a kind of liquid-solid two-phase hydrogenation technique and device thereof
Background technology
The sustainable development of world economy at present and the increasingly stringent of environmental regulation, need to produce a large amount of light clean fuels, and these all require existing oil Refining Technologies to improve, and produce satisfactory product with minimum cost.Along with worsening shortages and heaviness, the in poor quality of crude resources develop, catalytic cracking and coking become the important means of producing light Fuel product, but the quality product that these two kinds of techniques obtain is generally difficult to the quality index requirement that reaches strict.In light Fuel quality product system, sulphur content is most important index, how to reduce sulphur content in petroleum products and be one of most significant problems that current petroleum chemical industry faces, the cetane value of diesel product receives publicity always in addition, and its specification requirement is also more and more stricter.At present, be applied widely in Clean Fuel Production taking desulfurization and upgrading as main purpose hydrogenation technique.
Hydrogen addition technology is to improve one of conventional technology of hydrocarbon ils quality, along with global crude oil market supply is tending towards the crude oil of higher sulfur content, refinery need process the hydrocarbon ils inferior that sulfur-bearing is higher, sulphur, nitrogen, oxygen and metal impurities are removed in refining process, change its quality by the molecular structure that changes hydrocarbon ils, thereby make various products meet code requirement.The hydrogen that in fact hydrocarbon oil hydrogenation process participates in reaction only has the hydrogen for chemical hydrogen consumption, and traditional trickle-bed reactor hydrogen addition technology need to have excessive hydrogen to exist, and maintains the exess of H2 gas and need to use circulating hydrogen compressor.
In traditional hydrogenation technique, hydrogen need to be delivered to liquid phase from gas phase, and then co-absorbed, on the surface of catalyzer, is reacted under the effect of catalyst active center.Because hydrogenation reaction is a strong exothermal reaction, conventionally utilize a large amount of hydrogen and stock oil to take away by beds the heat that reaction produces, and in hydrogenation process the hydrogen of actual needs, be that chemical hydrogen consumption is fewer, major part is not participated in the hydrogen of reaction, is recycled to hydrogenator and continues to participate in reaction; It is the hydrogen dividing potential drop that maintains hydrocarbon oil hydrogenation reaction that tradition hydrocarbon oil hydrogenation technology adopts another major cause of excessive hydrogen, maintains higher hydrogen and divides to be pressed on thermodynamics and be conducive to hydrofining and hydrocracking reaction, suppresses to generate the condensation reaction of coke.
The hydrogen of not participating in reaction is by separator and liquid phase separation and remove after impurity, by circulating hydrogen compressor, its pressure is elevated to the required pressure of reaction and delivers to reactor and continue to participate in hydrogenation reaction.The effect of circulating hydrogen compressor is exactly the hydrogen that does not participate in hydrogenation reaction to be improved to pressure it is recycled, therefore circulating hydrogen compressor becomes requisite equipment in existing hydrogen addition technology, claim that in the industry circulating hydrogen compressor is the heart of hydrogenation unit, its importance in hydrogenation unit is general as seen.
In traditional fixed bed hydrogenation reactor, be gas, liquid, solid three-phase and deposit, gas phase is the steam of hydrogen and hydrocarbon raw material, and liquid phase is the hydrocarbon raw material of not vaporizing, and solid phase is catalyzer.Gas-liquid two-phase is to pass through beds with the form of drip, therefore also claims trickle-bed reactor.
In trickle-bed reactor, the stock oil of actual participation reaction is relevant with liquid hourly space velocity, and air speed has reflected the processing power of device, and industrial hope adopts larger air speed operation, but air speed is subject to the restriction of speed of response.Air speed is unusual at 0.5～10h according to catalyst activity, feedstock property, reaction depth
-1between fluctuation.The unifining process of industrial application can improve olefin saturated rate, hydrogenating desulfurization rate and hydrodenitrification rate at certain temperature of reaction condition decline low-speed at present.
The object that adopts the exess of H2 gas is strengthen mass transfer and take away the amount of heat producing because of hydrogenation reaction, circulating hydrogen compressor is as the heart of hydrogenation process, investment and process cost are all higher, in order to cancel circulating hydrogen compressor, people start to consider to utilize hydrogen supply agent to provide hydrogen source for hydrocarbon oil hydrogenation process, USP4698147 discloses and has utilized hydrogen supply agent to reduce the residence time, and after reaction, hydrogen supply agent utilizes hydrogen to regenerate, and after regeneration, recycles.In order to strengthen cracking reaction, USP4857168 discloses and has utilized hydrogen supply agent and hydrogen to provide the heavy-oil hydrogenation cracking method of hydrogen source for heavy-oil hydrogenation, and hydrogen supply agent mainly works to suppress to generate the condensation reaction of coke.
Above-mentioned improvement still needs recycle hydrogen and circulating hydrogen compressor, US6428686 has proposed a kind of two-phase hydrogenation method, hydrogen is dissolved in stock oil before reactor, recycle hydrogen and circulating hydrogen compressor are cancelled, investment and the process cost of hydrogenation unit are reduced, this technology adopts the liquid phase circulation of reaction product, improve the meltage of hydrogen, to meet the requirement to hydrogen in hydrogenation process, and take reaction heat out of, this technology is to enter hydrogenator after turning oil is mixed with stock oil and hydrogen, its shortcoming is the speed of response that the existence of a large amount of turning oil can affect fresh feed and hydrogen, because fresh feed is fiercer with hydrogen reaction in the time starting to contact with catalyzer, in turning oil, the existence of H2S has suppressed the touch opportunity of fresh feed oil and hydrogen and catalyzer, mass transfer and the speed of response of fresh feed oil and hydrogen are reduced, reduce hydrogenation effect.
Summary of the invention
The present invention proposes a kind of liquid-solid two-phase hydrogenation technique, strengthen the touch opportunity of fresh feed oil and hydrogen and catalyzer, improve mass transfer and speed of response, greatly improved transformation efficiency and the quality product of hydrogenation reaction.
A kind of liquid-solid two-phase hydrogenation technique of the present invention, it is characterized in that: hydrogen and fresh feed oil and turning oil are mixed to form mixture flow in the first mixing dissolver, mixture flow enters the first reactor, isolate after gas in the first reactor head, liquid contacts and reacts with catalyzer, the first reactor reaction effluent is through gas-liquid separation, a part is as turning oil I, another part enters the second reactor, mix with hydrogen after stripping medium stripping at the second reactor, gas is discharged from the second reactor head, the liquid of molten hydrogen contacts and reacts with catalyzer, the reaction effluent of the second reactor carries out gas-liquid separation, it is product that product liquid is made part, another part is as turning oil II.
The first described catalyst in reactor is at least divided into two beds, is provided with mixing dissolver in device between beds.
Described turning oil I is recycled to the first mixing dissolver, or turning oil I is partly recirculated to the first mixing dissolver, and another part is partly recirculated to mixing dissolver in the device between the beds of the first reactor.
Mixture flow enters reactor from the first reactor top or bottom, and reaction effluent flows out from reactor lower part or top.
Described stripping medium is at least one in steam, hydrogen, rare gas element.
Described turning oil II is recycled to the second reactor inlet, or a part is recycled to the second reactor inlet, another part be recycled to the first reactor inlet and or the first reactor catalyst bed between.
Described a kind of liquid-solid two-phase hydrogenation technique, at least removes in fresh feed oil a kind of pollutent in sulphur, nitrogen, oxygen, metallic impurity, and saturated aromatic hydrocarbons, changes the molecular structure of hydrocarbon ils.
Described fresh feed oil is the distillate of hydrocarbon ils or hydrocarbon ils, as petroleum fractions, distillate, diesel oil, deasphalted oil, residual oil, lubricating oil, liquefied coal coil and shale oil or its product.
A kind of liquid-solid two-phase hydrogenation device, comprises the first reactor, the second reactor, separator, and its spy is: the first reactor is communicated with the second reactor, and the second reactor is communicated with and is communicated with separator.
The first described reactor, comprises the first reactor shell, beds and mixing dissolver, and beds is arranged in the first reactor shell, and mixing dissolver is in device or the outer mixing dissolver of device.
The first described mixing dissolver is mixing dissolver in the outer or device of device.
The second described reactor, comprises the second reactor shell, stripping stage, beds and mixing dissolver, and stripping stage, beds and mixing dissolver are arranged in the second reactor shell.
The first described reactor and the second reactor can be arranged in a reactor.
Described the first reactor and the second reactor are provided with entrance and exit, and the first described reactor inlet and outlet are by being communicated with communicating pipe, and the second reactor was communicated with by communicating pipe.
The second described reactor outlet is communicated with by communicating pipe with the first reactor inlet.
Maximum problem of hydrogenation process is beds coking, under reaction conditions, can there is coking reaction, if there is no enough hydrogen, cracking reaction meeting causes coke to form, and is deposited on catalyst surface, and the present invention is owing to adopting turning oil circulation, it is saturated that turning oil obtains much aromatic hydrocarbons through hydrogenation, there is the function of hydrogen supply, can suppress coke and form, the life-span of extending catalyst.Compared with prior art, a kind of liquid-solid two-phase hydrogenation technique of the present invention and device thereof, the high-tension apparatuses such as circulating hydrogen compressor, high pressure heat exchanger, high-pressure air cooler and high-pressure separator are cancelled, significantly reduce investment and the process cost of hydrogenation unit, improved fresh feed oil transformation efficiency and quality product.
A kind of liquid-solid two-phase hydrogenation technique of the present invention and device thereof can be used for straight run, FCC turning oil, coker gas oil CGO, or it mixes kerosene and diesel oil hydrogenation processing, also can be used for FCC raw materials pretreatment, for new device and mild hydrocracking transformation, for the production of ULSD, for the pre-treatment of raw material or the aftertreatment of product.
Two-stage hydrogenation technique of the present invention has following advantage:
1) catalyst levels is few;
2) hydrogen loss is less;
3) lower process cost;
4) liquid yield is higher;
5) larger flexibility of operation;
6) the sulphur nitrogen content of product is very low;
7) for producing ultra-low-sulphur diesel, improvement expenses is very low.
Compared with other existing hydrogen addition technology, the present invention: can desulfurization more than 98%～99%, and hydrogen consumption is only 70%～90% of conventional trickle bed hydrogenator.
Below with brief description of the drawings the present invention, but do not limit the scope of the invention.
Brief description of the drawings
Fig. 1 is a kind of liquid-solid two-phase hydrogenation process flow sheet of the present invention.
Fig. 2 is two kinds of liquid-solid two-phase hydrogenation process flow sheets of the present invention.
Fig. 3 is three kinds of liquid-solid two-phase hydrogenation process flow sheets of the present invention
Fig. 4 is four kinds of liquid-solid two-phase hydrogenation process flow sheets of the present invention
Fig. 5 is five kinds of liquid-solid two-phase hydrogenation process flow sheets of the present invention
Fig. 6 is six kinds of liquid-solid two-phase hydrogenation process flow sheets of the present invention
Fig. 7 is seven kinds of liquid-solid two-phase hydrogenation process flow sheets of the present invention
Fig. 8 is eight kinds of liquid-solid two-phase hydrogenation process flow sheets of the present invention
In figure: 1. fresh feed oil, 2. hydrogen, 3. the first mixing dissolver, 4. the first reactor feed, 5-the first reactor, 6. turning oil I turning oil, 7. the first reactor gas, 8. the first reactor partial reaction effluent, 9. the second reactor feed, 10. the second gas reactor, 11. second reactors, 12. turning oil II, 13.. the second reactor divides reaction effluent, 14. gases, 15. separators, 16. liquid, 17,20. beds, 18,19. second mixing dissolvers, 21. stripping stages.
Embodiment
Below more detailed description, with embodiment, the present invention is described, but does not limit the scope of the invention.
As shown in Figure 1, hydrogen and fresh feed oil and turning oil are mixed to form mixture flow in the first mixing dissolver, the first mixing dissolver is the outer mixing dissolver of device, mixture flow enters the first reactor from the first reactor top, isolate after gas in the first reactor head, liquid contacts and reacts with catalyzer, the first reactor reaction effluent is through gas-liquid separation, a part is recycled to the first mixing dissolver as turning oil I, another part enters the second reactor, mix with hydrogen after stripping medium stripping at the second reactor, gas is discharged from the second reactor head, the liquid of molten hydrogen contacts and reacts with catalyzer, the reaction effluent of the second reactor carries out gas-liquid separation, product liquid is as product, also can a part be recycled to the second reactor inlet as turning oil II, the first catalyst in reactor arranges two beds, between beds, be provided with mixing dissolver in device.
As shown in Figure 2, identical with accompanying drawing 1, difference is that turning oil I is partly recirculated to the first mixing dissolver, and another part is partly recirculated to mixing dissolver in the device between the beds of the first reactor.
As shown in Figure 3, identical with accompanying drawing 2, difference is that a turning oil II part is recycled to the second reactor inlet, and another part mixes with turning oil I.
As shown in Figure 4, identical with accompanying drawing 1, difference is, the first mixing dissolver is mixing dissolver in device.
As shown in Figure 5, identical with accompanying drawing 4, difference is, turning oil I is partly recirculated to the first mixing dissolver, and another part is partly recirculated to mixing dissolver in the device between the beds of the first reactor.
As shown in Figure 6, identical with accompanying drawing 4, difference is, distinguishes and is that a turning oil II part is recycled to the second reactor inlet, and another part mixes with turning oil I.
As shown in Figure 7, identical with accompanying drawing 1, difference is, the first reactor and the second reactor are arranged in a reactor shell, there is no turning oil I, and turning oil II is recycled to the first reactor inlet.
As shown in Figure 8, identical with accompanying drawing 7, difference is, a turning oil II part is recycled to the first reactor inlet, and another part is recycled to the mixing dissolver between beds.
Described stripping medium is at least one in steam, hydrogen, rare gas element.
Described turning oil II is recycled to the second reactor inlet, or a part is recycled to the second reactor inlet, another part be recycled to the first reactor inlet and or the first reactor catalyst bed between.
Described a kind of liquid-solid two-phase hydrogenation technique, at least removes in fresh feed oil a kind of pollutent in sulphur, nitrogen, oxygen, metallic impurity, and saturated aromatic hydrocarbons, changes the molecular structure of hydrocarbon ils.
Described fresh feed oil is the distillate of hydrocarbon ils or hydrocarbon ils, as petroleum fractions, distillate, diesel oil, deasphalted oil, residual oil, lubricating oil, liquefied coal coil and shale oil or its product.
The first reactor, 6. turning oil I turning oil, 7. the first reactor gas, 8. the first reactor partial reaction effluent, 9. the second reactor feed, 10. the second gas reactor, 11. second reactors, 12. turning oil II, 13.. the second reactor divides reaction effluent, 14. gases, 15. separators, 16. liquid, 17,20. beds, 18,19. second mixing dissolvers, 21. stripping stage hydrogenators are two-stage catalytic agent bed.Hydrogen 2 is mixed to form mixture flow with fresh feed oil 1 and turning oil 6 in the first mixing dissolver 3, mixture flow 4 enters the first reactor 5, isolate after gas 7 in the first reactor head, liquid contacts and reacts with catalyzer, gas is discharged from the first reactor head, a reaction effluent part 6 is as turning oil, another part 8 directly or after step-down, remove the second reactor 11, remove the H2S in the first reaction effluent at the second reactor top segregation section, then after mixing with hydrogen, enter beds, liquid contacts and reacts with catalyzer, the second reactor head combustion gas, after the reaction effluent step-down out of the second reactor, enter light pressure separator 20 and carry out gas-liquid separation (also can draw as required a part circulates as turning oil 12), the gas 21 that light pressure separator obtains after separating obtains product after further separating with liquid 22 and goes out device.
Claims (15)
1. a liquid-solid two-phase hydrogenation technique, it is characterized in that: hydrogen and fresh feed oil and turning oil are mixed to form mixture flow in the first mixing dissolver, mixture flow enters the first reactor, isolate after gas in the first reactor head, liquid contacts and reacts with catalyzer, the first reactor reaction effluent is through gas-liquid separation, a part is as turning oil I, another part enters the second reactor, mix with hydrogen after stripping medium stripping at the second reactor, gas is discharged from the second reactor head, the liquid of molten hydrogen contacts and reacts with catalyzer, the reaction effluent of the second reactor carries out gas-liquid separation, product liquid part is as product, another part is as turning oil II.
2. according to a kind of liquid-solid two-phase hydrogenation technique claimed in claim 1, it is characterized in that: the first catalyst in reactor is at least divided into two beds, between beds, be provided with mixing dissolver in device.
3. according to a kind of liquid-solid two-phase hydrogenation technique claimed in claim 1, it is characterized in that: described turning oil I is recycled to the first mixing dissolver, or turning oil I is partly recirculated to the first mixing dissolver, another part is partly recirculated to mixing dissolver in the device between the beds of the first reactor.
4. according to a kind of liquid-solid two-phase hydrogenation technique claimed in claim 1, it is characterized in that: mixture flow enters reactor from the first reactor top or bottom, reaction effluent flows out from reactor lower part or top.
5. according to a kind of liquid-solid two-phase hydrogenation technique claimed in claim 1, it is characterized in that: described turning oil II is recycled to the second reactor inlet, or a part is recycled to the second reactor inlet, another part be recycled to the first reactor inlet and or the first reactor catalyst bed between.
6. according to a kind of liquid-solid two-phase hydrogenation technique claimed in claim 1, it is characterized in that: described stripping medium is at least one in steam, hydrogen, rare gas element, preferably hydrogen.
7. according to a kind of liquid-solid two-phase hydrogenation technique claimed in claim 1, it is characterized in that: at least remove in fresh feed oil a kind of pollutent in sulphur, nitrogen, oxygen, metallic impurity, and saturated aromatic hydrocarbons, change the molecular structure of hydrocarbon ils.
8. according to a kind of liquid-solid two-phase hydrogenation technique claimed in claim 1, it is characterized in that: the distillate that described fresh feed oil is hydrocarbon ils or hydrocarbon ils, as petroleum fractions, distillate, diesel oil, deasphalted oil, residual oil, lubricating oil, liquefied coal coil and shale oil or its product.
9. a liquid-solid two-phase hydrogenation device, comprise the first reactor, the second reactor, separator, its spy is: the first reactor is communicated with the second reactor, and the second reactor is communicated with and is communicated with separator, and the first reactor and the second reactor are provided with entrance and exit.
10. according to a kind of liquid-solid two-phase hydrogenation device claimed in claim 9, it is characterized in that: the first described reactor, comprise the first reactor shell, beds and mixing dissolver, beds is arranged in the first reactor shell, and mixing dissolver is in device or the outer mixing dissolver of device.
11. according to a kind of liquid-solid two-phase hydrogenation device claimed in claim 9, it is characterized in that: the first described mixing dissolver is mixing dissolver in the outer or device of device.
12. according to a kind of liquid-solid two-phase hydrogenation device claimed in claim 9, it is characterized in that: the second described reactor, comprise the second reactor shell, stripping stage, beds and mixing dissolver, stripping stage, beds and mixing dissolver are arranged in the second reactor shell.
13. according to a kind of liquid-solid two-phase hydrogenation device claimed in claim 9, it is characterized in that: the first described reactor and the second reactor can be arranged in a reactor.
14. according to a kind of liquid-solid two-phase hydrogenation device claimed in claim 9, it is characterized in that: the first described reactor inlet and outlet are by being communicated with communicating pipe, and the second reactor was communicated with by communicating pipe.
15. according to a kind of liquid-solid two-phase hydrogenation device claimed in claim 9, it is characterized in that: the second described reactor outlet is communicated with by communicating pipe with the first reactor inlet.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN116199293A (en) * | 2021-11-30 | 2023-06-02 | 中国石油化工股份有限公司 | Reinforced negative pressure gas stripping device and gas stripping method thereof |
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- 2013-05-22 CN CN201310206879.0A patent/CN104178206A/en active Pending
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| CN101787305A (en) * | 2009-01-23 | 2010-07-28 | 中国石油化工股份有限公司 | Method of liquid phase circulation hydrotreatment and reaction system |
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| CN116199293A (en) * | 2021-11-30 | 2023-06-02 | 中国石油化工股份有限公司 | Reinforced negative pressure gas stripping device and gas stripping method thereof |
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Application publication date: 20141203 |