CN102311794A - Diesel hydrogenation method - Google Patents
Diesel hydrogenation method Download PDFInfo
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Abstract
The invention discloses a diesel hydrogenation method, which comprises: reacting a diesel raw material in a conventional liquid-phase circulating hydrogenation reactor, and subjecting the efflux to gas-liquid separation; after hydrogen dissolved in a liquid phase is saturated, delivering the liquid phase to a liquid phase circulating hydrogenation reactor for reaction; and after liquid-phase circulating oil passes through a hydrogen sulfide removal reactor, circulating the liquid-phase circulating oil to the entrance of a liquid phase hydrogenation reactor. In the method, the raw material oil is pretreated by gas-phase circulating hydrogenation, the sulfur content in the generated oil is reduced to 500 mu g/g; and after a liquid-phase hydrogenation reaction, the hydrogen sulfide removal content in the circulating oil is reduced; and after hydrogen sulfide is removed from the circulating oil by absorption, the hydrogen sulfide content can be reduced to below 100 mu g/g, a sulfur-containing environment required by a catalyst is maintained, the activity of the catalyst is not inhibited, and thus, smooth deep removal of aromatics and deep desulfuration reaction in the liquid-phase hydrogenation reactor are promoted.
Description
Technical field
The present invention relates to a kind of hydrocarbon hydroprocessing technique, the improving one's methods of a kind of specifically diesel oil liquid phase circulation hydrogen addition technology.
Background technology
The raising of Along with people's environmental consciousness and the increasingly stringent of environmental regulation are produced and the use fuel for cleaning vehicle more and more becomes a kind of development trend.And for the cleaning of diesel oil, desulfurization and to take off aromatic hydrocarbons be its key that cleans.
In traditional hydrotreatment, need hydrogen is transformed into liquid phase from vapor phase, in liquid phase it can be on catalyst surface with petroleum hydrocarbon in impurity such as sulfocompound react.Through using very a large amount of hydrogen and oil circulationly realizing this point through beds.Oil passes through beds with hydrogen, and absorption of hydrogen goes into to be distributed in the film of oil of catalyst surface.Because the requirement of hydrogen maybe be bigger, so reactor drum is very large.In addition, in the conventional reactors system, be difficult to the controlling reactor temperature, can be through the feeding temperature of oil in the controlling reactor and hydrogen, but the temperature of inside reactor then the cold hydrogen of needs regulate.And liquid phase circulation hydrogen addition technology solves these problems, and in liquid phase circulation hydrogenation technique, hydrogen is dissolved in the raw oil through mixing the hydrogen device earlier; Get into reactor drum again and react, gas phase does not circulate, and the liquid phase elute partly loops back reactor drum; Like this, make that the liquid phase hydrogenation reactor size is less, practice thrift cost; Simultaneously, need not to inject cold hydrogen in the reaction process.Because liquid phase circulation hydrogenator size is less; Be normally used for diesel hydrotreating unit and transform, at liquid phase circulation hydrogenation pretreatment reaction device of the anterior increase of conventional gas phase circulation hydrogenator, but simultaneously; There is a problem in liquid phase circulation hydrogenation; Being raw oil continues in oil, to circulate through the hydrogen sulfide that generates behind the hydrogenation, causes in the turning oil hydrogen sulfide content higher, is unfavorable for that deep desulfuration, aromatic hydrocarbons saturated reaction carry out.
CN200680018017.3 discloses a kind of liquid phase circulation method of hydrotreating, and the hydrogen sulfide in this patent in the turning oil can't remove, to deep desulfuration, take off virtue considerable influence is arranged.
Summary of the invention
Influence the problem that desulphurization reaction carries out to hydrogen sulfide content in the existing liquid phase circulation hydrogen addition technology liquid phase is too high, the invention provides a kind of improved diesel oil hydrogenation process method.
Diesel oil hydrogenation process method of the present invention comprises following content:
(1) diesel raw material is mixed with hydrogen and through after the process furnace heating, is got into first reactor drum and react, and to remove most of sulfocompound, said first reactor drum is a gas phase circulation hydrogenator;
(2) reaction effluent of step (1) gets into gas-liquid separation device, and the gained gas phase loops back first reactor drum behind washing hydrogen sulfide;
(3) liquid phase that obtains of step (2) gets into gas liquid mixer, behind the saturated dissolved hydrogen, gets into second reactor drum and reacts, and with deep desulfuration, take off aromatic hydrocarbons, said second reactor drum is a liquid phase circulation hydrogenator;
(4) part in the reaction effluent that obtains of step (3) gets into the depriving hydrogen sulphide reactor drum, behind adsorbing and removing hydrogen sulfide, loops back second reactor inlet.
According to diesel oil hydrogenation process method provided by the invention, the another part in the reaction effluent that step (3) obtains directly goes out device as the clean diesel product.
Depriving hydrogen sulphide reactor drum described in the step (4) can comprise single reactor drum, also can comprise two reactor drums of parallel connection.After the adsorbents adsorb in one of them adsorptive reactor is saturated, promptly switch and use another adsorptive reactor, the reactor drum of saturated absorption carries out the regenerative operation of sorbent material.
In the diesel oil hydrogenation process method of the present invention; Described gas liquid mixer can be selected static mixer or dynamic mixer; The different shapes hybrid element of static mixer through being provided with in the mixing tank; Mass-transfer efficiency between the fluid is improved greatly, static mixers such as the SV type of static mixing implement body such as domestic-developed, SL type, SH type, SX type, SK type, static mixers such as the ISG type of external exploitation, SMV type.The moving member that dynamic mixer is provided with through mixing apparatus improves the mass-transfer efficiency between the fluid, and is concrete like star gear shape mixing tank, sound gear ring shape mixing tank, crescent moon trough mixer or ball-and-socket type mixing tank etc.
In the diesel oil hydrogenation process method of the present invention, first reactor drum (being gas phase circulation hydrogenator) and second reactor drum (being liquid phase circulation hydrogenator) can use identical or different Hydrobon catalyst, preferably use different Hydrobon catalysts.Hydrobon catalyst can use the commercially available prod as required, also can be by the conventional knowledge preparation in this area.When using different Hydrobon catalysts, preferably use the higher relatively Hydrobon catalyst of hydrogenation activity at second reaction zone, first reaction zone uses desulphurizing activated higher relatively Hydrobon catalyst.In the depriving hydrogen sulphide reactor drum behind second reactor drum adsorption desulfurize hydrogen catalyst is housed.The selectivity of Hydrobon catalyst is main relevant with contained active metal component; In general it is higher that active metal component contains the denitrification activity and the saturated performance of aromatic hydrocarbons of Hydrobon catalyst of W and/or Ni, and active metal component contains Hydrobon catalyst desulphurizing activated higher of Mo and/or Co.Adsorbing and removing hydrogen sulfide catalyzer can use the commercially available prod as required, also can be by the conventional knowledge preparation in this area.Usually select alkaline-earth metal catalyst for use.
In the diesel oil hydrogenation process method of the present invention, the operational condition that first reactor drum adopts is following: 280 ℃~400 ℃ of temperature of reaction, preferred 300 ℃~380 ℃, reaction pressure 3.0MPa~10.0MPa, preferred 4.0MPa~8.0MPa, volume space velocity 1.0h during liquid
-1~6.0h
-1, preferred 1.5h
-1~4.0h
-1, hydrogen to oil volume ratio 100~1000, preferred 400~800.The operational condition of second reaction zone is specific as follows: 300 ℃~420 ℃ of temperature of reaction, preferred 320 ℃~400 ℃, reaction pressure 3.0MPa~10.0MPa, preferred 4.0MPa~8.0MPa, volume space velocity 1.0h during liquid
-1~6.0h
-1, preferred 1.5h
-1~4.0h
-1The operational condition of depriving hydrogen sulphide reactor drum is specific as follows: 280 ℃~400 ℃ of temperature of reaction, preferred 300 ℃~380 ℃, reaction pressure 3.0MPa~10.0MPa, preferred 4.0MPa~8.0MPa, volume space velocity 0.5h during liquid
-1~6.0h
-1, preferred 1.0h
-1~3.0h
-1Wherein volume space velocity can be the same or different during the liquid in differential responses district, and temperature of reaction can be the same or different.Actual conditions can require to confirm according to feedstock property and quality product.
In the present invention; Described " gas phase circulation " refers in the fixed bed hydrogenation technological process of routine; For the temperature of reaction of control catalyst bed with avoid the catalyst carbon deposit inactivation, adopt bigger hydrogen to oil volume ratio usually, after hydrogenation reaction is accomplished, must have a large amount of hydrogen more than needed; These hydrogen more than needed mix the hydrogen feed of continued as reaction with new hydrogen usually after the circulating hydrogen compressor supercharging, promptly hydrogen recycle is used.
The present invention is added in the liquid phase hydrogenator that circulates conventional gas phase circulation hydrogenator and forms associated plant at the back, to carry out deep desulfuration, to take off virtue, adopts the hydrogen sulfide in the adsorbing and removing turning oil simultaneously.The conventional gas phase circulation hydrogenator of front carries out pre-treatment to raw oil, makes the sulphur content that generates in the oil reduce to below the 500 μ g/g, and the raw materials quality of liquid phase hydrogenation reactor processing improves like this; Through the corresponding reduction of hydrogen sulfide content in the turning oil of liquid-phase hydrogenatin reaction back, after further removing hydrogen sulfide through the depriving hydrogen sulphide reactor drum, the hydrogen sulfide content in the turning oil is reduced to less than 100 μ g/g.Such hydrogen sulfide content can be ignored reaction of the deep hydrodesulfurizationof in the liquid phase circulation hydrogenator and hydrogenation aromatics-removing reaction inhibition, can make that like this deep hydrodesulfurizationof of diesel oil reaction is able to carry out smoothly in liquid phase circulation hydrogenator.
Description of drawings
Fig. 1 is the principle process synoptic diagram of diesel oil hydrogenation process method of the present invention.
Embodiment
In the diesel oil hydrogenation technology of the present invention, the hydrogenation catalyst of employing be meant have hydrogenating desulfurization, the non-noble metal hydrogenation catalyst of hydrodenitrification, the saturated function of aromatic hydrocarbons, the function of catalyzer can stress some aspect.This non-precious metal catalyst generally exists with the oxidation state form before use, need carry out prevulcanized, makes non-noble metal oxide be converted into sulfide and just has reactive behavior, and therefore, non-precious metal catalyst in use will keep sulphided state.
The used hydrogenation catalyst of the present invention can adopt conventional diesel oil hydrofining catalyst, is active ingredient with VI B family and/or group VIII metal generally, is carrier with aluminum oxide or siliceous aluminum oxide.Weight with catalyzer is benchmark, and the group VIB metal content is counted 8wt%~28wt% with oxide compound, and group VIII metal content is counted 2wt%~15wt% with oxide compound, and its character is following: specific surface is 100~650m
2/ g, pore volume are 0.15~0.8ml/g.The group VIB metal is generally Mo and/or W, and group VIII metal is generally Co and/or Ni.Employed sorbent material can use the commercially available prod as required in the depriving hydrogen sulphide reactor drum of the present invention, also can be by the conventional knowledge preparation in this area.Generally be active ingredient with the earth alkali metal, carrier can be natural inorganic clay or gac, and wherein the content of alkaline earth metal cpds is 50wt%~90wt%, and natural inorganic clay or gac content are 10wt%~50wt%.
Principle technical process of the present invention is as shown in Figure 1, diesel raw material 1 through after the heat exchange with after hydrogen from pipeline 2 mixes, and flow into first reactor drum 3, in the presence of the sulphided state Hydrobon catalyst, carry out hydrogenation reaction downwards; Reaction effluent gets into gas-liquid separator 4 and carries out gas-liquid separation, and gas phase loops back first reactor drum 3 through pipeline 2, and liquid phase gets into through pipeline 5 and mixes hydrogen jar 6 and new hydrogen 7 thorough mixing, and saturated dissolved hydrogen is after pipeline 8 gets into second reactor drum 9; Reaction mass part after 9 reactions of second reactor drum gets into depriving hydrogen sulphide reactor drum 12 through pipeline 11; Remove the hydrogen sulfide that is dissolved in the oil; Elute is got back to through recycle pump 13 circulations and through pipeline 14 and pipeline 5 and is mixed hydrogen jar 6, and another part elute directly removes the product jar by pipeline 10.
Through embodiment the present invention program and effect are described below.
Adopt flow process of the present invention such as Fig. 1.Use nickel-tungsten-molybdenum type Hydrobon catalyst in following examples, the composition and the character of catalyzer are seen table 1, and used feedstock property is seen table 2, and embodiment 1~4 used processing condition are listed in table 3, and the evaluation result of embodiment 1~4 is seen table 4.
The composition and the main character of table 1 embodiment catalyst system therefor
Project | Catalyst A | Catalyst B |
Chemical constitution, quality % | ||
MoO 3 | 6.2 | 19.8 |
NiO | 12.3 | - |
CoO | - | 3.7 |
WO 3 | 15.2 | - |
Carrier | Aluminum oxide | Aluminum oxide |
Physico-chemical property | ||
Pore volume, ml/g | 0.45 | 0.41 |
Specific surface area, m 2/g | 265 | 206 |
Table 2 raw oil character
Raw oil | Raw oil |
Density, g/cm 3 | 0.8569 |
Boiling range, ℃ | 199~379 |
Sulphur content, μ g/g | 8800 |
Nitrogen content, μ g/g | 316 |
Aromaticity content, wt% | 21.5 |
Table 3 embodiment 1~4 operational condition that adopts
Table 4 embodiment 1~4 evaluation result
|
|
|
|
|
Sulphur content, μ g/g | 348 | 106 | 136 | 8 |
Aromaticity content, wt% | 18.6 | 17.3 | 17.5 | 9.2 |
Claims (11)
1. diesel oil hydrogenation process method may further comprise the steps:
(1) diesel raw material is mixed with hydrogen and through after the process furnace heating, is got into first reactor drum and react, and said first reactor drum is a gas phase circulation hydrogenator;
(2) reaction effluent that obtains of step (1) gets into gas-liquid separation device, and the gained gas phase loops back first reactor drum behind washing hydrogen sulfide;
(3) liquid phase that obtains of step (2) gets into gas liquid mixer, behind the saturated dissolved hydrogen, gets into second reactor drum and reacts, and said second reactor drum is a liquid phase circulation hydrogenator;
(4) part in the reaction effluent that obtains of step (3) gets into the depriving hydrogen sulphide reactor drum, behind adsorbing and removing hydrogen sulfide, loops back second reactor inlet.
2. according to the described process method of claim 1, it is characterized in that the depriving hydrogen sulphide reactor drum described in the step (4) comprises a reactor drum or comprises two reactor drums of parallel connection.
3. according to the described process method of claim 2; It is characterized in that; Described depriving hydrogen sulphide reactor drum comprises two reactor drums; After the adsorbents adsorb in one of them adsorptive reactor is saturated, promptly switch and use another adsorptive reactor, the reactor drum of saturated absorption carries out the regenerative operation of sorbent material.
4. according to the described process method of claim 1, it is characterized in that first reactor drum and second reactor drum use identical or different Hydrobon catalyst.
5. according to the described process method of claim 4; It is characterized in that; First reactor drum uses different Hydrobon catalysts with second reactor drum; First reactor drum uses desulphurizing activated higher relatively Hydrobon catalyst, and second reactor drum uses the higher relatively Hydrobon catalyst of hydrogenation activity.
6. according to claim 4 or 5 described process methodes; It is characterized in that; Consisting of of described Hydrobon catalyst: the weight with catalyzer is benchmark, and the group VIB metal content is counted 8wt%~28wt% with oxide compound, and group VIII metal content is counted 2wt%~15wt% with oxide compound; Its character is following: specific surface is 100~650m
2/ g, pore volume are 0.15~0.8ml/g.
7. according to the described process method of claim 1, it is characterized in that the processing condition of said first reactor drum are: 280 ℃~400 ℃ of temperature of reaction, reaction pressure 3.0MPa~10.0MPa, volume space velocity 1.0h during liquid
-1~6.0h
-1, hydrogen to oil volume ratio 100~1000; The processing condition of second reaction zone are: 300 ℃~420 ℃ of temperature of reaction, reaction pressure 3.0MPa~10.0MPa, volume space velocity 1.0h during liquid
-1~6.0h
-1The processing condition of depriving hydrogen sulphide reactor drum are: 280 ℃~400 ℃ of temperature of reaction, reaction pressure 3.0MPa~10.0MPa, volume space velocity 0.5h during liquid
-1~6.0h
-1
8. according to the described process method of claim 7, it is characterized in that the processing condition of said first reactor drum are 300 ℃~380 ℃ of temperature of reaction, reaction pressure 4.0MPa~8.0MPa, volume space velocity 1.5h during liquid
-1~4.0h
-1, hydrogen to oil volume ratio 400~800; The processing condition of second reaction zone are 320 ℃~400 ℃ of temperature of reaction, reaction pressure 4.0MPa~8.0MPa, volume space velocity 1.5h during liquid
-1~4.0h
-1The processing condition of depriving hydrogen sulphide reactor drum are 300 ℃~380 ℃ of temperature of reaction, reaction pressure 4.0MPa~8.0MPa, volume space velocity 1.0h during liquid
-1~3.0h
-1
9. according to the described process method of claim 1; It is characterized in that; The adsorption desulfurize hydrogen catalyst that uses in the described depriving hydrogen sulphide reactor drum is active ingredient with earth alkali metal; Carrier is natural inorganic clay or gac, and wherein the content of alkaline earth metal cpds is 50wt%~90wt%, and natural inorganic clay or gac content are 10wt%~50wt%.
10. according to the described process method of claim 1, it is characterized in that the gas liquid mixer described in the step (3) is selected static mixer or dynamic mixer.
11., it is characterized in that described static mixer is SV type, SL type, SH type, SX type, SK type, ISG type or SMV type static mixer according to the described process method of claim 10; Described dynamic mixer is star gear shape mixing tank, sound gear ring shape mixing tank, crescent moon trough mixer or ball-and-socket type mixing tank.
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CN109679682A (en) * | 2017-10-19 | 2019-04-26 | 中国石油化工股份有限公司 | A kind of molten hydrogen storage equipment and molten hydrogen methods |
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CN114433058B (en) * | 2020-10-31 | 2023-11-07 | 中国石油化工股份有限公司 | Liquid phase hydrogenation catalyst composition |
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