CN103773499B - A kind of hydrorefining petroleum waxes method - Google Patents
A kind of hydrorefining petroleum waxes method Download PDFInfo
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- CN103773499B CN103773499B CN201210408517.5A CN201210408517A CN103773499B CN 103773499 B CN103773499 B CN 103773499B CN 201210408517 A CN201210408517 A CN 201210408517A CN 103773499 B CN103773499 B CN 103773499B
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Abstract
The invention discloses a kind of hydrorefining petroleum waxes method, comprise: petroleum wax raw material and hydrogen are in a counter-current fashion by gas-liquid counter current hydrogenator, after non-noble metal hydrogenation catalyst for refining contact reacts wherein, gas phase is discharged it from reactor head and is used, liquid phase stream effluent directly enters the second hydroconversion reaction zone, successively through hydrogenation protecting reaction zone and main hydrofining reaction district, contact with reduced form Hydrobon catalyst with hydrogenation protecting agent wherein successively and carry out hydrogenation reaction, hydrotreated product is after being separated, gas phase loops back gas-liquid counter current hydrogenator, liquid phase is the petroleum paraffin product after refining.High-pressure separator and gas stripping column can be saved in the inventive method between two hydrogenators, simplify technical process, save facility investment, improve the effect of hydrogenation removing impurities matter and aromatic saturation.
Description
Technical field
The present invention relates to a kind of hydrorefining petroleum waxes method, particularly adopt gas-liquid counter current reactor and conventional hydro combination of reactors to carry out the hydrofinishing process of petroleum wax hydrotreatment.
Background technology
At present, in world wide petroleum resources particularly paraffinic crude resource is day by day well sold and in short supply.Along with the continuous growth to paraffin demand, refinery has to expand the raw material range of producing petroleum wax, adopts and expands cut or use the measures such as non-paraffinic crude to carry out supplementary raw material sources.But according to existing complete processing, the product obtained can not meet specification of quality.In addition, along with the continuous proposition of environmental regulation and perfect, the raising of petroleum wax standard also makes existing technological operation face stricter challenge.
The Main Means that current petroleum wax is refined is hydrofining.To remove in wax material the heteroatoms such as sulphur, nitrogen by hydrofining and carry out aromatic hydrogenation saturated, finally make product meet harsh product performance index.On the basis of traditional one stage hydrofining, there have been developed the techniques such as one section series hydrogenation refining.In these hydrogenation techniques, adopt non-precious metal catalyst hydrogenation.Hydrogenation due to petroleum wax is subject to the restriction not allowing cracking, and temperature of reaction can not superelevation, which limits this kind of hydrorefined quality product.
On one-stage hydrogenation Process ba-sis, researched and developed two-section hydrotreating technique further again, wherein second segment adopts highly active noble metal catalyst, but Typical precious metal catalyzer can not bear sulfide.Before material enters second segment, need the hydrogen sulfide stripping in first paragraph hydrofining wax product.Current common way adopts water vapour stripping and drying process.But this process need will make material elder generation by high pressure relief to normal pressure and negative pressure, then boost to high pressure, and process energy consumption is larger.
In the hydro-refining unit of routine, gas-liquid is downward and flows to into reactor.The H generated in reaction process
2s, NH
3deng gaseous impurities competitive adsorption on the active centre of catalyst surface, restraining effect is produced to hydrogenation reaction.In addition, H
2s, NH
3deng gaseous impurities and C
1, C
2enter in hydrogen Deng micro-molecular gas hydro carbons, cause hydrogen dividing potential drop to reduce, affect the effect of hydrogenation removing impurities matter and aromatic saturation.
Hydrogenator adopts gas-liquid counter current operation can avoid above-mentioned shortcoming, can remove most of H in time
2s, NH
3deng gaseous impurities, increase hydrogen dividing potential drop, promote hydrogenation reaction, be therefore subject to the attention of researchist.In gas-liquid counter current hydrogenator, liquid stream enters from the top of reactor, and flow out from the bottom of reactor, hydrogen then enters from the bottom of reactor, flows out from top.Gas-liquid by beds, realizes hydrogenation reaction in a counter-current fashion.The principal element of current restriction gas-liquid counter current hydrogenator development is that beds easily produces liquid flooding, and the turndown ratio of reactor is little.
In hydrorefining petroleum waxes process, the alkane accounting for material most does not react substantially, the main reaction participated in be the less impurity of content, consumption hydrogen is few, and beds temperature rise is little.Temperature is easy to control, and gas yield is also little.The gas flow in each portion of reactor is close, therefore adopts counter-current reactor more satisfactory.
Summary of the invention
For the deficiencies in the prior art, the invention provides a kind of new hydrorefining petroleum waxes method, described method adopts two reactors in series modes, and the method can deep desulfuration denitrogenation and aromatic saturation, effectively improves purified product stability and energy consumption is little.
The invention provides a kind of hydrorefining petroleum waxes method, comprise following content: petroleum wax raw material and hydrogen are in a counter-current fashion by gas-liquid counter current hydrogenator, after non-noble metal hydrogenation catalyst for refining contact reacts wherein, gas phase is discharged it from reactor head and is used, liquid phase stream effluent directly enters the second hydroconversion reaction zone, successively through hydrogenation protecting reaction zone and main hydrofining reaction district, contact with reductibility Hydrobon catalyst with hydrogenation protecting agent wherein successively and carry out hydrogenation reaction, hydrotreated product is after being separated, gas phase loops back gas-liquid counter current hydrogenator, liquid phase is the petroleum paraffin product after refining.
In the inventive method; described gas-liquid counter current hydrogenator comprises upper cover from top to bottom successively, distributes Yi Fan district, hydroconversion reaction zone, air lift district and lower cover; described air lift district increases gradually to hydroconversion reaction zone diameter; upper cover is provided with feed(raw material)inlet and gas discharge outlet; lower cover is provided with liquid phase relief outlet and hydrogen inlet; the protective material of described distribution Yi Fan district filling inert ceramic balls or low reactivity; described hydroconversion reaction zone filling base metal catalyst for hydrorefining pertroleum wax, described air lift district filling open grain inert filler.
In the inventive method, gas-liquid counter current hydrogenator arranges in reactor head and distributes-Yi Fan district, mainly plays the effect of flow distribution, when producing at large load, can keep in hydrops.The stripping zone of filling open grain inert filler is set below hydroconversion reaction zone, consider that the gas that air lift process need is higher is fast fully to take the hydrogen sulfide produced in hydrogenation process out of, and air lift gas is exactly the gas-hydrogen participating in hydrogenation reaction, its amount is the same with the hydrogen in reaction zone, therefore air lift district diameter design is necking down structure, and this section of diameter is 1/2 ~ 2/3 of reactor hydroconversion reaction zone diameter.
In the inventive method, the base metal petroleum waxes hydrofining catalytic catalyzer that the hydroconversion reaction zone filling in gas-liquid counter current hydrogenator is conventional, is mainly used in removing the heteroatoms such as sulphur, nitrogen and realizing most aromatic saturation.Described catalyzer chief active metal component is the oxide compound of Wu, Molybdenum, nickel.Such as 481-2B, FV-1, FV-10 etc. of Fushun Petrochemical Research Institute's development.Described catalyzer can be single catalyzer, the combination of several catalyzer, can also load protective material.Each catalyst void rate is consistent or inconsistent, when voidage is inconsistent, the voidage of beds bottom higher than top because be easy to when lower space rate is lower hold liquid and back-mixing, to eliminating hydrogen sulfide and second segment hydrogenation reaction unfavorable.
In the inventive method, the operational condition of gas-liquid counter current hydrogenator is: reaction pressure is 3.0 ~ 12.0MPa, is preferably 4.5 ~ 8.0MPa; Volume space velocity is 0.3 ~ 2.5h
-1, be preferably 0.6 ~ 1.5h
-1; Temperature of reaction is 210 ~ 320 DEG C, is preferably 250 ~ 300 DEG C; Hydrogen to oil volume ratio is 80:1 ~ 600:1, is preferably 150:1 ~ 400:1.
Other parameter according to feedstock property and quality product requirement, can be determined by experiment.
In the inventive method, because reactant concn is very low in the second hydroconversion reaction zone, density of hydrogen declines seldom, adopts conventional gas and liquid flowing reactor to ensure larger turndown ratio.
In the inventive method, hydrogenation protecting reaction zone and main hydrofining reaction district, in same reactor or respectively in different reactors, can also flow or adverse current.
In the inventive method, described hydrogenation protecting agent take catalyst weight as benchmark, and active metal is cupric oxide 5% ~ 50%, zinc oxide 10% ~ 45%, ferric oxide 3% ~ 35%, and catalyst property is: pore volume 0.1 ~ 1.2mL/g, specific surface area 10 ~ 400m
2/ g.Be preferably cupric oxide 10% ~ 40%, zinc oxide 15% ~ 30%, ferric oxide 5% ~ 20%, catalyst property is as follows: pore volume is 0.2 ~ 1.0mL/g, and specific surface area is 30 ~ 200m
2/ g.
In the inventive method, described main Hydrobon catalyst is noble metal hydrogenation catalyst or high nickel hydrogenation catalyst.
The optional platinum of noble metal hydrogenation catalyst or palladium hydrogenation catalyst, take catalyst weight as benchmark, active metallic content is 0.1% ~ 3.0%, and support on the carrier such as aluminum oxide or silicon-dioxide, its specific surface area is 80 ~ 400m
2/ g, pore volume are 0.2 ~ 1.0mL/g.Preferred active metallic content is 0.3% ~ 2.0%, and specific surface area is 150 ~ 300m
2/ g, pore volume are 0.3 ~ 0.8mL/g.
High nickel hydrogenation catalyst described in the inventive method, namely active component nickel is supported on Al
2o
3on carrier, with catalyst weight, the massfraction of nickel is 10% ~ 60%, preferably 15% ~ 50%, and surplus is carrier A l
2o
3.Described catalyst property is as follows: specific surface area is 20 ~ 300m
2/ g, is preferably 30 ~ 200m
2/ g, pore volume is 0.2 ~ 1.0mL/g, is preferably 0.3 ~ 0.8mL/g.
In the inventive method, the operational condition of the second hydroconversion reaction zone is: reaction pressure is 3 ~ 13MPa, preferably 5 ~ 7MPa, and temperature of reaction is 110 ~ 220 DEG C, preferably 140 ~ 200 DEG C, volume space velocity 0.4 ~ 3.0h
-1, preferably 0.5 ~ 1.5h
-1, hydrogen wax volume ratio 80 ~ 500, preferably 100 ~ 300.
The optional process of second segment hydrogenated products wax or raise the finished product without new hydrogen.
Compared with prior art, the present invention has following effect.
1, in the inventive method, first paragraph hydrogenation adopts gas-liquid counter current hydrogenator, avoids H
2s, NH
3deng gaseous impurities and C
1, C
2enter in hydrogen Deng micro-molecular gas hydro carbons, cause hydrogen dividing potential drop to reduce, thus improve the effect of hydrogenation removing impurities matter and aromatic saturation.
2, in gas-liquid counter current hydrogenator of the present invention, air lift district to hydroconversion reaction zone diameter increases gradually, relative hydroconversion reaction zone, and air lift district diameter is relatively little, more favourable H
2s, NH
3trip out hydrogenator Deng gas with hydrogen one, make dissolving H in the liquid phase
2s, NH
3reduce further etc. gas concentration, like this, the first hydrogenation products can directly enter second segment hydrogenator without high-pressure separator and gas stripping column, simplifies technical process, saves facility investment.
3, in the inventive method, desulfurization protective agent is set on second segment hydrogenator upper strata, can a small amount of sulphur further more than absorption of residual, second segment catalyzer deactivation can be prevented preferably.What afterbody adopted new hydrogen to carry can to remove preferably paraffin smells taste.
Accompanying drawing explanation
Fig. 1 is a kind of hydrorefining petroleum waxes method flow of the present invention schematic diagram.
Fig. 2 is gas-liquid counter current reactor schematic diagram of the present invention.
Embodiment
The invention will be further described for composition graphs 1.Raw material petroleum wax 21 by feed(raw material)inlet 7 and the hydrogen 20 that enters through hydrogen inlet 10 in a counter-current fashion by gas-liquid counter current hydrogenator 1, contact after reacting with wherein Hydrobon catalyst, gas phase is discharged it from the gas discharge outlet 8 at gas-liquid counter current hydrogenator 1 top and is used, liquid phase stream effluent 11 directly enters the second hydrogenator 12 through the liquid phase relief outlet 9 of gas-liquid counter current hydrogenator 1, contact with Hydrobon catalyst wherein and carry out hydrofining reaction, hydrogenation products 13 enters high-pressure separator 14 and carries out gas-liquid separation, separating obtained gas phase 15 is back to gas-liquid counter current hydrogenator 1 as reaction hydrogen through desulfurization supercharging Posterior circle, separating obtained liquid phase 16 enters stripping tower 17, hydrogen sulfide and gas products is removed through air lift, gas stripping column top gas 18 loops back the second hydrogenator as recycle hydrogen after desulfurization supercharging, turpentole wax 19 is obtained at the bottom of gas stripping column.
In composition graphs 2 pairs of the inventive method, gas-liquid counter current hydrogenator is described further, described gas-liquid counter current hydrogenator 1 comprises upper cover 2 from top to bottom successively, distribute Yi Fan district 3, hydroconversion reaction zone 4, air lift district 5 and lower envelope 6, described air lift district 5 to hydroconversion reaction zone 4 diameter increases gradually, upper cover 2 is provided with feed(raw material)inlet 7 and gas discharge outlet 8, lower cover 6 is provided with liquid phase relief outlet 9 and hydrogen inlet 10, the protective material of inert ceramic balls or low reactivity is loaded in described distribution Yi Fan district 3, base metal catalyst for hydrorefining pertroleum wax is loaded in described hydroconversion reaction zone 4, open grain inert filler is loaded in described air lift district 5.
The solution of the present invention and effect is further illustrated below in conjunction with embodiment.
Prepared by palladium catalyst:
Preparation test palladium catalyst: by 80g gamma-aluminium oxide carrier (specific surface 210m
2/ g, pore volume 0.4mL/g) be placed in 500ml glass beaker, pouring 160ml concentration into is 0.024mol/L, and temperature is the Na of 20 DEG C
2pdCI
4(Na
2pdCl
4) solution, flood 1h under slow stirring, then leach catalyzer, at 120 DEG C, dry 3h, 480 DEG C of roasting 4h.Obtain the palladium catalyst containing Pd0.5%.
Copper-zinc protective material preparation:
Preparation test copper-zinc protective material: according to 40%CuO, 40%ZnO and 20%AI
2o
3original weight ratio prepare its nitrate solution respectively and mix, then add 10%NaOH solution and make PH reach 6.8, the suspension of formation is stirred 2h at 75 DEG C, then filter and use cold water washing to remove nitrate radical.By filtration cakes torrefaction, roasting 3h at 350 DEG C, is then squeezed into 2.0* (3 ~ 8) mm bar, then at 450 DEG C, burn 1.5h sizing.
Test raw material: No. 58 paraffin: fusing point 58.6 DEG C, Saybolt color numbers+15, No. 7, light stability, oleaginousness 0.25%, containing toluene amount 40mg/kg.
Hydrogen: purity 99.9%.
Embodiment 1
Gas-liquid counter current reactor charge FV-10 catalyzer 100mL.Gas-liquid counter current reactor reaction condition is working pressure 6.0MPa, temperature of reaction 250 DEG C, volume space velocity 1.5h
-1with hydrogen wax volume ratio 300:1.Second hydrogenator loads above-mentioned copper-zinc protective material 20g and palladium catalyst 100mL, with hydrogen, above-mentioned two kinds of catalyzer is carried out reduction treatment under 180 DEG C and normal pressure.The operational condition of the second hydrogenator is: pressure 6.0MPa, temperature of reaction 180 DEG C, volume space velocity 1.5h
-1with hydrogen wax volume ratio 300:1.Run 30,300 hr collections products respectively, and measure product property, the results are shown in Table 1.
Embodiment 2
Identical with embodiment 1, difference is arrange a High Pressure Absorption devulcanizer between the high-pressure separator gaseous phase outlet of the second hydrogenator and the hydrogen inlet of gas-liquid counter current reactor bottom, the sweetening agent CDS-200 that inner filling is commercially available.Run 30,300 hr collections products respectively, and measure product property, the results are shown in Table 1.
Embodiment 3
Identical with embodiment 1, difference is the second hydrogenator filling NCG catalyzer, steady running 30 hours, 300 h before harvest products, and measures product property, the results are shown in Table 1.
Comparative example 1
Identical with embodiment 1, difference is that gas-liquid counter current hydrogenator is changed to routine and flows hydrogenator, and is provided with after-treatment system, and hydrogenated products enter the second reactor again after hydrogen air lift.Run 30,300 hr collections products respectively, and measure product property, the results are shown in Table 1.
Comparative example 2
Identical with comparative example 1, difference is copper-zinc protective material that the second hydrogenator does not load.
The product property of each embodiment of table 1 and comparative example
| Embodiment 1 | Embodiment 2 | Embodiment 3 | Comparative example 1 | Comparative example 2 | |
| Run 30h mono-section of product property | |||||
| Saybolt color, number | +30 | +30 | +30 | +30 | +30 |
| Light stability | 3 | 3 | 3 | 3 | 3 |
| Smell taste | 1.0 | 1.0 | 1.0 | 1.0 | 1.0 |
| Toluene mg/kg | 4 | 3 | 6 | 12* | 13* |
| Run 30h bis-sections of product properties | |||||
| Saybolt color, number | +30 | +30 | +30 | +30 | +30 |
| Light stability | 2-3 | 2-3 | 2-3 | 2-3 | 2-3 |
| Smell taste | 0 | 0 | 0 | 0 | 0 |
| Run 300h bis-sections of product properties | |||||
| Saybolt color, number | +30 | +30 | +30 | +30 | +30 |
| Light stability | 2-3 | 2-3 | 2-3 | 2-3 | 2-3 |
| Smell taste | 0 | 0 | 0.5 | 0 | 0.5 |
In table, * represents toluene level in non-air lift product.
Claims (10)
1. a hydrorefining petroleum waxes method, comprise: petroleum wax raw material and hydrogen are in a counter-current fashion by gas-liquid counter current hydrogenator, after non-noble metal hydrogenation catalyst for refining contact reacts wherein, gas phase is discharged it from reactor head and is used, liquid phase stream effluent directly enters the second hydroconversion reaction zone, successively through hydrogenation protecting reaction zone and main hydrofining reaction district, contact with reduced form Hydrobon catalyst with hydrogenation protecting agent wherein successively and carry out hydrogenation reaction, hydrotreated product is after being separated, gas phase loops back gas-liquid counter current hydrogenator, liquid phase is the petroleum paraffin product after refining, wherein, described gas-liquid counter current hydrogenator comprises upper cover from top to bottom successively, distribute Yi Fan district, hydroconversion reaction zone, air lift district and lower cover, described air lift district increases gradually to hydroconversion reaction zone diameter, described air lift district diameter is 1/2 ~ 2/3 of hydroconversion reaction zone diameter, upper cover is provided with feed(raw material)inlet and gas discharge outlet, lower cover is provided with liquid phase relief outlet and hydrogen inlet, the protective material of described distribution Yi Fan district filling inert ceramic balls or low reactivity, described hydroconversion reaction zone filling catalyst for hydrorefining pertroleum wax, described air lift district filling open grain inert filler.
2. in accordance with the method for claim 1, it is characterized in that: non-noble metal hydrogenation catalyst for refining is base metal petroleum waxes hydrofining catalytic catalyzer, described base metal petroleum waxes hydrofining catalytic catalyzer comprises one or more.
3. in accordance with the method for claim 1, it is characterized in that: the operational condition of gas-liquid counter current hydrogenator is: reaction pressure 3.0 ~ 12.0MPa, volume space velocity 0.3 ~ 2.5h
-1, temperature of reaction 210 ~ 320 DEG C, hydrogen to oil volume ratio 80:1 ~ 600:1.
4. in accordance with the method for claim 1, it is characterized in that: hydrogenation protecting reaction zone and main hydrofining reaction district are in same reactor or respectively in different reactors.
5. in accordance with the method for claim 1, it is characterized in that: described hydrogenation protecting agent, take catalyst weight as benchmark; active metal is cupric oxide 5% ~ 50%, zinc oxide 10% ~ 45%, ferric oxide 3% ~ 35%; catalyst property is: pore volume 0.1 ~ 1.2mL/g, specific surface area 10 ~ 400m
2/ g.
6. in accordance with the method for claim 1, it is characterized in that: main Hydrobon catalyst is noble metal hydrogenation catalyst or high nickel hydrogenation catalyst.
7. in accordance with the method for claim 6, it is characterized in that: described noble metal hydrogenation catalyst with aluminum oxide or silicon-dioxide for carrier, take catalyst weight as benchmark, group vib active metallic content is with oxide basis for 0.1% ~ 3.0%, and this catalyst property is: specific surface area 80 ~ 400m
2/ g, pore volume 0.2 ~ 1.0mL/g.
8. in accordance with the method for claim 6, it is characterized in that: described high nickel hydrogenation catalyst, with catalyst weight, nickel content is 10% ~ 60%, and this catalyst property is: specific surface area 20 ~ 300m
2/ g, pore volume 0.2 ~ 1.0mL/g.
9. in accordance with the method for claim 1, it is characterized in that: the operational condition of described second hydroconversion reaction zone is: reaction pressure 3 ~ 13MPa, temperature of reaction 110 ~ 220 DEG C, volume space velocity 0.4 ~ 3.0h
-1, hydrogen wax volume ratio 80 ~ 500.
10. in accordance with the method for claim 1, it is characterized in that: main hydrofining product wax passes through or carries without new hydrogen.
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| CN106675622B (en) * | 2015-11-11 | 2018-10-12 | 中国石油化工股份有限公司 | A kind of vulcanization start-up method reducing FCC gasoline deep hydrodesulfurizationof loss of octane number |
| CN118222321A (en) * | 2022-12-21 | 2024-06-21 | 中国石油天然气股份有限公司 | Oil hydrogenation device and oil hydrofining method |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101619241A (en) * | 2008-07-04 | 2010-01-06 | 中国石油化工股份有限公司 | Method for hydrofining paraffin wax |
| CN102041069A (en) * | 2009-10-16 | 2011-05-04 | 中国石油化工股份有限公司 | Gas-liquid countercurrent hydrogenation method for desulfurization, denitrification and aromatic hydrocarbon of diesel |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101619241A (en) * | 2008-07-04 | 2010-01-06 | 中国石油化工股份有限公司 | Method for hydrofining paraffin wax |
| CN102041069A (en) * | 2009-10-16 | 2011-05-04 | 中国石油化工股份有限公司 | Gas-liquid countercurrent hydrogenation method for desulfurization, denitrification and aromatic hydrocarbon of diesel |
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