CN104888821A - High alkaline nitrogen-containing shale oil hydrogenation upgrading catalyst - Google Patents
High alkaline nitrogen-containing shale oil hydrogenation upgrading catalyst Download PDFInfo
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Abstract
The invention discloses a high alkaline nitrogen-containing shale oil hydrogenation upgrading catalyst which is prepared from 5%-25% by mass of a tungsten oxide or nickel oxide main active metal, 1%-15% by mass of a ferrous oxide second active metal, 0%-5% by mass of one or two or more of P, Ti, Zn and Zr as an assistant agent, and balance of a porous oxide carrier by once strip-extrusion moulding. The high alkaline nitrogen-containing shale oil hydrogenation upgrading catalyst is suitable for use in high nitrogen-containing shale oil, coal tar, wax oil and other inferior oil hydrogenation upgrading, and can be used for preparation of high octane gasoline number components and high cetane number diesel components.
Description
Technical field
The invention belongs to catalysis technical field, relate to a kind of hydrogenation of shale oil upgrading catalyst, for the hydrogenation upgrading of shale oil, coal tar, the contour nitrogen poor oil of wax oil.
Background technology
Oil shale in retort process, the product liquid shale oil that its organic decomposes generates.Different according to the place of production, oil shale oil content is not from 3.5% to 19% etc.China's oil shale resources are enriched, and its reserves occupy the 4th, the world, are equivalent to 16,000,000,000 tons of shale oil.Along with the exhaustion day by day of petroleum resources, the exploitation of shale oil become more and more important, and shale oil industry is the important component part of energy industry, are also the supplementary energy of natural oil.
The similar natural oil of shale oil composition, but comparatively natural oil contains more unsaturated hydrocarbons, and nitrogenous, the non-hydrocarbons organic compound such as sulphur, oxygen.These unsaturated hydro carbons and non-hydrocarbons organic compound be cause that oil product colloid increases, sediment forms and causes that stability is deteriorated, the main cause of color blackening.Current shale oil is mainly with producing fuel and chemical products.Shale oil upgrading is produced the light Fuels such as gasoline, kerosene and diesel oil and is had to pass through hydrogenation upgrading desulfurization, denitrogenation, deoxidation, olefin saturated, aromatic saturation and ring opening and demetalization and depitching impurity etc.
Patent CN101067089A discloses a kind of method of hydrotreating of shale oil, in the method, shale oil generates hydrogenated oil through hydrotreatment, hydrogenated oil is separated into light and heavy fractions, and heavy end obtains dry gas, liquefied gas, gasoline, diesel oil and catalytic heavy through hydro-conversion.Catalysis adopts hydrogenation protecting and hydrotreating catalyst, and wherein hydrotreating catalyst active component is the VIth B and group VIII metal element, and carrier is zeolite molecular sieve.The method low-carbon olefines high-output.
After patent USP4419218 relates to a kind of demetalization, hydrogenation of shale oil Cracking catalyst produces the method for jet fuel.Catalyst be with Mo-Ni-P be active metal hydrofinishing agent and take Co-Cr-Mo as the hydrocracking catalyst of active component, carrier is molecular sieve.Jet combustion productive rate can reach 70%.
Patent CN1785512A discloses a kind of containing ferrous hydrocarbon cracking catalyzer, ferrous iron by 5 ~ 15%, phosphoric acid hydrogen two aluminium of 5 ~ 20% and the clay of surplus form, be applicable to the catalytic cracking of fixed bed containing hydro carbons in high nitrogen shale oil and high wax content oil, cracking performance is good.
Patent CN101492605 discloses a kind of shale oil hydrogenation process, shale oil raw material and hydrogen are reverse by Hydrobon catalyst bed from reactor upper and lower respectively, carry out oil hydrogenation to refine, reduce the object that basic nitrogen and acidity of catalyst central contact time reduce product nitrogen content.Catalyst is conventional hydro catalyst for refining.
Above hydrogenation of shale oil processing method reduces shale oil nitrogen content from the angle of process optimization mostly, and catalyst adopts conventional crude hydrofinishing and hydrocracking catalyst substantially, and this kind of catalyst is carrier mainly with zeolite molecular sieve greatly.Zeolite molecular sieve cracking mechanism is hydro carbons Bronsted acid central role on catalyst, generates carbonium ion and chain fracture occurs.And basic nitrogen compound is easily adsorbed in zeolite molecular sieve acid site, zeolite molecular sieve activity is caused to reduce or inactivation.Performances such as being applicable to containing high nitrogen shale oil and high-wax oil hydrocarbon hydrocracking catalyst although patent CN1785512A discloses a class, only considering hydrocracking performance, to consider in oil product that unsaturated hydro carbons is saturated, aromatic saturation and ring opening and hetero atom remove.
Summary of the invention
The present invention is directed to the deficiency that existing catalysis technique exists in shale oil process, a kind of hydrogenation upgrading Catalysts and its preparation method containing high alkalinity nitrogen shale oil is proposed, the bed hydroprocessing upgradings such as feedstock oil is saturated through unsaturated hydro carbons, aromatic saturation and ring opening and hetero atom remove reaction, directly obtains the low high octane gasoline component of nitrogen content and high cetane number diesel component.
A kind of hydrogenation upgrading catalyst containing high alkalinity nitrogen shale oil of the present invention comprises following content: catalyst is by the tungsten oxide/nickel oxide of percetage by weight 5% ~ 25%, the ferrous oxide of 1% ~ 15%, P, Ti, Zn, Zr of 0% ~ 5% and the porous oxide carrier one-shot forming preparation of surplus.
The main active metal of catalyst is tungsten and/or nickel, and calculate with oxide mass percentage, active metal component content is 5% ~ 25%.Second active metal is ferrous oxide, and calculate with oxide mass percentage, content is 1% ~ 15%, and carrying out the inorganic salts of self-contained ferrous ion, can be ferrous nitrate, ferrous sulfate, frerrous chloride.Auxiliary agent is one or more of P, Ti, Zn, Zr, and content is 0% ~ 5%.Surplus is catalyst porous oxide carrier, and porous oxide is γ-A
2o
3, porous SiO
2, one or more in column clay.The solution of the active metal salt and auxiliary agent that compare preparation by metering fully mixes with carrier, kneading, and an extruded moulding, 120 DEG C of dried overnight, 350 DEG C ~ 550 DEG C roastings are made.
Kaolinite Preparation of Catalyst of the present invention is applicable to the hydrogenation upgrading containing high nitrogen poor oil such as shale oil, coal tar, wax oil, and the hydrogenation conditions of optimization is temperature 300 ~ 450 DEG C, Hydrogen Vapor Pressure 5 ~ 12MPa, volume space velocity 0.3 ~ 2.0h during liquid
-1be 600 ~ 1400:1 with hydrogen-oil ratio.
Detailed description of the invention
Embodiment (one):
1. take ammonium metatungstate 58.1g, ferrous sulfate 309.6g, activated alumina 727.0g, concentration is the phosphoric acid solution 500g of 10%, and above material is mixed rear extrusion, extrusion pressure 300N, 120 DEG C of dried overnight, and 350 DEG C of roastings are made.In gained 1000g catalyst, in oxide weight percent, containing tungsten oxide 5%, ferrous oxide 8%, activated alumina 72.7%, phosphorus 3.6%, all the other are sulfate radical.
2. take Nickelous nitrate hexahydrate 467.2g, ferrous sulfate 580.5g, porous silica 494.0g, concentration is the phosphoric acid solution 500g of 10%, and above material is mixed rear extrusion, extrusion pressure 300N, 120 DEG C of dried overnight, and 450 DEG C of roastings are made.In gained 1000g catalyst, in oxide weight percent, containing nickel oxide 12%, ferrous oxide 15%, porous silica 49.4%, phosphorus 3.6%, all the other are sulfate radical.
3. take ammonium metatungstate 219.9g, Nickelous nitrate hexahydrate 237.2g, ferrous sulfate 309.6g, column clay 527.0g, concentration is the phosphoric acid solution 500g of 10%, and above material is mixed rear extrusion, extrusion pressure 300N, 120 DEG C of dried overnight, 550 DEG C of roastings are made.In gained 1000g catalyst, in oxide weight percent, containing tungsten oxide and nickel oxide 25% (mol ratio WO
3: NiO=1:1), ferrous oxide 8%, column clay 52.7%, phosphorus 3.6%, all the other are sulfate radical.
Column clay preparation method: get na-montmorillonite clay and add deionized water slurrying, controlling pulp density (soil/water) is 4.5 ~ 10g/L, makes soil paste dispersed, and controlling reaction temperature is 50 ~ 90 DEG C, by M
n+molal quantity and montmorillonite mass ratio are the ratio of 10mmol/g, are slowly added drop-wise in sodium monotmorillonite slurries by pillared liquid, continue stirring 2 ~ 10 hours after dripping off pillared liquid, then ageing 24 ~ 48h at temperature is 60 ~ 80 DEG C.By column-supporting product centrifugation, dry at 80 ~ 100 DEG C, then sample is put into roasting 4 ~ 10h at Muffle furnace 500 ~ 700 DEG C, obtain column clay.Wherein M
n+for Fe
3+, Fe
3+from the nitrate (detailed preparation method is shown in patent ZL201110092299.4) of iron content.
Embodiment (two):
1. take Nickelous nitrate hexahydrate 194.7g, ferrous nitrate 200.3g, activated alumina 834.0g, concentration is the phosphoric acid solution 500g of 10%, and above material is mixed rear extrusion, extrusion pressure 300N, 120 DEG C of dried overnight, and 350 DEG C of roastings are made.In gained 1000g catalyst, in oxide weight percent, containing nickel oxide 5%, ferrous oxide 8%, activated alumina 83.4%, phosphorus 3.6%.
2. take ammonium metatungstate 467.2g, ferrous nitrate 25.0g, porous silica 834.0g, concentration is the phosphoric acid solution 500g of 10%, and above material is mixed rear extrusion, extrusion pressure 300N, 120 DEG C of dried overnight, and 450 DEG C of roastings are made.In gained 1000g catalyst, in oxide weight percent, containing tungsten oxide 12%, ferrous oxide 1%, activated alumina 83.4%, phosphorus 3.6%.
3. take ammonium metatungstate 176.8g, Nickelous nitrate hexahydrate 381.4g, ferrous nitrate 200.3g, column clay 634.0g (column clay preparation method is shown in patent ZL201110092299.4), concentration is the phosphoric acid solution 500g of 10%, and above material is mixed rear extrusion, extrusion pressure 300N, 120 DEG C of dried overnight, 550 DEG C of roastings are made.In gained 1000g catalyst, in oxide weight percent, containing tungsten oxide and nickel oxide 25% (mol ratio WO
3: NiO=1:2), ferrous oxide 8%, activated alumina 63.4%, phosphorus 3.6%.
Embodiment (three):
1. take ammonium metatungstate 44.1g, Nickelous nitrate hexahydrate 47.5g, frerrous chloride 141.2g, activated alumina 755.0g, concentration is the phosphoric acid solution 500g of 10%, and above material is mixed rear extrusion, extrusion pressure 300N, 120 DEG C of dried overnight, 350 DEG C of roastings are made.In gained 1000g catalyst, in oxide weight percent, containing tungsten oxide and nickel oxide 5% (mol ratio WO
3: NiO=1:1), ferrous oxide 8%, activated alumina 75.5%, phosphorus 3.6%, all the other are chlorine.
2. take ammonium metatungstate 105.6g, Nickelous nitrate hexahydrate 113.8g, frerrous chloride 17.7g, porous silica 765.0g, concentration is the phosphoric acid solution 500g of 10%, and above material is mixed rear extrusion, extrusion pressure 300N, 120 DEG C of dried overnight, 450 DEG C of roastings are made.In gained 1000g catalyst, in oxide weight percent, containing tungsten oxide and nickel oxide 12% (mol ratio WO
3: NiO=1:1), ferrous oxide 1%, activated alumina 76.5%, phosphorus 3.6%, all the other are chlorine.
3. take ammonium metatungstate 250.4g, Nickelous nitrate hexahydrate 135.1g, frerrous chloride 141.2g, column clay 555.0g (column clay preparation method is shown in patent ZL201110092299.4), concentration is the phosphoric acid solution 500g of 10%, and above material is mixed rear extrusion, extrusion pressure 300N, 120 DEG C of dried overnight, 550 DEG C of roastings are made.In gained 1000g catalyst, in oxide weight percent, containing tungsten oxide and nickel oxide 25% (mol ratio WO
3: NiO=2:1), ferrous oxide 8%, activated alumina 55.5%, phosphorus 3.6%, all the other are chlorine.
In embodiment (), (two), (three), used carrier material can also select activated alumina, porous silica, column clay with the mixture of any ratio combination.
By the catalyst of the present invention that above-described embodiment is obtained, adopt fixed bed reactors to carry out testing containing the hydrogenation upgrading of high nitrogen shale oil raw material, hydrogenation products cuts to obtain gasoline fraction and diesel oil distillate through cut.Experiment proves that the present invention prepares catalysis and has that anti-nitrogen performance is good, hydrotreated lube base oil, aromatic hydrocarbons open loop, the active high feature of desulfurization nitrogen oxygen heteroatom.Detailed Experimental data are as follows:
Experiment 1: the hydrogenation upgrading of Huadian shale oil
With catalyst prepared by embodiment () 2, adopt fixed bed reactors, gas-liquid is from reactor bottom and flow to material, loaded catalyst 100mL, and hydrogenation conditions is temperature 360 DEG C, Hydrogen Vapor Pressure 8MPa, volume space velocity 0.8h during liquid
-1be 1000:1 with hydrogen-oil ratio, Detailed Experimental data list in table 1.
Table 1 Huadian hydrogenation of shale oil upgrading data
| Raw material | Gasoline component | Diesel component | |
| Yield (%) | —— | 19.8 | 75.4 |
| Density (g/cm 3) | 0.8804 | 0.7769 | 0.8316 |
| Viscosity (mPas) | 16.05 | 0.8847 | 3.045 |
| S(ppm) | 5800 | 44.1 | 81.3 |
| N(ppm) | 95900 | 89.7 | 115.4 |
| O(ppm) | 10500 | 82.2 | 78.1 |
| H/C mol ratio | 1.71 | 1.89 | 1.94 |
| Octane number | —— | 89.5 | —— |
| Cetane number | —— | —— | 48.7 |
Experiment 2: the hydrogenation upgrading of Beipiao City's shale oil
With catalyst prepared by embodiment (two) 2, adopt fixed bed reactors, gas-liquid is from reactor bottom and flow to material, loaded catalyst 100mL, and hydrogenation conditions is temperature 380 DEG C, Hydrogen Vapor Pressure 10MPa, volume space velocity 0.8h during liquid
-1be 1000:1 with hydrogen-oil ratio, Detailed Experimental data list in table 2.
Table 2 Beipiao City hydrogenation of shale oil upgrading data
| Raw material | Gasoline component (< 180 DEG C) | Diesel component (180 ~ 360 DEG C) | |
| Yield (%) | —— | 20.4 | 76.7 |
| Density (g/cm 3) | 0.8892 | 0.7769 | 0.8316 |
| Viscosity (mPas) | 16.23 | 0.8847 | 3.045 |
| S(ppm) | 7100 | 50.4 | 78.7 |
| N(ppm) | 19800 | 43.4 | 57.6 |
| O(ppm) | 58500 | 89.5 | 175.3 |
| H/C mol ratio | 1.65 | 2.07 | 1.98 |
| Octane number | —— | 92.1 | —— |
| Cetane number | —— | —— | 49.8 |
Experiment 3: the hydrogenation upgrading of Beipiao City's shale oil
With catalyst prepared by embodiment (three) 2, adopt fixed bed reactors, gas-liquid is from reactor bottom and flow to material, loaded catalyst 100mL, and hydrogenation conditions is temperature 380 DEG C, Hydrogen Vapor Pressure 10MPa, volume space velocity 0.8h during liquid
-1be 1000:1 with hydrogen-oil ratio, Detailed Experimental data list in table 3.
Table 3 Beipiao City hydrogenation of shale oil upgrading data
| Raw material | Gasoline component (< 180 DEG C) | Diesel component (180 ~ 360 DEG C) | |
| Yield (%) | —— | 21.3 | 76.2 |
| Density (g/cm 3) | 0.8892 | 0.7758 | 0.8260 |
| Viscosity (mPas) | 16.23 | 0.8743 | 2.904 |
| S(ppm) | 7100 | 37.0 | 47.9 |
| N(ppm) | 19800 | 13.1 | 8.77 |
| O(ppm) | 58500 | 85.0 | 165.0 |
| H/C mol ratio | 1.65 | 1.96 | 1.81 |
| Octane number | —— | 92.2 | —— |
| Cetane number | —— | —— | 50.9 |
As can be seen from above-mentioned experimental result, under catalyst action of the present invention, liquid fuel yield is all more than 95%, and gasoline component yield is about 20%, and diesel component yield is about 75%, S, N, O hetero atom removal efficiency is greater than 98%.Petrol and diesel oil component H/C mol ratio comparatively raw material significantly improves, free under catalyst action is described that hydrogenation of unsaturated hydrocarbons is saturated, aromatic hydrogenation is saturated and ring-opening reaction, product saturation degree improves, and this is also ensure that gasoline component has the main cause that high-octane rating and diesel component have high cetane number.
Claims (7)
1. one kind contains high alkalinity nitrogen hydrogenation of shale oil upgrading catalyst, it is characterized in that: this catalyst is the main active metal of 5% ~ 25% by mass percent, ferrous oxide second active metal of 1% ~ 15%, one or more of P, Ti, Zn, Zr of 0% ~ 5% are auxiliary agent, surplus is porous oxide carrier, an extruded moulding preparation.
2. one according to claim 1 is containing high alkalinity nitrogen hydrogenation of shale oil upgrading catalyst, and it is characterized in that: the main active metal of catalyst is tungsten/nickel, with oxide mass percent basis, active metal component content is 5% ~ 25%.
3. one according to claim 1 is containing high alkalinity nitrogen hydrogenation of shale oil upgrading catalyst, it is characterized in that: catalyst second active metal ferrous oxide is from the one of inorganic metal salt ferrous nitrate, ferrous sulfate, frerrous chloride.
4. one according to claim 1 is containing high alkalinity nitrogen hydrogenation of shale oil upgrading catalyst, it is characterized in that: catalyst carrier porous oxide is γ-A
2o
3, porous SiO
2, one or more in column clay.
5. one according to claim 1 is containing high alkalinity nitrogen hydrogenation of shale oil upgrading catalyst, it is characterized in that: this catalyst is applicable to the hydrogenation upgrading of shale oil, coal tar, wax oil, especially high alkalinity nitrogen shale oil.
6. the preparation method containing high alkalinity nitrogen hydrogenation of shale oil upgrading catalyst according to any one of claim 1-5, it is characterized in that: method for preparing catalyst be by metering ratio active metal salt solution fully mix with carrier, kneading, an extruded moulding, 120 DEG C of dried overnight, 350 DEG C ~ 550 DEG C roastings are made.
7. obtain through refining a catalyst containing high alkalinity nitrogen hydrogenation of shale oil, it is characterized in that using catalyst described in any one of claim 1-5, hydrogenation conditions is temperature 300 ~ 450 DEG C, Hydrogen Vapor Pressure 5 ~ 12MPa, volume space velocity 0.3 ~ 2.0h during liquid
-1be 600 ~ 1400:1 with hydrogen-oil ratio.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109569578A (en) * | 2017-09-28 | 2019-04-05 | 中国石油化工股份有限公司 | Fuel oil hydrogenation catalysts are produced for tar |
| CN109569635A (en) * | 2017-09-28 | 2019-04-05 | 中国石油化工股份有限公司 | For Tar production fuel oil hydrogenation catalysts |
| CN109575989A (en) * | 2017-09-28 | 2019-04-05 | 中国石油化工股份有限公司 | Method for tar made fuel oil |
| CN109569700A (en) * | 2017-09-28 | 2019-04-05 | 中国石油化工股份有限公司 | For tar made fuel oil hydrogenation catalyst |
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| CN109569578A (en) * | 2017-09-28 | 2019-04-05 | 中国石油化工股份有限公司 | Fuel oil hydrogenation catalysts are produced for tar |
| CN109569635A (en) * | 2017-09-28 | 2019-04-05 | 中国石油化工股份有限公司 | For Tar production fuel oil hydrogenation catalysts |
| CN109575989A (en) * | 2017-09-28 | 2019-04-05 | 中国石油化工股份有限公司 | Method for tar made fuel oil |
| CN109569700A (en) * | 2017-09-28 | 2019-04-05 | 中国石油化工股份有限公司 | For tar made fuel oil hydrogenation catalyst |
| CN109575985A (en) * | 2017-09-28 | 2019-04-05 | 中国石油化工股份有限公司 | The method for producing fuel oil for tar |
| CN109575986A (en) * | 2017-09-28 | 2019-04-05 | 中国石油化工股份有限公司 | Method for Tar production fuel oil |
| CN109575986B (en) * | 2017-09-28 | 2020-12-29 | 中国石油化工股份有限公司 | Method for producing fuel oil from tar |
| CN109575989B (en) * | 2017-09-28 | 2020-12-29 | 中国石油化工股份有限公司 | Method for preparing fuel oil from tar |
| CN109575985B (en) * | 2017-09-28 | 2020-12-29 | 中国石油化工股份有限公司 | Method for preparing fuel oil from tar |
| CN109569578B (en) * | 2017-09-28 | 2021-12-28 | 中国石油化工股份有限公司 | Hydrogenation catalyst for preparing fuel oil from tar |
| CN109569700B (en) * | 2017-09-28 | 2021-12-28 | 中国石油化工股份有限公司 | Hydrogenation catalyst for producing fuel oil from tar |
| CN109569635B (en) * | 2017-09-28 | 2021-12-28 | 中国石油化工股份有限公司 | Hydrogenation catalyst for producing fuel oil from tar |
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