CN102994141A - Poor quality aviation kerosene hydrotreatment method - Google Patents
Poor quality aviation kerosene hydrotreatment method Download PDFInfo
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- CN102994141A CN102994141A CN201110274171XA CN201110274171A CN102994141A CN 102994141 A CN102994141 A CN 102994141A CN 201110274171X A CN201110274171X A CN 201110274171XA CN 201110274171 A CN201110274171 A CN 201110274171A CN 102994141 A CN102994141 A CN 102994141A
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Abstract
The present invention relates to a poor quality aviation kerosene hydrotreatment method, wherein a catalyst is a composite catalyst prepared from one or a plurality of materials selected from cobalt, molybdenum, nickel and tungsten and P, and comprises, by weight, 5-50% of the metal component, 5-30% of a phosphide, and the balance of a carrier. The method comprises: dissolving ammonium hypophosphite and a metal salt containing Co, Ni, Mo or/and W in deionized water, adding a complexing agent to prepare a metal impregnation solution, and carrying out impregnation drying on the carrier; carrying out a calcination treatment to obtain a catalyst containing the metal such as Co, Ni, Mo or W and P, wherein a treatment temperature is 200-400 DEG C, and a treatment time is 2-10 h; and carrying out a vulcanization treatment on the catalyst to prepare a vulcanization state catalyst, wherein a vulcanization temperature is 250-450 DEG C, a time is 10 h, and the catalyst can be used for treating poor quality aviation kerosene fraction so as to improve a freezing point, a smoke point and chrominance of the aviation kerosene, substantially increase aviation kerosene product quality, and produce qualified No.3 aviation kerosene fuel.
Description
Technical field
The present invention relates to the method that a kind of coal distillate hydrogenation that navigates is processed, take poor quality boat coal as raw material, improve freezing point, the smoke point of raw material boat coal, simultaneously hydrorefined method.
Background technology
Boat jet system is generally hydrofining, adopts traditional Hydrobon catalyst can remove the impurity such as wherein sulphur, nitrogen, but to improving boat coal smoke point DeGrain.The high activated catalyst of industrial application generally speaking has two types at present, and a kind of is noble metal catalyst, and hydrogenation activity is high, and the operational condition severity is low, but the noble metal catalyst cost is high, and the thing that easily cures is poisoned and reduced activity, and be affected running period.Another kind is non-precious metal catalyst, nickel-based aluminum oxide type catalyzer, and the hydrogenation saturated activity is higher, and raw materials cost is lower, but needs High Temperature High Pressure and high hydrogen-oil ratio, and plant energy consumption is higher.
CN1053636 discloses a kind of preparation method of catalyst used for hydrogenation of distilled oil fraction, a kind of catalyst used for hydrogenation of distilled oil fraction with sulfur resistance is provided, it is characterized in that being consisted of by amorphous silicon oxide-alumina supporter and platinum, palladium bimetal active ingredient, the catalyzer that provides has good sulfur resistance and aromatic saturation performance, can be used for sulphur content up to the hydrogenation process of the distillate of 6000ppm (in thiophene).In addition, because the present invention after the carrier dealumination treatment, need not high-temperature roasting, thereby simplified technique, reduced facility investment, reduced energy consumption, but the noble metal catalyst cost has been high.CN101172261 relates to a kind of preparation method of catalyst composition.Adopt coprecipitation method to generate Ni
xW
yO
zThe composite oxides precursor is then with MoO
3Making beating mixing, filtration, moulding, activation are final catalyzer.Gelatinous mixture namely is composite oxides Ni
xW
yO
zPrecursor.The catalyst metal of the inventive method preparation is uniformly dispersed, and use properties is high, and particularly the activity for deep impurity removal process is higher.And the inventive method is easy, and loss rate of metal is low.CN1342102 relates to a kind of method for preparing hydrotreating catalyst, described method comprises, at least two ethnic vib metal compositions of at least one ethnic VIII base metal composition of solubilised state and solubilised state are mixed in reaction mixture and react, obtain a kind of throw out of oxidation stability, then with this throw out sulfuration.Because it is high to change the catalyst metal content of method preparation, need to add a certain amount of binding agent and come moulding, the keying action between reactive metal and binding agent does not cause by force catalyst strength not high, has limited the industrial application of such catalyzer.CN101089133, CN1339985 provide a kind of preparation of solid bodies phase catalyst, but all can not well solve the low problem of reactive metal utilization ratio, and the catalyzer preparation cost is higher.
The metal phosphide catalyzer is as a kind of novel hydrogenation catalyst broad research.
At present, the metal phosphorizing nickel catalyzator generally adopts the temperature-programmed reduction method preparation, and the method need to be carried out under comparatively high temps and reducing atmosphere.Adopt Al
2O
3During for carrier, in the process of high temperature reduction nickel ion, cause easily nickel aluminate to generate, so that with Al
2O
3For the catalyst of phosphatizing nickel hydrodesulfurization activity of carrier lower.At present, efficient phosphide Hydrobon catalyst is generally with SiO
2Be carrier, still, SiO
2The forming technique of carrier and Surface acidity thereof and Acidity have limited the industry of catalyzer and have promoted.The present invention is directed to the characteristics of above-mentioned phosphide, develop the approach that a low temperature prepares phosphide material, realize the high high active of hydrogenation catalysis of catalyzer.
Summary of the invention
The purpose of this invention is to provide the method that a kind of kerosene hydrogenation inferior is processed, used catalyzer is a kind of high reactivity oil purification catalyzer with better hydrogenation ability.
The method that kerosene hydrogenation of the present invention is processed, at pressure 3.0-6.0MPa, temperature 250-400 ℃, air speed are 1.5-5.0h
-1With hydrogen-oil ratio be hydrogenating desulfurization under the condition of 150-800/1, can realize feed sulphur content is higher than 2000 μ g/g, nitrogen content is higher than 500 μ g/g, density is greater than 0.80g/cm
3Poor quality boat coal distillate catalytic hydroprocessing.
Catalyzer is a kind of one or more and composite catalyst of phosphide that contains in cobaltous sulfide, moly-sulfide, nickelous sulfide, tungsten sulfide, nickel tungsten sulphur, cobalt molybdenum sulphur, the nickel cobalt molybdenum sulphur.
Catalyzer is take resistant to elevated temperatures inorganic porous oxide material as carrier, such as Al
2O
3, SiO
2, SiO
2-Al
2O
3, TiO
2, ZrO
2, molecular sieve, amorphous aluminum silicide one or more, in the carrier preparation process by ammoniacal liquor, organic acid control pH value 7.0-8.0; The carrier specific surface area is 150-350m after the moulding
2/ g, pore volume are 0.10-0.50ml/g, and mean pore size is 3-15nm, and face shaping is sphere, bar shaped or sheet.The equi-volume impregnating that the method for preparing catalyst employing is traditional or vacuum impregnation, distribution dipping, supersaturation pickling process.
Catalyzer preparation: (1) is at first with ammonium hypophosphite and contain the metal-salt of Co, Ni, Mo or W, in deionized water, dissolve, add complexing agent and be made into certain density stable metal steeping fluid, then shaping carrier is dropped in the steeping fluid and filter after 1-2 hour, 120 ℃ of oven dry.(2) obtain having the metal that contains Co, Ni, Mo or W and the catalyzer of P phase by calcination process, 200～400 ℃ for the treatment of temps, the treatment time is 2～10h.The catalyzer that (3) then will contain this phosphide at a certain temperature sulfidizing is prepared into the sulphided state catalyzer, and the pre-curing temperature of catalyzer is 250～450 ℃, and the prevulcanized time is 10h.In catalyst weight %: metal component accounts for 5～50%, and it is 5～30% that phosphide accounts for, and surplus is carrier.Described complexing agent is 0.5～5: 1 for the mol ratio with metal Ni or Co.
The invention has the beneficial effects as follows and realized low-cost preparation phosphide hydrogenation catalyst, the sulphided state catalyst surface active metal that contains phosphide is uniformly dispersed, and to have the hydrogenation catalyst ability strong, the catalyzer carbon accumulation resisting ability is good, can the operational condition that comparatively relaxes be issued to distillate deep desulfuration, take off virtue, produce qualified aviation fuel.
Embodiment
Below describe realization and the characteristics of the present invention of the object of the invention in detail by specific embodiment, but practical range of the present invention is not consisted of any restriction.
Embodiment 1
Al is pressed in the carrier preparation
2O
3Compare SiO
2Weight feeds intake at 1: 4, takes by weighing aluminum nitrate and silicon sol (contains SiO
230%), then add the weak ammonia titration, regulate pH value 7.0-8.0, aging 90min, suction filtration, behind 120 ℃ of dry 8h, extruded moulding on banded extruder through 450-550 ℃ of roasting 4h, makes support of the catalyst again with filter cake.11.13g ammonium hypophosphite, 39.14g nickelous nitrate, 5.0g citric acid are dissolved in the deionized water, and dipping solution impregnated on the 50g carrier, 80～250 ℃ of lower oven dry, contains Ni through what 350～400 ℃ of roastings obtained again
2The precursor of the catalyzer of the active phase of P.The logical H of catalyzer precursor with gained
2S vulcanizes, and obtains catalyst n i
2P-NiS/ γ-Al
2O
3The called after catalyst A.
Embodiment 2
The preparation of the catalyzer of embodiment 2 is according to the same method of embodiment 1, and wherein the catalyst activity metal forms difference, adds tungsten when impregnated catalyst, the called after catalyst B, and see Table 1 concrete the composition.
Embodiment 3
The preparation of the catalyzer of embodiment 3 is according to the same method of embodiment 2, and wherein the catalyst activity metal forms difference, adds cobalt metal when impregnated catalyst, called after catalyzer C, and see Table 1 concrete the composition.
Embodiment 4
Al is pressed in the carrier preparation
2O
3Compare SiO
2Weight 1: 4, Al
2O
3Feed intake at 3: 1 than ZrO2 weight, take by weighing aluminum nitrate, zirconium nitrate and silicon sol and (contain SiO
230%), then add the weak ammonia titration, regulate pH value 7.0-8.0, aging 90min, suction filtration, behind 120 ℃ of dry 8h, extruded moulding on banded extruder through 450-550 ℃ of roasting 4h, makes support of the catalyst again with filter cake.8.45g ammonium hypophosphite, 29.48g nickelous nitrate, 3.7g citric acid and 2.46g ammonium metawolframate are dissolved in the deionized water, and dipping solution impregnated on the 50g carrier, 80～250 ℃ of lower oven dry, contains Ni through what 350～400 ℃ of roastings obtained again
2The precursor of the catalyzer of the active phase of P.The logical H of catalyzer precursor with gained
2S vulcanizes, and obtains catalyst n i
2P-NiWS/ γ-Al
2O
3Called after catalyzer D.
Embodiment 5
The preparation of the catalyzer of embodiment 5 is according to the same method of embodiment 4, and wherein support of the catalyst forms difference, presses Al
2O
3Feed intake at 2: 1 than ZrO2 weight, called after catalyzer E, see Table 1 concrete the composition.
Embodiment 6
The preparation of the catalyzer of embodiment 6 is according to the same method of embodiment 4, and wherein support of the catalyst forms difference, presses Al
2O
3Feed intake at 1: 1 than ZrO2 weight, called after catalyzer F, see Table 1 concrete the composition.
Comparative Examples 1
Carrier adopts the carrier preparation method among the embodiment 5, and identical among total metal content and the embodiment 5 is prepared into the sulphided state hydrogenation catalyst, and concrete composition sees Table 1.
Comparative Examples 2
Adopt a kind of commercial hydrogenation catalyst of widespread use, the catalyst metal composition sees Table 1.
Table 1 embodiment catalyzer forms data
| Project | A | B | C | D | E | F | Comparative Examples 1 | Comparative Examples 2 |
| Ni，％ | 15.8 | 11.9 | 10.3 | 11.9 | 11.9 | 11.9 | 11.8 | 5.4 |
| W，％ | 3.3 | 3.3 | 3.3 | 3.3 | 3.3 | 4.2 | 15.5 | |
| Co，％ | 1.6 | |||||||
| P，％ | 8.3 | 6.3 | 5.4 | 6.3 | 6.3 | 6.3 | 3.0 | |
| ZrO2，％ | 4.2 | 8.3 | 17.0 | 8.3 | ||||
| Specific surface area, m 2/g | 202.0 | 210.0 | 205.0 | 198.0 | 190.0 | 187.0 | 203.0 | 230 |
| Pore volume, ml/g | 0.42 | 0.45 | 0.46 | 0.50 | 0.51 | 0.51 | 0.50 | 0.33 |
| Intensity, N/mm | 20.1 | 19.0 | 19.4 | 16.8 | 17.0 | 15.0 | 16.7 | 16.8 |
Embodiment 7
This case introduction activity rating of catalyst process.
Adopting a kind of aviation kerosene is raw material, and feedstock property sees Table 2.
Catalyzer in embodiment and the Comparative Examples is carried out the evaluation tests in 500 hours of the same terms, sampling analysis product mercaptan sulfur, total sulfur content and smoke point value, analytical results is averaged and is seen Table 3.Catalyst loading and appreciation condition are as follows:
Estimating with device is the 20ml fixed-bed reactor, and the reactor interlude can be realized thermostatic control, and evaluate catalysts is got length between 2-5mm, is seated in the control that the reactor interlude is beneficial to temperature of reaction, and upper-lower section loads N with 20-30 order quartz sand
2Airtight qualified rear temperature programming, 150 ℃ of dry 2h, logical hydrogen advance raw material boat coal, are raised to 340 ℃ of temperature of reaction with the speed of 20 ℃/h.Appreciation condition: reaction pressure 5.0MPa, raw material volume space velocity 3.0h
-1, hydrogen-oil ratio 500: 1.
Table 2 catalyst activity is estimated stock oil character
The result can find out from table 3 catalyst activity, adopt the standby catalyzer that contains phosphide of patent system of the present invention higher than the hydrogenation activity of conventional sulfide catalyst, can realize reducing working pressure, temperature, under the condition of higher position reason air speed, reduce loaded catalyst, increase economic efficiency, that the novel high-activity oil hydrogenation is processed catalyzer, process boat coal raw material inferior in the decrease mercaptan sulfur, can improve significantly the product smoke point, improve quality product.
Table 3 catalyst activity evaluation result
Claims (3)
1. the method for an aviation kerosene hydrotreatment inferior is characterized in that:
The catalyzer of catalytic hydroprocessing is the composite catalyst of one or more and P in cobalt, molybdenum, nickel, the tungsten metal; Take catalyst weight as 100%, metal component accounts for 5～50%; It is 5～30% that phosphide accounts for; Surplus is carrier;
Carrier is resistant to elevated temperatures inorganic porous oxide material, and the carrier specific surface area is 150-350m after the moulding
2/ g, pore volume are 0.10-0.80ml/g, and mean pore size is 3-15nm, and face shaping is sphere, bar shaped or sheet;
The preparation method of catalyzer: (1) is at first with ammonium hypophosphite and contain Co, Ni, Mo or/and the metal-salt of W, in deionized water, dissolve, add complexing agent and be made into metal impregnation liquid, then shaping carrier is dropped in the steeping fluid and filter after 1-2 hour, 120 ℃ of oven dry;
(2) obtain having the metal that contains Co, Ni, Mo or W and the catalyzer of P by calcination process, 200～400 ℃ for the treatment of temps, the treatment time is 2～10h;
The catalyst vulcanization that (3) then will contain above-mentioned phosphide is processed and to be prepared into the sulphided state catalyzer, and the pre-curing temperature of catalyzer is 250～450 ℃, and curing time is 10h.
2. according to the method for aviation kerosene hydrotreatment inferior claimed in claim 1, it is characterized in that: resistant to elevated temperatures inorganic porous oxide material is Al
2O
3, SiO
2, SiO
2-Al
2O
3, TiO
2, ZrO
2, in molecular sieve or the amorphous aluminum silicide one or more, in the carrier preparation process by ammoniacal liquor, organic acid control pH value 7.0-8.0.
3. according to the method for aviation kerosene hydrotreatment inferior claimed in claim 1, it is characterized in that: fixed-bed reactor are adopted in hydrotreatment, and at pressure 3.0-6.0MPa, temperature 250-400 ℃, air speed are 1.5-5.0h
-1With hydrogen-oil ratio be hydrogenating desulfurization under the condition of 150-800/1.
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Cited By (5)
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| CN109603839A (en) * | 2019-01-09 | 2019-04-12 | 泰州学院 | A kind of preparation method of figure cobalt molybdenum Hydrobon catalyst |
| CN109722290A (en) * | 2017-10-27 | 2019-05-07 | 中国石油化工股份有限公司 | Reduce the method that height does boat coal freezing point |
| CN112871201A (en) * | 2021-03-15 | 2021-06-01 | 云南师范大学 | Multi-element/composite semiconductor photocatalytic material for preparing aviation kerosene by photo-thermal coupling catalysis of biomass and preparation method and application thereof |
| CN116060049A (en) * | 2021-10-29 | 2023-05-05 | 中国石油化工股份有限公司 | Hydrogenation catalyst and preparation method and application thereof |
| CN116474797A (en) * | 2022-01-13 | 2023-07-25 | 中国石油化工股份有限公司 | Silicon-containing hydrogenation catalyst and preparation method and application thereof |
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| CN109722290A (en) * | 2017-10-27 | 2019-05-07 | 中国石油化工股份有限公司 | Reduce the method that height does boat coal freezing point |
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| CN112871201A (en) * | 2021-03-15 | 2021-06-01 | 云南师范大学 | Multi-element/composite semiconductor photocatalytic material for preparing aviation kerosene by photo-thermal coupling catalysis of biomass and preparation method and application thereof |
| CN112871201B (en) * | 2021-03-15 | 2023-04-18 | 云南师范大学 | Multi-element/composite semiconductor photocatalytic material for preparing aviation kerosene through photo-thermal coupling catalysis of biomass, and preparation method and application thereof |
| CN116060049A (en) * | 2021-10-29 | 2023-05-05 | 中国石油化工股份有限公司 | Hydrogenation catalyst and preparation method and application thereof |
| CN116060049B (en) * | 2021-10-29 | 2024-05-10 | 中国石油化工股份有限公司 | Hydrogenation catalyst and preparation method and application thereof |
| CN116474797A (en) * | 2022-01-13 | 2023-07-25 | 中国石油化工股份有限公司 | Silicon-containing hydrogenation catalyst and preparation method and application thereof |
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Application publication date: 20130327 |