CN1083476C - Hydrorefining catalyst for fraction oil and its preparing process - Google Patents
Hydrorefining catalyst for fraction oil and its preparing process Download PDFInfo
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- CN1083476C CN1083476C CN99113281A CN99113281A CN1083476C CN 1083476 C CN1083476 C CN 1083476C CN 99113281 A CN99113281 A CN 99113281A CN 99113281 A CN99113281 A CN 99113281A CN 1083476 C CN1083476 C CN 1083476C
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- catalyst
- distillate oil
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- hydrorefining distillate
- hydrorefining
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Abstract
The present invention discloses a hydrofining catalyst for distillate oil and a preparation method thereof. The catalyst is prepared by using alumina or silicon contained alumina as a carrier, using W, Mo and Ni as active components and adding P as an auxiliary agent. By using a sectional co-immersion technique, the metal distribution on the catalyst is more uniform, and the activity of the catalyst, particularly the hydrodenitrogenation activity, is greatly enhanced.
Description
The present invention relates to a kind of catalyst for hydrorefining distillate oil and preparation method thereof.
Typical Hydrobon catalyst, being carrier with aluminum oxide or siliceous aluminum oxide often, is active ingredient with VIII family and group vib metallic element, in order to improve activity of such catalysts and stability, normal adopt multiple improving one's methods, as to support modification, optimize the preparation method, add auxiliary agent etc.Auxiliary agent commonly used has P, F, B, Ti, Zr etc.Chinese patent CN86107828A has made the W-Mo-Ni-P co-impregnated solution, and adopt one to go on foot the immersion process for preparing catalyzer, but adopt a step immersion process for preparing catalyzer that several point defects are arranged: when 1) the W-Mo-Ni-P co-impregnated solution adopts one section dipping, because strength of solution height, metal component disperses bad on carrier, easily generate nonactive phase, thus the loss activity of such catalysts; 2) the W-Mo-Ni-P soltion viscosity of high density is big, and the moist catalysis behind dipping bonding easily is agglomerating, causes metal-salt to decompose in roasting process not exclusively, thereby catalyst activity is had infringement; 3) only use nickelous carbonate in this patent, dissolved NiO concentration is less in the co-impregnated solution, and NiO content＜3.0% (W) on the final catalyzer is not in the optimum content scope.
The purpose of this invention is to provide a kind of Hydrobon Catalyst And Its Preparation Method, further improve hydrofining activity, the especially denitrification activity of catalyzer.
The composition and the physico-chemical property of catalyzer of the present invention are as follows:
With aluminum oxide or siliceous aluminum oxide is carrier, is active ingredient with W, Mo, Ni, and for helping catalyst component, in catalyst weight, each component concentration is respectively WO with P
313%～25%, MoO
36%～14%, NiO2%～7%, P
2O
51%～9%; WO preferably
3Be 16%～22%, MoO
37%～11%, NiO3%～5%, P
2O
52%～7%; Described active ingredient and to help catalyst component be to load on the support of the catalyst by the substep mode of soaking is altogether promptly carried out at least double-steeping with load active component with help catalyst component with the co-impregnated solution that contains W, Mo, Ni, P to support of the catalyst; 0.22～0.37 milliliter/gram of catalyzer pore volume, 110～170 meters of specific surface areas
2/ gram.
Preparation of catalysts method of the present invention is as follows:
Catalyzer of the present invention is a carrier with aluminum oxide or siliceous aluminum oxide, is active ingredient with W-Mo-Ni, adds the P auxiliary agent, through 70～120 ℃ of heating, makes stable W-Mo-Ni-P co-impregnated solution.With above-mentioned co-impregnated solution with the mode impregnated carrier of secondary at least (promptly substep soaks altogether), preferred 2～4 times.Moist catalysis was through 80～150 ℃ of dryings 2～8 hours, and 450～550 ℃ of roastings made in 2～5 hours.
The preparation of described aluminum oxide or siliceous alumina supporter can be that aluminum oxide is added peptization solvent and extrusion aid or silicon sol, mixes and pinches the back extruded moulding or drip ball forming, makes in 2～5 hours through 2～8 hours, 500～650 ℃ roastings of 80～150 ℃ of dryings.Described aluminum oxide can be the macropore aluminium hydrate powder that adopts aluminum chloride-ammoniacal liquor method, Tai-Ace S 150-sodium metaaluminate method, carborization and alkyl aluminum hydrolysis method to make.
The compound method of W-Mo-Ni-P co-impregnated solution can be: tungsten compound, nickel compound, molybdenum compound, phosphorus compound and deionized water are added in the there-necked flask simultaneously, stir after 70～120 ℃ of heating make stable co-impregnated solution.
Above-mentioned tungsten compound can be one or more in ammonium metawolframate, wolframic acid or other the alkaline tungstate, preferably ammonium metawolframate; Molybdenum compound can be one or more in molybdic oxide or the ammonium molybdate, preferably molybdic oxide; Nickel salt can be at least a in nickelous carbonate, nickelous nitrate and the nickel acetate, better is two kinds, preferably nickelous carbonate and nickelous nitrate; Phosphorus compound is a phosphoric acid;
Each component concentrations is in the described co-impregnated solution:
WO
3:/100 milliliters of 10～40 grams, NiO:2～10 restrain/100 milliliters, MoO
3:/100 milliliters of 5～20 grams, P
2O
5:/100 milliliters of 2～8 grams.
Can adopt saturated dipping under the room temperature the method supported catalyst active ingredient and help catalyst component.
Described extrusion aid can be: one or more in sesbania powder, citric acid, the acetic acid.
Above-mentioned peptizing agent is: one or more in nitric acid, hydrochloric acid and the deionized water.
Compared with prior art, catalyzer of the present invention not only overcomes the shortcoming that one step of prior art dipping brings, and the catalyzer that adopts the inventive method to prepare, when the processing poor quality is urged bavin, its hydrodenitrogenationactivity activity exceeds about 50% than W-Mo-Ni-B catalyzer, W-Mo-Ni-P catalyzer than one section dipping is high by about 35%, and this catalyzer is higher by about 45% than the W-Mo-Ni-P catalyst activity that the substep pickling process makes.This catalyzer has very high hydrofining activity to distillate, is specially adapted to 80～370 ℃ straight run oil, the hydrodenitrification and the hydrogenating desulfurization of secondary processing oil.
Further set forth feature of the present invention below in conjunction with specific examples.
Embodiment 1
With macropore aluminium hydrate powder 1000g, add 20 milliliters in nitric acid, 700 milliliters of deionized waters and the mixing of 25g sesbania powder and roll, become trifolium-shaped through extrusion, 3 hours, 550 ℃ roastings of 110 ℃ of dryings made carrier T-1 in 3 hours.
Embodiment 2
With macropore aluminium hydrate powder 900g, add 18 milliliters in nitric acid, 600 milliliters of deionized waters, silicon sol 450g and the mixing of 22g sesbania powder and roll, become trifolium-shaped through extrusion, 3 hours, 550 ℃ roastings of 110 ℃ of dryings made carrier T-2 in 3 hours.
Comparative example 1
Use ammonium metawolframate 67g, nickelous nitrate 35g adds 110 milliliters of deionized waters, and stirring and dissolving gets the W-Ni aqueous solution, adopts saturated pickling process to flood this solution with above-mentioned carrier T-1150g, and wet bar was through 110 ℃ of dryings 3 hours, and 480 ℃ of roastings are standby after 2 hours, are numbered A-1A.With the 27g molybdic oxide, the 10g nickelous carbonate, 14g phosphoric acid is with after 120 ml deionized water are mixed, be warming up to 90 ℃ of constant temperature 2 hours, and obtained Mo-Ni-P solution, after above-mentioned work in-process A-1A adopts saturated pickling process to flood this solution, through 110 ℃ of dryings 3 hours, 480 ℃ of roastings 3 hours made catalyst A.
Comparative example 2
Ammonium metawolframate 90 grams, nickelous carbonate 26.5 grams, molybdenum oxide 35.5 grams, phosphatase 11 9 grams and 120 ml deionized water are mixed, and are warming up to 80 ℃ of dissolvings 2 hours then, obtain the W-Mo-Ni-P co-impregnated solution, be diluted to 200 milliliters with deionized water, the 200 carrier T-1s of gram after the roastings flooded under room temperature with above-mentioned steeping fluid, through 120 ℃ of dryings 3 hours, 500 ℃ of roastings 3 hours obtain catalyst B.
Embodiment 3
Ammonium metawolframate 90 grams, nickelous carbonate 26.5 grams, molybdenum oxide 35.5 grams, phosphatase 11 9 grams and 120 ml deionized water are mixed, be warming up to 85 ℃ of dissolvings 3 hours then, obtain the W-Mo-Ni-P co-impregnated solution, be diluted to 400 milliliters with deionized water, the carrier T-1 after the 200 gram roastings floods under room temperature with above-mentioned steeping fluid, through 110 ℃ of dryings 3 hours, 500 ℃ of roastings were flooded under room temperature with above-mentioned steeping fluid after 2 hours, and drying and roasting make final catalyzer again, and catalyzer is numbered C.
Embodiment 4
Metal-salt add-on and compound method are identical with embodiment 3, and the distilled water consumption is 400 milliliters, and final volume is 600 milliliters, divide dipping preparation catalyzer three times, and each dipping finishes and all needs drying and roasting, and final catalyzer is numbered D.
Embodiment 5
Ammonium metawolframate 90 grams, nickelous carbonate 26.5 grams, molybdenum oxide 35.5 grams, phosphatase 11 9 grams and 120 ml deionized water are mixed, be warming up to 110 ℃ of dissolvings 1 hour then, add nickelous nitrate 55g again, obtain the W-Mo-Ni-P co-impregnated solution after the stirring and dissolving, be diluted to 400 milliliters with deionized water, the carriers of 200 grams after the roastings flood under room temperature with above-mentioned steeping fluid, and through 150 ℃ of dryings 2 hours, 480 ℃ of roastings were flooded under room temperature with above-mentioned steeping fluid after 2 hours, drying and roasting make final catalyzer again, and catalyzer is numbered E.
Embodiment 6
Ammonium metawolframate 73 grams, nickelous carbonate 26.5 grams, molybdenum oxide 58 grams, phosphatase 11 9 grams and 120 ml deionized water are mixed, be warming up to 75 ℃ of dissolvings 3 hours then, obtain the W-Mo-Ni-P co-impregnated solution, be diluted to 400 milliliters with deionized water, the carrier T-1 after the 200 gram roastings floods under room temperature with above-mentioned steeping fluid, through 110 ℃ of dryings 3 hours, 500 ℃ of roastings were flooded under room temperature with above-mentioned steeping fluid after 2 hours, and drying and roasting make final catalyzer again, and catalyzer is numbered F.
Embodiment 7
Method for preparing catalyst is identical with comparative example 1, but the phosphoric acid add-on is 25g, and final catalyzer is numbered G.
Embodiment 8
Method for preparing catalyst is identical with embodiment 3, but carrier T-2, final catalyzer is numbered H.
Embodiment 9
With Iranian catalytic diesel oil is raw material, is 6.0MPa at hydrogen pressure, hydrogen-oil ratio 300: 1, air speed 2.0h
-1, temperature of reaction is under 330 ℃ the condition, catalyzer of the present invention and existing commercial catalysts (W-Mo-Ni-B) to be carried out active comparative evaluation, stock oil character and evaluation result see Table 1 and table 2 respectively.
The Iranian catalytic diesel oil character of table 1
| Density (20 ℃), g/cm 3 | 0.9227 |
| IBP/10％ | 197/236 |
| 30％/50％ | 256/275 |
| 70％/90％ | 307/320 |
| 95％/EBP | 336/339 |
| Sulphur content, w% | 0.71 |
| The alkali nitrogen content, PPm | 146 |
| Nitrogen content, PPm | 1203 |
Table 2 catalyst activity comparative evaluation result
Annotate: the reference agent is industrial commercial catalyst commonly used.
| The catalyzer numbering | Form | Corresponding carrier | The hydrodenitrification relative reactivity, % | |||
| WO 3 | MoO 3 | NiO | B 2O 3/P 2O 5 | |||
| The reference agent | 18.7 | 9.3 | 4.5 | 4.1/ | T-1 | 100 |
| A | 19.1 | 9.2 | 4.2 | /3.0 | T-1 | 98 |
| B | 19.5 | 9.1 | 2.7 | /3.0 | T-1 | 105 |
| C | 18.9 | 9.4 | 2.8 | /3.1 | T-1 | 136 |
| D | 20.3 | 9.3 | 2.7 | /3.0 | T-1 | 141 |
| E | 19.5 | 9.1 | 4.2 | /3.0 | T-1 | 150 |
| F | 14.5 | 13.6 | 2.8 | /3.1 | T-1 | 95 |
| G | 18.5 | 10.3 | 4.3 | /5.8 | T-1 | 96 |
| H | 19.1 | 9.2 | 4.1 | /3.1 | T-2 | 155 |
As can be seen from the above table, adopt substep to soak the catalyzer of the present invention of technology preparation altogether, catalyst A, B than reference agent and employing step impregnation and step dipping preparation have higher hydrodenitrogenationactivity activity, and adopt the catalyzer E of mixing nickel salt preparation to have higher hydrodenitrogenationactivity activity.
Claims (18)
1. a catalyst for hydrorefining distillate oil is an active ingredient with VIII family and group vib metal, adds phosphate builder, with aluminum oxide or siliceous aluminum oxide is carrier, with W, Mo, Ni is active ingredient, for helping catalyst component, it is characterized in that catalyzer consists of by weight: WO with P
313%～25%, MoO
36～14%, NiO
2%～7%, P
2O
51%～9%; 0.22～0.37 milliliter/gram of catalyzer pore volume, 110～170 meters of specific surface areas
2/ gram.
2. according to the described catalyst for hydrorefining distillate oil of claim 1, it is characterized in that described active ingredient and helping catalyst component is to load on the support of the catalyst by the mode that substep soaks altogether.
3. according to the described catalyst for hydrorefining distillate oil of claim 1, it is characterized in that described WO
3Weight percent with catalyzer is a benchmark, is 16%～22%.
4. according to the described catalyst for hydrorefining distillate oil of claim 1, it is characterized in that described MoO
3Weight percent with catalyzer is a benchmark, is 7%～11%.
5. according to the described catalyst for hydrorefining distillate oil of claim 1, it is characterized in that described NiO is a benchmark with the weight percent of catalyzer, is 3%～5%.
6. according to the described catalyst for hydrorefining distillate oil of claim 1, it is characterized in that described P
2O
5Be 2%～7%.
7. the preparation method of a catalyst for hydrorefining distillate oil, comprise: with aluminum oxide or siliceous aluminum oxide is carrier, with W, Mo, Ni is active ingredient, add the P auxiliary agent, make W, Mo, Ni, P co-impregnated solution with W, Mo, Ni, P-compound, after 70～120 ℃ of heating, the mode impregnated carrier that described co-impregnated solution is soaked altogether with gradation, after 80～150 ℃ of dryings 2～8 hours, 450～550 ℃ of roastings made in 2～5 hours.
8. according to the preparation method of the described catalyst for hydrorefining distillate oil of claim 7, it is characterized in that the dipping number of times that described gradation is soaked altogether is 2～4 times.
9. according to the preparation method of the catalyst for hydrorefining distillate oil of claim 7, it is characterized in that described tungsten compound is one or more in wolframic acid or the quaternary ammonium tungstate.
10. according to the preparation method of the catalyst for hydrorefining distillate oil of claim 7, it is characterized in that described molybdenum compound be in molybdic oxide or the ammonium molybdate one or more.
11. according to the preparation method of the catalyst for hydrorefining distillate oil of claim 7, it is characterized in that nickel compound be at least a in nickelous carbonate, nickelous nitrate and the nickel acetate.
12. the preparation method according to the catalyst for hydrorefining distillate oil of claim 7 is characterized in that described P-compound is one or more in phosphoric acid or the phosphorous acid.
13., it is characterized in that described tungsten compound is an ammonium metawolframate according to the preparation method of claim 7 or 9 described catalyst for hydrorefining distillate oil.
14., it is characterized in that described molybdenum compound is a molybdic oxide according to the preparation method of claim 7 or 10 described catalyst for hydrorefining distillate oil.
15., it is characterized in that described nickel compound is nickelous carbonate and nickelous nitrate according to the preparation method of claim 7 or 11 described catalyst for hydrorefining distillate oil.
16., it is characterized in that described phosphorus compound is a phosphoric acid according to the preparation method of claim 7 or 12 described catalyst for hydrorefining distillate oil.
17. according to the preparation method of the described catalyst for hydrorefining distillate oil of claim 7, the concentration that it is characterized in that described co-impregnated solution is WO
3/ 100 milliliters of 10～40 grams, NiO2～10 restrain/100 milliliters, MoO
3/ 100 milliliters of 5～20 grams, P
2O
5/ 100 milliliters of 2～8 grams.
18. according to the described catalyst for hydrorefining distillate oil preparation method of claim 7, it is characterized in that the temperature of described solution preparation is 70～120 ℃, dissolution time is 0.3～3 hour.
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|---|---|---|---|
| CN99113281A CN1083476C (en) | 1999-09-29 | 1999-09-29 | Hydrorefining catalyst for fraction oil and its preparing process |
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| CN99113281A CN1083476C (en) | 1999-09-29 | 1999-09-29 | Hydrorefining catalyst for fraction oil and its preparing process |
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| CN1083476C true CN1083476C (en) | 2002-04-24 |
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