CN102784656A - Hydro-fining catalyst roasted at low temperature and preparation method thereof - Google Patents
Hydro-fining catalyst roasted at low temperature and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a hydro-fining catalyst roasted at a low temperature and a preparation method thereof. The preparation method comprises the following steps of: taking aluminum hydroxide dry glue or modified aluminum hydroxide dry glue as a raw material to prepare a catalyst carrier, then impregnating metal active components in VIB and VIII groups and preparing the hydro-fining catalyst through drying and roasting. The content of an alumina carrier is 60-90 weight percent, the content of metallic oxide in the VIB group is 5-35 weight percent, and the content of metallic oxide in the VIII group is 1-10 weight percent. An activity phase of the catalyst has proper stacking layer number and film crystal length, the interaction between the carrier and metal is reduced, the better dispersion state of the active components can be kept, and the HDS (Hydro-desulfurization) ability of sulfide difficult to remove in an oil product is improved. The hydro-fining catalyst is particularly suitable for the hydro-desulfurization of naphtha, the hydro-fining of inferior diesel oil and the hydro-treatment of FCC (Fluid Catalytic Cracking) raw materials or hydro-cracking raw materials and other distillate oil.
Description
Technical field:
The present invention relates to a kind of Hydrobon Catalyst And Its Preparation Method; This catalyst adopt low-temperature bake degrading activity component predecessor control reactive metal the dispersive property of carrier surface and with carrier interactions intensity; Improve activity of such catalysts and stability, reduce the Preparation of catalysts cost.Prepared catalyst has higher desulfurization, denitrification activity; Be specially adapted to the hydrofinishing of distillate; Like the hydrotreatment of hydrodesulfurizationof of naphtha, poor ignition quality fuel hydrofinishing, FCC raw material or hydrocracking raw material etc., can satisfy the hydrorefined production requirement of cleaning oil product.
Background technology:
Hydrofinishing is technology important in the petroleum refining process, and this technology has great importance for the processing characteristics of improving secondary operations charging (catalytic cracking and hydrocracking etc.) and raising oil product (vapour, diesel oil etc.) quality.The key of hydrofinishing technology is catalyst, and present hydrorefined catalyst is many to be carrier with aluminium oxide or modified aluminas, is active component with VI B family's metal molybdenum and/or tungsten with VIII family metallic nickel and/or cobalt, and the employing immersion process for preparing forms.The Preparation of catalysts process does; At first prepare aluminium oxide or modified aluminium oxide supports; With VI B family's metal molybdenum and/or tungsten and VIII family metallic nickel and/or cobalt is that active component is mixed with maceration extract, adopts one or many dipping method impregnated carrier, is prepared from catalyst through super-dry, roasting.
Roasting is one of committed step in the catalyst preparation process, it be the degrading activity metal precursor form active mutually or the committed step of active phase presoma, also be the committed step that influence active component and carrier interaction and active character mutually.Select suitable sintering temperature and roasting time in the catalyst preparation process, help improving reactive metal the dispersive property of carrier surface and and carrier interactions, thereby the hydrofinishing that improves catalyst is active and stable.For this reason, obtained paying attention to widely and studying.Patent CN101089132A discloses a kind of catalyst for hydrodesulfurizationfraction fraction oil and preparation method thereof; This catalyst is being carrier with aluminium oxide or siliceous aluminium oxide; With Co, Mo, Ni, W is active component; Once saturated impregnated carrier, through 80-150 ℃ of dry 2-8 hour, 350-550 ℃ made in roasting 2-5 hour.
In order to reduce the production stage of catalyst, US5198100, US5336654 and US5338717 disclose and have a kind ofly come impregnated carrier to prepare the method for hydrotreating catalyst through the heteropolyacid salt with VI B family's metal and VIII family metal.This catalyst can use in reactor is directly packed in roasting into, but catalyst use before during sulfuration, need be dry under high vacuum condition, remove the whole moisture in the catalyst, give and use and operation has caused difficult and do not promoted the use of.
Chinese patent CN101279289A and CN101279291A a kind of preparation method of hydrotreatment catalyst of openly knowing clearly; It is characterized in that catalyst carrier is in the supported active metal component or introduce organic compound afterwards again; A kind of active component of every introducing or organic compound; All need carry out drying, have one or more drying steps in the catalyst preparation process.This preparation method can effectively improve carrier surface character, helps reactive metal and disperses and activation, improves the serviceability of catalyst.But owing to lack calcination steps; Interaction between metal-carrier weakens greatly, causes the activity at catalyst initial stage very high, but along with the prolongation in reaction time; Reactive metal can be assembled gradually; Active sites can reduce gradually, and activity of such catalysts descends gradually, influences activity of such catalysts stability.
Summary of the invention:
Deficiency to prior art; Technical problem to be solved by this invention provides the hydrorefined Catalysts and its preparation method of a kind of low-temperature bake; This method earlier is prepared into carrier with aluminum hydroxide solid elastomer or modified aluminum hydroxide solid elastomer on the basis that does not change original Hydrobon catalyst technological process and prescription, VI B family's metal molybdenum and/or tungsten and VIII family metallic nickel and/or cobalt are mixed with solution; Impregnated carrier prepares catalyst through dry and low-temperature bake.
Technical problem of the present invention adopts following technical scheme to solve:
Described catalyst is to be carrier with aluminium oxide or modified aluminas; With VI B family's metal and VIII family metal is that active component is prepared from; Wherein, The content of aluminium oxide or modified aluminium oxide supports is 60-90wt%, and VI B family metal oxide content is 5-35wt%, and VIII family metal oxide content is 1-10wt%.
Above-mentioned Preparation of catalysts method may further comprise the steps:
The first step: preparation catalyst carrier.In aluminum hydroxide solid elastomer or modified aluminum hydroxide solid elastomer, add binding agent with extrusion aid after mix pinch, extruded moulding, 80 ℃-150 ℃ times dry 1-20 hour, processed catalyst carrier again at 400 ℃ of-700 ℃ of following roasting 2-12 hours.Described modified aluminum hydroxide solid elastomer is the aluminum hydroxide solid elastomer of one or more modifications in silicon, boron, titanium, zirconium and the fluorine etc., and wherein silicon, boron, titanium, zirconium or fluorine are the 2%-50% of aluminum hydroxide solid elastomer quality in the mass content of oxide, preferred 5%-20%; Described baking temperature is the best with 100 ℃-120 ℃, is preferably 4-12 hour drying time; Preferred 500 ℃-600 ℃ of described sintering temperature; The preferred 3-6 of roasting time hour.
Described binding agent is one or more in nitric acid, citric acid, acetic acid and the oxalic acid, and addition is the 1-10% of aluminum hydroxide solid elastomer gross weight, is best with 3-5%.
Described extrusion aid is one or more in sesbania powder, active carbon and the polyvinyl alcohol etc., and addition is the 2-10% of aluminum hydroxide solid elastomer gross weight, is best with 3-5%.
Second step: preparation maceration extract.With nickeliferous and/or cobalt compound, contain molybdenum and/or tungsten compound and auxiliary agent and be mixedly configured into the aqueous solution.
Described nickeliferous and/or cobalt compound is one or more in basic nickel carbonate and/or basic cobaltous carbonate, nickel nitrate and/or cobalt nitrate, nickel oxalate and/or cobalt oxalate and nickel acetate and/or the cobalt acetate; Molybdate compound is ammonium molybdate and/or molybdenum oxide; Tungstenic compound is ammonium tungstate and/or ammonium metatungstate; Phosphorus-containing compound is one or more in phosphoric acid, ammonium hydrogen phosphate and the ammonium dihydrogen phosphate (ADP), and said auxiliary agent is one or more in phosphoric acid, citric acid, ammoniacal liquor or the ethylenediamine.
Preparation during maceration extract the addition of each compound be to calculate out with the content of its oxide in the catalyst, be benchmark with the weight of catalyst, require wherein to comprise: molybdenum trioxide and/or tungstic acid 5-35wt%, preferred 15-25wt%; Nickel oxide and/or cobalt oxide 1-10wt%, preferred 2-5wt%; P
2O
5Be 0.5-5wt%, preferred 1-3wt%.
The 3rd step: preparation catalyst.Adopt equi-volume impregnating, the aqueous solution that second step was prepared sprays on the catalyst carrier of first step gained, and dipping is after drying and roasting make catalyst according to the invention.Described baking temperature is 80 ℃-150 ℃, with 100 ℃-120 ℃ be the best, be 1-10 hour drying time, was the best with 2-5 hour; Described sintering temperature is 150 ℃-550 ℃, and preferred 180 ℃-250 ℃, roasting time is 2-10 hour, preferred 3-5 hour.
The catalyst of preparation is specially adapted to the hydrotreatment of hydrodesulfurizationof of naphtha, poor ignition quality fuel hydrofinishing, FCC raw material or hydrocracking raw material as stated above.
The invention has the beneficial effects as follows: since adopt low-temperature bake degrading activity component predecessor controlled reactive metal the dispersive property of carrier surface and with carrier interactions intensity; Improve activity of such catalysts and stability, reduced the Preparation of catalysts cost.
The specific embodiment:
Further describe technical characterictic of the present invention below in conjunction with embodiment and comparative example, but be not limited to embodiment.
Embodiment 1:
Take by weighing fluorine-containing 2wt%, contain the modified aluminum hydroxide solid elastomer 100g of zirconia 6wt%; Add citric acid and each 3g of sesbania powder, after carbon black 5g mixed, adding 90ml concentration was 3% dilute nitric acid solution; Mix the back extruded moulding; Institute's moulding bar that obtains 120 ℃ dry 4 hours down, 550 ℃ of following roastings 4 hours, preparation carrier S-1.The character of carrier S-1 is as shown in table 1.
The physico-chemical property of table 1 carrier S-1
To contain the maceration extract incipient impregnation catalyst carrier S-1 of an amount of molybdenum trioxide, basic nickel carbonate and phosphoric acid, soaked carrier to be descended dry 4 hours at 120 ℃, 200 ℃ of following roastings made catalyst C-1 in 4 hours.The catalyst that makes contains the molybdenum (in oxide) of 22wt%, and the phosphorus of 4wt% nickel (in oxide) and 1.5wt% is (with P
2O
5Meter).Comparative Examples 1:
To contain the maceration extract incipient impregnation catalyst carrier S-1 of same amount molybdenum trioxide, basic nickel carbonate and phosphoric acid, soaked carrier was made contrast medium RA-1 in 4 hours 120 ℃ of dryings.
Containing the maceration extract incipient impregnation catalyst carrier S-1 of same amount molybdenum trioxide, basic nickel carbonate and phosphoric acid, 120 ℃ of dryings 4 hours, 350 ℃ of roastings made contrast medium RA-2 in 4 hours with soaked carrier.
Containing the maceration extract incipient impregnation catalyst carrier S-1 of same amount molybdenum trioxide, basic nickel carbonate and phosphoric acid, 120 ℃ of dryings 4 hours, 480 ℃ of roastings made contrast medium RA-3 in 4 hours with soaked carrier.
Activity adopts transmission electron microscope observing to find mutually behind the catalyst vulcanization of different sintering temperatures preparations, mutually active because MoS behind the prepared catalyst vulcanization of the present invention
2The stacking number of plies is more, and platelet length is shorter, has more active higher activated centres, edge, and the reactive metal decentralization is higher.
Table 2 has provided different sintering temperature catalyst MoS
2The average stacking number of plies, average lamella length and Mo atom decentralization statistic analysis result.
The average stacking number of plies of table 2 different catalysts, average lamella length and Mo atom decentralization
Annotate: the average stacking number of plies of Na-;
The average lamella length of La-, nm;
f
MoThe decentralization of-Mo atom, i.e. the shared ratio of position, corner Mo atom, %.
Catalyst and contrast medium active appraisal experiment carry out on 100ml fixed bed hydrogenation experimental provision, and feedstock oil is straight-run gas oil and wax tailings.Before the activity rating catalyst is carried out presulfurization.The evaluating catalyst condition is reaction stagnation pressure 10.0MPa, volume space velocity 1.5h
-1, hydrogen-oil ratio 700 ︰ 1,380 ℃ of reaction temperatures.Raw materials used oiliness matter is seen table 3, and evaluation result is seen table 4.
Table 3 feedstock oil character
Table 4 catalyst and contrast medium evaluation result
Embodiment 2:
Use the modified aluminum hydroxide solid elastomer of siliceous 4wt%, the preparation method who repeats embodiment 1 prepares catalyst carrier S-2, and the character of carrier S-2 is as shown in table 5.
The physico-chemical property of table 5 carrier S-2
To contain the maceration extract incipient impregnation catalyst carrier S-2 of an amount of molybdenum trioxide, basic nickel carbonate and phosphoric acid, preparation catalyst C-2, preparation method repetition embodiment 1.The catalyst that makes contains the molybdenum (in oxide) of 20wt%, and the phosphorus of 3.8wt% nickel (in oxide) and 1.4wt% is (with P
2O
5Meter).
Comparative Examples 2:
With with the maceration extract impregnated catalyst carrier S-2 of embodiment 2 same metal content, prepare contrast medium RB-1, RB-2, RB-3 respectively.The preparation method repeats Comparative Examples 1.
Catalyst and contrast medium active appraisal experiment carry out on 100ml fixed bed hydrogenation experimental provision, and feedstock oil is the coking gasoline and diesel cut.Before the activity rating catalyst is carried out presulfurization.The evaluating catalyst condition is reaction stagnation pressure 6.0MPa, volume space velocity 1.8h
-1, hydrogen-oil ratio 400: 1,350 ℃ of reaction temperatures.Raw materials used oiliness matter is seen table 6, and evaluation result is seen table 7.
Table 6 feedstock oil character
Table 7 embodiment 2 catalyst and contrast medium evaluation result
Embodiment 3:
Use the modified aluminum hydroxide solid elastomer of siliceous 4wt%, titaniferous 6wt%, the preparation method who repeats embodiment 1 prepares catalyst carrier S-3, and the character of carrier S-3 is as shown in table 8.
The physico-chemical property of table 8 carrier S-3
To contain the maceration extract incipient impregnation catalyst carrier S-3 of an amount of molybdenum trioxide, basic nickel carbonate and phosphoric acid, preparation catalyst C-3, preparation method repetition embodiment 1.The catalyst that makes contains the molybdenum (in oxide) of 18wt%, and the phosphorus of 3.5wt% nickel (in oxide) and 1.4wt% is (with P
2O
5Meter).
Comparative Examples 3:
With with the maceration extract impregnated catalyst carrier S-2 of embodiment 3 same metal content, prepare contrast medium RC-1, RC-2, RC-3 respectively, preparation method repeats Comparative Examples 1.
Catalyst and contrast medium active appraisal experiment carry out on 100ml fixed bed hydrogenation experimental provision, and feedstock oil is straight-run naphtha.Before the activity rating catalyst is carried out presulfurization.The evaluating catalyst condition is reaction stagnation pressure 2.6MPa, volume space velocity 8.0h
-1, hydrogen-oil ratio 200: 1,300 ℃ of reaction temperatures.Raw materials used oiliness matter is seen table 9, and evaluation result is seen table 10.
Table 9 feedstock oil character
Table 10 embodiment 3 catalyst and contrast medium evaluation result
Method for preparing catalyst provided by the present invention is earlier aluminum hydroxide solid elastomer or modified aluminum hydroxide solid elastomer to be prepared into carrier; VI B family's metal molybdenum and/or tungsten and VIII family metallic nickel and/or cobalt are mixed with solution; Adopt the infusion process impregnated carrier, be prepared into catalyst through dry, roasting.Since adopt low-temperature bake degrading activity component predecessor controlled reactive metal the dispersive property of carrier surface and with carrier interactions intensity, improved activity of such catalysts and stability, reduced the Preparation of catalysts cost.
Claims (9)
1. the Hydrobon catalyst of a low-temperature bake; It is characterized in that this catalyst is a carrier with aluminium oxide or modified aluminas; With VI B family's metal and VIII family metal is active component; Wherein aluminium oxide or modified aluminium oxide supports content 60-90wt%, VI B family metal oxide content 5-35wt%, VIII family metal oxide content 1-10wt%.
2. one kind according to the said Preparation of catalysts method of claim 1, it is characterized in that may further comprise the steps:
The first step: preparation catalyst carrier: in aluminum hydroxide solid elastomer or modified aluminum hydroxide solid elastomer, add binding agent with extrusion aid after mix pinch, extruded moulding, 80 ℃-150 ℃ descended dry 1-20 hour, made at 400 ℃ of-700 ℃ of following roasting 2-12 hours again;
Second step: preparation maceration extract: with nickeliferous and/or cobalt compound, contain molybdenum and/or tungsten compound and auxiliary agent and be mixedly configured into the aqueous solution;
The 3rd step: preparation catalyst: adopt equi-volume impregnating; The aqueous solution of second step preparation is sprayed on the catalyst carrier of first step gained; Dipping after 80 ℃-150 ℃ dry 1-10 hour down, 150 ℃ made catalyst of the present invention in-500 ℃ of following roasting 2-10 hours;
Modified aluminum hydroxide solid elastomer described in the first step is the aluminum hydroxide solid elastomer of one or more modifications in silicon, boron, titanium, zirconium and the fluorine, and wherein silicon, boron, titanium, zirconium or fluorine are the 2%-50% of aluminum hydroxide solid elastomer quality in the mass content of oxide; Said binding agent is one or more in nitric acid, citric acid, acetic acid and the oxalic acid, and adding weight is the 1-10% of aluminum hydroxide solid elastomer gross weight; Described extrusion aid is one or more in sesbania powder, active carbon and the polyvinyl alcohol, and adding weight is the 2-10% of aluminum hydroxide solid elastomer gross weight;
Nickeliferous and/or cobalt compound described in second step is one or more in basic nickel carbonate and/or basic cobaltous carbonate, nickel nitrate and/or cobalt nitrate, nickel oxalate and/or cobalt oxalate and nickel acetate and/or the cobalt acetate; Said molybdate compound is ammonium molybdate and/or molybdenum oxide; Said Tungstenic compound is ammonium tungstate and/or ammonium metatungstate; Said auxiliary agent is one or more in phosphoric acid, citric acid, ammoniacal liquor or the ethylenediamine.
3. according to the described method for preparing catalyst of claim 2, it is characterized in that silicon, boron, titanium, zirconium or fluorine are preferably the 5%-20% of aluminum hydroxide solid elastomer quality in the first step in the mass content of oxide.
4. according to the described method for preparing catalyst of claim 2, it is characterized in that the baking temperature described in the first step is the best with 100 ℃-120 ℃, be the best with 2-8 hour drying time; Described sintering temperature is the best with 500 ℃-600 ℃; Roasting time 3-6 hour is best.
5. according to the described method for preparing catalyst of claim 2, it is characterized in that it is the best with the 3-5% that accounts for the aluminum hydroxide solid elastomer gross weight that the binding agent described in the first step adds weight; It is the best with the 3-5% that accounts for the aluminum hydroxide solid elastomer gross weight that described extrusion aid adds weight.
6. according to the described method for preparing catalyst of claim 2, it is characterized in that described nickel and/or cobalt, molybdenum and/or W content are benchmark with the weight of catalyst, require wherein to comprise: molybdenum trioxide and/or tungstic acid 5-35w%; Nickel oxide and/or cobalt oxide 1-10w%.
7. according to the described method for preparing catalyst of claim 2, it is characterized in that the addition of described nickeliferous and/or cobalt, molybdenum and/or tungsten is a benchmark with the weight of catalyst, require wherein to comprise: the preferred 15-25w% of molybdenum trioxide and/or tungstic acid; The preferred 2-5w% of nickel oxide and/or cobalt oxide.
8. according to the described method for preparing catalyst of claim 2, it is characterized in that the baking temperature described in the 3rd step is the best with 100 ℃-120 ℃, be the best with 2-5 hour drying time; Described sintering temperature is the best with 180 ℃-250 ℃, and roasting time was the best with 3-5 hour.
9. according to the prepared Hydrobon catalyst of arbitrary described method for preparing catalyst among the claim 2-8, it is characterized in that this catalyst is used for the hydrotreatment of hydrodesulfurizationof of naphtha, poor ignition quality fuel hydrofinishing, FCC raw material or hydrocracking raw material.
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Application publication date: 20121121 |