CN1128858C - Hydrocatalyst and its preparing process - Google Patents
Hydrocatalyst and its preparing process Download PDFInfo
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- CN1128858C CN1128858C CN 01127448 CN01127448A CN1128858C CN 1128858 C CN1128858 C CN 1128858C CN 01127448 CN01127448 CN 01127448 CN 01127448 A CN01127448 A CN 01127448A CN 1128858 C CN1128858 C CN 1128858C
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Abstract
The present invention provides a hydrocatalyst and a preparation method thereof. The catalyst is composed of metal active ingredients and a carrier, wherein the metal active ingredients of the catalyst are arbitrary two or three kinds of metal oxide MoO3, CoO and Nio. The metal active ingredients are 2 to 35% of the total weight of the catalyst, and according to the total weight of the carrier, the carrier is composed of 5% to 80% of titanium dioxide, 10% to 80% of modified ZSM-5 molecular sieves and 10% to 85% of adhesive. The catalyst of the present invention is capable of reducing the content of sulfur and alkene in inferior gasoline and increasing a gasoline octane value.
Description
Technical field
The present invention relates to a kind of catalyzer that is used for the hydrocarbons hydrogenation process, relate to a kind of inferior patrol catalyst for hydro-upgrading or rather, the invention still further relates to hydrogenization catalyst preparation method.
Background technology
Along with the harshness day by day of environmental regulation in the world wide, people are also more and more higher to the specification of quality of oil fuel, and it is important all the more that the production of clean fuel just seems.II level gasoline requires octane value (RON) to be not less than 91 in " world fuel charter ", and sulphur content is not higher than 200 μ g/g, and aromatic hydrocarbons is not higher than 40%, and alkene is not higher than 20%.Alkene, aromatic hydrocarbons and sulphur content in the restriction gasoline is in order to reduce the objectionable impurities in the motor vehicle exhaust, to reduce atmospheric pollution.China is because gasoline product mainly is made up of catalytically cracked gasoline, and wherein sulphur content and olefin(e) centent all are higher than this standard far away.The alkene of gasoline products and sulphur 90% are from catalytically cracked gasoline.Therefore, improve quality of gasoline, produce clean fuel, key is to improve the quality of catalytically cracked gasoline.
In the production of clean fuel, hydrogenation technique has other technology incomparable advantage.But when conventional Hydrobon catalyst is used to handle catalytic gasoline, sulphur, alkene and the aromaticity content in reducing gasoline, improve the color and stability of catalytic gasoline in, but reduced gasoline octane rating, loss of octane number can reach tens units at most.As having introduced a kind of catalytic gasoline deep desulfuration novel process in the U.S. Pat 6042719, though refining back product has reached sweetening effectiveness, octane value descends to some extent, and its motor-method octane number loss can reach 5%, and the research octane number (RON) loss can reach 10%.Introduced a kind of high SiO that contains in the U.S. Pat 5041208
2/ Al
2O
3The faujusite noble metal platinum hydrogenation catalyst of ratio, it can reduce in the catalytic gasoline sulphur content effectively and improve its octane value, its weak point is that temperature of reaction is higher, be generally 400～540 ℃, this catalyzer requires the stock oil final boiling point to be no more than 177 ℃ in addition, and technology is more loaded down with trivial details, work in-process need carry out prefractionation to stock oil, isolate lighting end less than 82 ℃, treat other fraction hydrogenating modification after, again this lighting end is blended in the gasoline behind the upgrading and obtains the finished product.
Summary of the invention
The present invention mainly provides a kind of inferior patrol hydrogenation catalyst, with the sulfur impurity in the effective elimination catalytically cracked gasoline, reduces olefin content in gasoline, improves gasoline octane rating simultaneously.The present invention also provides this Preparation of catalysts method.
Hydrogenation catalyst of the present invention is made up of metal active constituent and carrier, and the activity of such catalysts component is metal oxide MoO
3, among CoO and the NiO any two kinds or three kinds, in total catalyst weight, metal active constituent accounts for 2～35%; Carrier is made up of the ZSM-5 molecular sieve and the tackiness agent of titanium oxide, modification, and wherein titanium oxide accounts for 5%～80% of total weight of carrier, and optimum is 10%～60%; Modified zsm-5 zeolite accounts for 10%～80% of total weight of carrier, and optimum is 15～65%; 10%～85% of binder constitutes total weight of carrier in the carrier, optimum are 20%～75%, and above percentage number average is in oxide dry basis; Described modified zsm-5 zeolite adopts nitrate, acetate or the ammonium salt of zinc, zirconium, gallium, chromium, barium or phosphorus to carry out modification, and properties-correcting agent accounts for 1～10% of molecular sieve gross weight, and optimum is 3%～6%.
Among the present invention, when the activity of such catalysts component is MoO
3During with the mixture of CoO, MoO
3Account for 1～30% of total catalyst weight, preferably 5～25%, CoO accounts for 1～20% of total catalyst weight, and preferably 4～10%; When the activity of such catalysts component is MoO
3With the mixture of NiO, wherein MoO
3Account for 1～30% of total catalyst weight, preferably 5～25%, NiO accounts for 1～18% of total catalyst weight, and preferably 2～8%; When the activity of such catalysts component is the mixture of CoO and NiO, wherein CoO accounts for 1～20% of total catalyst weight, and preferably 4～10%, NiO accounts for 1～18% of total catalyst weight, and preferably 2～8%; When the activity of such catalysts component is MoO
3, CoO and NiO mixture the time, MoO wherein
3Account for 1～30% of total catalyst weight, preferably 5～25%, CoO accounts for 1～20% of total catalyst weight, and preferably 4～10%, NiO accounts for 1～18% of total catalyst weight, and preferably 2～8%.
Among the present invention, described tackiness agent is this area typical binders, as aluminium hydroxide, aluminium colloidal sol or silicon sol.
Preparation of catalysts method of the present invention is:
(1) preparing carriers
The ZSM-5 molecular sieve powder and the tackiness agent of hydrated titanium dioxide powder, modification are mixed, add sesbania powder, nitric acid, citric acid and expanding agent then as kneading and compactings such as polyoxyethylene glycol, polyacrylamide, methylcellulose gum or carbon blacks, under 50～180 ℃ of temperature, preferably carry out drying under 80～140 ℃ of temperature then.Be 1～15 hour time of drying, is preferably 4～8 hours.Afterwards, under 350～850 ℃ of temperature, preferably carry out roasting under 400～600 ℃ of temperature again.Roasting time is 1～15 hour, is preferably 4～10 hours, makes carrier.
(2) Preparation of Catalyst
Any two kinds or three kinds in amine molybdate, Xiao Suangu or the nickelous nitrate are added in the deionized water at ambient temperature, make solution, under 15～90 ℃ of temperature, preferably use this solution dipping carrier under 20～70 ℃ of temperature.Soak time is 1～15 hour, is preferably 3～10 hours.Also can with solution with spray saturation method impregnated carrier after, left standstill under the room temperature 2～25 hours, be preferably 4～15 hours, then with it under 50～180 ℃ of temperature, preferably carry out drying under 80～140 ℃ of temperature.Be 1～15 hour time of drying, is preferably 4～8 hours, and roasting is preferably carried out under 350～550 ℃ of temperature in dry good back under 300～800 ℃ of temperature.Roasting time is 1～15 hour, is preferably 4～10 hours, can make pore volume 0.30～0.45ml/g, specific surface 200～300m
2/ g, crushing strength is greater than the catalyst for hydro-upgrading of 255N/cm.Its profile is cylindrical, cloverleaf pattern or Herba Galii Bungei shape or ball-type.
Compared with prior art, hydrogenation catalyst of the present invention not only has good hydrodesulfurization activity, also have stronger isomerization activity and aromizing ability simultaneously, inferior patrol is through after the hydrogenation catalyst hydrotreatment of the present invention, product is compared sulphur content and is reduced with stock oil, desulfurization degree is 85～98%, part alkene is by saturated, olefin(e) centent can being reduced to below 15% greater than 40% from raw material, aromaticity content improves 1～15 percentage point, and the content of isoparaffin is than 10～30 percentage points of raw material innages.Because the significantly increase of isoparaffin and the increase of aromaticity content, hydro-upgrading is given birth to olefiant octane value and is compared with raw material, and olefin(e) centent has reduced nearly 30 percentage points, 1～5 unit of octane value rising.
Hydrogenation catalyst of the present invention is applicable to the inferior patrol of handling high-sulfur and high olefin content, as catalytically cracked gasoline, coker gasoline, steam cracking gasoline etc.
The present invention does not have particular requirement to the initial boiling point and the final boiling point of stock oil, go for full cut inferior patrol such as catalytically cracked gasoline, in temperature of reaction is 350～450 ℃, the hydrogen dividing potential drop is 0.5～3.0Mpa, hydrogen/oil (volume) is 50～300, the liquid volume air speed is to operate under 0.5～3.0/ hour the condition, its sulphur content has obtained significantly reducing, can reduce to below the 200 μ g/g, desulfurization degree is 85～97%, and olefin(e) centent can reduce by 30 percentage points, and aromaticity content improves 1～15 percentage point, isomerization alkanes content improves 10～30 percentage points, and gasoline octane rating improves 1～5 unit.
Embodiment
Embodiment 1
Industry hydrous titanium oxide 100g, SB aluminium hydrate powder 60g is through the ZSM-5 molecular sieve 80g of zinc nitrate modification, wherein zinc nitrate accounts for 5% of ZSM-5 molecular sieve after the modification, after mixing, adds 8g sesbania powder, the 24g polyoxyethylene glycol, the 5g citric acid, the nitric acid of 30ml65% and appropriate amount of deionized water, mixed pinching becomes the bar of Φ 1.6mm, dry 4h under 110 ℃ of temperature, in 550 ℃ of roasting temperature 4h, make carrier a again, its physico-chemical property sees Table 1.
The physico-chemical property of table 1 carrier
The numbering pore volume, ml/g specific surface, m
2/ g crushing strength, N/cm
a 0.45 280 230
b 0.39 265 250
c 0.43 275 226
d 0.40 270 221
Add amine molybdate, Xiao Suangu in deionized water, solution composition is 50g amine molybdate/100ml, 35g Xiao Suangu/100ml.100g carrier a is immersed in the above-mentioned solution of 200ml, soak 2h under 40 ℃ of temperature, filter back dry 4h under 110 ℃ of temperature, at 500 ℃ of roasting temperature 4h, make catalyst A afterwards, its physico-chemical property sees Table 2.
Embodiment 2
Industry hydrous titanium oxide 100g, SB aluminium hydrate powder 60g is through the ZSM-5 molecular sieve 50g of zinc nitrate modification, wherein zinc nitrate accounts for 5% of ZSM-5 molecular sieve after the modification, after mixing, adds 7g sesbania powder, the 21g polyoxyethylene glycol, the 4g citric acid, the nitric acid of 25ml65% and appropriate amount of deionized water, mixed pinching becomes the bar of Φ 1.6mm, dry 4h under 110 ℃ of temperature, in 550 ℃ of roasting temperature 4h, make carrier b again, its physico-chemical property sees Table 1.
Add amine molybdate, nickelous nitrate in deionized water, solution composition is 50g amine molybdate/100ml, 36.6g nickelous nitrate/100ml.100g carrier b is carried out saturated spray dipping.Leave standstill 10h under the room temperature, dry 4h under 110 ℃ of temperature at 500 ℃ of roasting temperature 4h, makes catalyst B afterwards, and its physico-chemical property sees Table 2.
Embodiment 3
Industry hydrous titanium oxide 100g, SB aluminium hydrate powder 60g, through the ZSM-5 molecular sieve 80g of primary ammonium phosphate modification, wherein primary ammonium phosphate accounts for 3.5% of ZSM-5 molecular sieve after the modification, makes carrier c by the method for embodiment 1, and carrier character sees Table 1; Make catalyzer C by the method for embodiment 1 again, its character sees Table 2.
Embodiment 4
Industry hydrous titanium oxide 100g, SB aluminium hydrate powder 60g, through the ZSM-5 molecular sieve 80g of zirconium nitrate modification, wherein zirconium nitrate accounts for ZSM-5 molecular sieve 2.0% after the modification, makes carrier d by the method for embodiment 1, and its character sees Table 1.
Add amine molybdate, Xiao Suangu, nickelous nitrate in deionized water, solution composition is 40g amine molybdate/100ml, 21g Xiao Suangu/100ml, 18g nickelous nitrate/100ml.Make catalyzer D by the method for embodiment 2, its character sees Table 2.
By the data in the table 2 as can be seen, the catalyzer by the present invention's preparation has bigger pore volume, specific surface and excellent mechanical intensity.
Embodiment 5
With the catalytically cracked gasoline is raw material, on the medium-sized fixed bed hydrogenation device of 100ml above-mentioned catalyzer has been carried out the processing condition investigation.Stock oil character sees Table 3.Catalyzer carries out prevulcanized before use, and the reactive metal on the catalyzer is converted into sulphided state by oxidation state.After a period of stabilisation, begin that it is carried out activity and investigate test.Processing condition and generation oil nature see Table 4.
The physico-chemical property of table 2 catalyzer
Pore volume specific surface crushing strength chemical constitution, the % numbering
ml/g m
2/g N/cm MoO
3 CoO NiOA 0.40 250 266 14.5 4.2 /B 0.37 234 285 12.8 / 5.0C 0.37 246 263 14.2 4.5 /D 0.35 240 258 11.6 2.5 2.5
Table 3 stock oil character
Stock oil character
Density, kg/m
3734.1
Refractive power, n
D 201.421
Boiling range, ℃
IBP/10％ 37.9/63.8
30％/50％ 81.9/103.2
70％/90％ 135.4/166.3
FBP 193.9
Sulphur/nitrogen, μ g/g 1757/90
Group composition, %
Normal paraffin 6.26
Isomerization alkanes 21.16
Alkene 41.32
Naphthenic hydrocarbon 9.86
Aromatic hydrocarbons 19.7
RON value 90.0
Table 4 processing condition and hydrogenated oil character numbering A-1 A-2 B-1 B-2 C D processing condition hydrogen dividing potential drop, MPa 1.0 1.0 1.0 1.0 1.0 1.0 temperature, ℃ 390 420 390 420 420 420 liquid hourly space velocitys, h
-11.0 1.0 1.0 1.0 2.0 2.0 hydrogen-oil ratios, v/v 100 100 100 100 100 100 generates oil nature sulphur, μ g/g 110 85 120 100 180 195 nitrogen, μ g/g 12 8 15 11 15 20 group compositions, v% normal paraffin 9.19 8.50 12.9 10.01 11.25 11.95 isomerization alkanes 42.48 34.42 40.79 38.28 37.58 42.81 alkene 13.73 11.25 12.82 11.94 12.35 13.02 naphthenic hydrocarbon 11.12 13.02 10.53 12.20 11.88 10.18 aromatic hydrocarbons 23.48 32.81 22.96 27.57 26.94 22.04RON values 91.8 93.0 91.4 92.2 92.0 91.3 liquid are received, and % 91.8 85.4 87.0 85.0 86.8 87.9
Claims (9)
1. hydrogenation catalyst, it is characterized in that: this catalyzer is made up of metal active constituent and carrier, and the metal active constituent of catalyzer is metal oxide MoO
3, among CoO and the NiO any two kinds or three kinds, in total catalyst weight, metal active constituent accounts for 2～35%; In total weight of carrier, carrier is made up of 5%～80% titanium dioxide, 10%～80% modified zsm-5 zeolite and 10%～85% tackiness agent; The properties-correcting agent that described modified zsm-5 zeolite adopts is nitrate, acetate or the ammonium salt of zinc, zirconium, gallium, chromium, barium or phosphorus, and properties-correcting agent accounts for 1～10% of molecular sieve weight.
2. according to the described hydrogenation catalyst of claim 1, it is characterized in that: in the carrier of total weight of carrier catalyzer by 10～60% titanium dioxide, 15%～65% modified zsm-5 zeolite, 20%～75% tackiness agent is formed; The used properties-correcting agent of modified zsm-5 zeolite accounts for 3%～6% of molecular sieve weight.
3. according to claim 1 or 2 described hydrogenation catalysts, it is characterized in that: the activity of such catalysts component is MoO
3With the mixture of CoO, wherein MoO
3Account for 1～30% of total catalyst weight, CoO accounts for 1～20% of total catalyst weight.
4. according to claim 1 or 2 described hydrogenation catalysts, it is characterized in that: the activity of such catalysts component is MoO
3With the mixture of NiO, wherein MoO
3Account for 1～30% of total catalyst weight, NiO accounts for 1～18% of total catalyst weight.
5. according to claim 1 or 2 described hydrogenation catalysts, it is characterized in that: the activity of such catalysts component is the mixture of CoO and NiO, and wherein CoO accounts for 1～20% of total catalyst weight, and NiO accounts for 1～18% of total catalyst weight.
6. according to claim 1 or 2 described hydrogenation catalysts, it is characterized in that: the activity of such catalysts component is MoO
3, CoO and NiO mixture, MoO wherein
3Account for 1～30% of total catalyst weight, CoO accounts for 1～20% of total catalyst weight, and NiO accounts for 1～18% of total catalyst weight.
7. according to the described hydrogenation catalyst of claim 6, it is characterized in that: MoO
3Account for 5～25% of total catalyst weight, CoO accounts for 4～10% of total catalyst weight, and NiO accounts for 2～8% of total catalyst weight.
8. a hydrogenization catalyst preparation method according to claim 1 comprises the steps:
(1) preparing carriers
The ZSM-5 molecular sieve powder and the tackiness agent of hydrated titanium dioxide powder, modification are mixed, add sesbania powder, nitric acid, citric acid and expanding agent kneading and compacting then, under 50～180 ℃ of temperature, carry out drying then, be 1～15 hour time of drying, afterwards, carry out roasting again under 350～850 ℃ of temperature, roasting time is 1～15 hour, makes carrier;
(2) Preparation of Catalyst
Add in the deionized water at ambient temperature with any two kinds or three kinds in amine molybdate, Xiao Suangu or the nickelous nitrate, make solution, under 15～90 ℃ of temperature, use this solution dipping carrier, soak time is 1～15 hour, perhaps utilize the spray saturation method with solution impregnation on carrier, left standstill under the room temperature 2～25 hours, then it is carried out drying under 50～180 ℃ of temperature, be 1～15 hour time of drying, dry good back obtains hydrogenation catalyst 300～800 ℃ of roasting temperatures 1～15 hour.
9. according to the described hydrogenization catalyst preparation method of claim 8, it is characterized in that: the described drying temperature of step (1) is 80～140 ℃, and be 4～8 hours time of drying, and maturing temperature is 400～600 ℃, and roasting time is 4～10 hours; The described soaking temperature of step (2) is 20～70 ℃, and soak time is 3～10 hours, and time of repose is 4～15 hours under the room temperature, and drying temperature is 80～140 ℃, and be 4～8 hours time of drying, and maturing temperature is 350～550 ℃, and roasting time is 4～10 hours.
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| CN 01127448 CN1128858C (en) | 2001-09-26 | 2001-09-26 | Hydrocatalyst and its preparing process |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100457869C (en) * | 2005-10-19 | 2009-02-04 | 中国石油化工股份有限公司 | Dewaxing catalyst for lubricant oil distillate and its uses |
| JP2020527103A (en) * | 2017-07-21 | 2020-09-03 | アルベマール ヨーロッパ エスアールエル | Hydrogenation catalyst containing titanium-containing carrier and sulfur-containing organic additive |
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| CN1323755C (en) * | 2004-10-18 | 2007-07-04 | 中国石油化工集团公司 | Method for preparing hydrogenation aromatization catalyst |
| CN100364668C (en) * | 2004-10-29 | 2008-01-30 | 中国石油化工股份有限公司 | Method for preparing surface modified IIB metal oxide hydrogenation catalyst |
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| CN100352896C (en) * | 2005-10-19 | 2007-12-05 | 长春惠工催化剂有限责任公司 | Diesel oil hydroforming pourpoint depressing catalyst and preparing process thereof |
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| CN101148395B (en) * | 2007-10-09 | 2010-06-02 | 浙江蓝天环保高科技股份有限公司 | Method for preparing 1,1,1,2,3,3-hexafluoropropane from 1,1,1,2,3,3-hexafluoropropylene and hydrogen gas |
| CN104174429B (en) * | 2013-05-22 | 2017-08-25 | 中国石油化工股份有限公司 | A kind of method of heavy aromatic hydrocarbon light |
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2001
- 2001-09-26 CN CN 01127448 patent/CN1128858C/en not_active Expired - Fee Related
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100457869C (en) * | 2005-10-19 | 2009-02-04 | 中国石油化工股份有限公司 | Dewaxing catalyst for lubricant oil distillate and its uses |
| JP2020527103A (en) * | 2017-07-21 | 2020-09-03 | アルベマール ヨーロッパ エスアールエル | Hydrogenation catalyst containing titanium-containing carrier and sulfur-containing organic additive |
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| CN1356378A (en) | 2002-07-03 |
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