CN103285898A - Preparation method of hydrogenization isomerization catalyst - Google Patents
Preparation method of hydrogenization isomerization catalyst Download PDFInfo
- Publication number
- CN103285898A CN103285898A CN 201310181372 CN201310181372A CN103285898A CN 103285898 A CN103285898 A CN 103285898A CN 201310181372 CN201310181372 CN 201310181372 CN 201310181372 A CN201310181372 A CN 201310181372A CN 103285898 A CN103285898 A CN 103285898A
- Authority
- CN
- China
- Prior art keywords
- precursor solution
- preparation
- catalyst
- dipping
- cerium
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Landscapes
- Low-Molecular Organic Synthesis Reactions Using Catalysts (AREA)
- Catalysts (AREA)
Abstract
The invention discloses a preparation method of a hydrogenization isomerization catalyst. The preparation method comprises the following steps of: (1) mixing silicon source and aluminum source solutions, stirring uniformly, and adjusting the pH value to be 7.5-9, transferring the mixed solution to a hydrothermal reaction kettle, heating the hydrothermal reaction kettle to 150-250 DEG C in a microwave reactor, performing microwave hydrothermal treatment for 0.5-3 hours, taking the mixture out of the microwave reactor, then cooling to the room temperature, centrifugally separating the obtained product, washing the product for three times by using deionized water, drying the product for 12 hours at 80-120 DEG C, and roasting at 500-700 DEG C to obtain silicon-aluminum oxide; (2) preparing a precursor solution of active ingredients, dipping the active ingredients to the silicon-aluminum oxide by adopting a dipping method in a dipping sequence of niobium, vanadium, sodium, phosphorus and cerium, and drying at 80-120 DEG C for 12 hours after dipping every time; and (3) roasting the catalyst obtained after dipping at 600-800 DEG C for 4-6 hours to obtain the hydrogenization isomerization catalyst. The catalyst prepared by the preparation method of the hydrogenization isomerization catalyst is high in yield of isomeric compounds when used for isomerization reaction.
Description
Technical field
The present invention relates to chemical field, be specifically related to a kind of catalyst.
Background technology
In the petroleum product, for example lubricating oil, light oil, jet fuel etc. are for paying attention to the goods of low temperature flow.Therefore comparatively ideally be with the n-alkane that causes low temperature flow to descend in the employed base oil in these goods and wax compositions such as isoparaffin with a little branch are removed fully or part is removed, perhaps to change into the composition beyond the wax composition.In addition, in recent years, utilize Fischer-Tropsch synthesis (Fischer-Tropsch Synthesis) (below, abbreviate " FT synthetic method " as) and the hydro carbons that obtains because carrying capacity of environment material such as sulfur-containing compound not, thereby the feedstock oil when making lubricating oil or fuel receives publicity, but also contains more wax composition in this hydro carbons.The wax isomerization need be used appropriate catalyst in order to obtain being characterized as the method for low " pour point " and base oil of high viscosity index lubricant.In fact, need be that carbon number be formed greater than 15 n-alkane by having with most of (by weight greater than 70-80%), so at room temperature be that the wax of solid is transformed into the branched chain isomer that corresponding fusing point is lower than linear paraffin.For example, C
16The fusing point of n-alkane is 19 ℃, and its isomers 5-methyl pentadecane is then-31 ℃ of just fusings.
Summary of the invention
For solving the deficiencies in the prior art, the object of the present invention is to provide a kind of preparation method of hydroisomerisation catalysts, the catalyst that makes, when being applied to react, the conversion ratio height.
In order to realize above-mentioned target, the present invention adopts following technical scheme:
A kind of preparation method of hydroisomerisation catalysts is characterized in that: comprise the steps:
(1) silicon source and aluminium source solution are mixed, the formation mixed solution stirs, regulate the pH value to 7.5-9, mixed solution is transferred to hydrothermal reaction kettle, and places microwave reactor to utilize heating using microwave to 150～250 ℃ microwave hydrothermal to handle 0.5～3h, naturally cool to room temperature after the taking-up, with the product centrifugation that obtains, deionized water washing 3 times in 80-120 ℃ of dry 12h, obtains sieve and silica-sesquioxide 500-700 ℃ of roasting;
(2) prepare the precursor solution of active component respectively, wherein contain weight percentage in the precursor solution of vanadium and cerium and be 1% OP-10 surfactant, adopt infusion process to flood active component at sieve and silica-sesquioxide, the sequencing of dipping is niobium, vanadium, sodium, phosphorus, cerium, and each dipping back is at 80-120 ℃ of dry 12h;
(3) catalyst after will flooding obtained catalyst at 600-800 ℃ of roasting 4-6 hour.
Aforementioned silicon source is ethyl orthosilicate or Ludox, and described aluminium source is aluminum sulfate or aluminum nitrate.
The precursor solution of vanadium is ammonium metavanadate solution, and the precursor solution of phosphorus is phosphoric acid, and the precursor solution of cerium is cerous nitrate, and the precursor solution of sodium is sodium chloride, and the precursor solution of niobium is niobium oxalate.
Aforementioned catalyst adopts sieve and silica-sesquioxide as carrier, and the mol ratio of silicon/aluminium is 2:1-1:4, and described catalyst activity component and weight percentage are: the vanadic anhydride of 3-5%, the niobium of 2-4%, the cerium of 2-4%, the sodium of 1-2% and the phosphorus of 2-5%, surplus is sieve and silica-sesquioxide.
Usefulness of the present invention is: the preparation method of a kind of hydroisomerisation catalysts provided by the invention, and the catalyst that makes, when being used for isomerization reaction, the yield height of isomeric compound.
The specific embodiment
Below in conjunction with specific embodiment the present invention is done concrete introduction.
Embodiment 1
Catalyst adopts sieve and silica-sesquioxide as carrier, the mol ratio of silicon/aluminium is 2:1, active component and weight percentage are: 3% vanadic anhydride, 2% niobium, 2% cerium, 1% sodium and 2% phosphorus, surplus is sieve and silica-sesquioxide, method for preparing catalyst comprises the steps: that (1) is with silicon source and the mixing of aluminium source solution, the formation mixed solution that stirs is regulated the pH value to 7.5-9, and mixed solution is transferred to hydrothermal reaction kettle, and place microwave reactor to utilize heating using microwave to 150～250 ℃ microwave hydrothermal to handle 0.5～3h, naturally cool to room temperature after the taking-up, with the product centrifugation that obtains, deionized water washing 3 times, in 80-120 ℃ of dry 12h, obtain sieve and silica-sesquioxide 500-700 ℃ of roasting; (2) prepare the precursor solution of active component respectively, wherein contain weight percentage in the precursor solution of vanadium and cerium and be 1% OP-10 surfactant, adopt infusion process to flood active component at sieve and silica-sesquioxide, the sequencing of dipping is niobium, vanadium, sodium, phosphorus, cerium, and each dipping back is at 80-120 ℃ of dry 12h; (3) catalyst after will flooding obtained catalyst at 600-800 ℃ of roasting 4-6 hour.Described silicon source is Ludox, and described aluminium source is aluminum sulfate.The precursor solution of vanadium is ammonium metavanadate solution, and the precursor solution of phosphorus is phosphoric acid, and the precursor solution of cerium is cerous nitrate, and the precursor solution of sodium is sodium chloride, and the precursor solution of niobium is niobium oxalate.When being used for the n-hexane isomerization reaction, reaction temperature is 250 ℃, and the conversion ratio of n-hexane reaches 90.2%, and the yield of isomeric compound can reach 82.0%.
Embodiment 2
Catalyst adopts sieve and silica-sesquioxide as carrier, the mol ratio of silicon/aluminium is 1:4, active component and weight percentage are: 4% vanadic anhydride, 3% niobium, 3% cerium, 2% sodium and 4% phosphorus, surplus is sieve and silica-sesquioxide, method for preparing catalyst comprises the steps: that (1) is with silicon source and the mixing of aluminium source solution, the formation mixed solution that stirs is regulated the pH value to 7.5-9, and mixed solution is transferred to hydrothermal reaction kettle, and place microwave reactor to utilize heating using microwave to 150～250 ℃ microwave hydrothermal to handle 0.5～3h, naturally cool to room temperature after the taking-up, with the product centrifugation that obtains, deionized water washing 3 times, in 80-120 ℃ of dry 12h, obtain sieve and silica-sesquioxide 500-700 ℃ of roasting; (2) prepare the precursor solution of active component respectively, wherein contain weight percentage in the precursor solution of vanadium and cerium and be 1% OP-10 surfactant, adopt infusion process to flood active component at sieve and silica-sesquioxide, the sequencing of dipping is niobium, vanadium, sodium, phosphorus, cerium, and each dipping back is at 80-120 ℃ of dry 12h; (3) catalyst after will flooding obtained catalyst at 600-800 ℃ of roasting 4-6 hour.Described silicon source is Ludox, and described aluminium source is aluminum sulfate.The precursor solution of vanadium is ammonium metavanadate solution, and the precursor solution of phosphorus is phosphoric acid, and the precursor solution of cerium is cerous nitrate, and the precursor solution of sodium is sodium chloride, and the precursor solution of niobium is niobium oxalate.When being used for the n-hexane isomerization reaction, reaction temperature is 250 ℃, and the conversion ratio of n-hexane reaches 90.6%, and the yield of isomeric compound can reach 82.6%.
Embodiment 3
Catalyst adopts sieve and silica-sesquioxide as carrier, the mol ratio of silicon/aluminium is 1:3, active component and weight percentage are: 3% vanadic anhydride, 3% niobium, 3% cerium, 1% sodium and 4% phosphorus, surplus is sieve and silica-sesquioxide, method for preparing catalyst comprises the steps: that (1) is with silicon source and the mixing of aluminium source solution, the formation mixed solution that stirs is regulated the pH value to 7.5-9, and mixed solution is transferred to hydrothermal reaction kettle, and place microwave reactor to utilize heating using microwave to 150～250 ℃ microwave hydrothermal to handle 0.5～3h, naturally cool to room temperature after the taking-up, with the product centrifugation that obtains, deionized water washing 3 times, in 80-120 ℃ of dry 12h, obtain sieve and silica-sesquioxide 500-700 ℃ of roasting; (2) prepare the precursor solution of active component respectively, wherein containing weight percentage in the precursor solution of vanadium and cerium is: 1% OP-10 surfactant, adopt infusion process to flood active component at sieve and silica-sesquioxide, the sequencing of dipping is niobium, vanadium, sodium, phosphorus, cerium, and each dipping back is at 80-120 ℃ of dry 12h; (3) catalyst after will flooding obtained catalyst at 600-800 ℃ of roasting 4-6 hour.Described silicon source is Ludox, and described aluminium source is aluminum sulfate.The precursor solution of vanadium is ammonium metavanadate solution, and the precursor solution of phosphorus is phosphoric acid, and the precursor solution of cerium is cerous nitrate, and the precursor solution of sodium is sodium chloride, and the precursor solution of niobium is niobium oxalate.When being used for the n-hexane isomerization reaction, reaction temperature is 250 ℃, and the conversion ratio of n-hexane reaches 89.3%, and the yield of isomeric compound can reach 81.6%.
Embodiment 4
Catalyst adopts sieve and silica-sesquioxide as carrier, the mol ratio of silicon/aluminium is 1:1, active component and weight percentage are: 5% vanadic anhydride, 4% niobium, 4% cerium, 2% sodium and 5% phosphorus, surplus is sieve and silica-sesquioxide, method for preparing catalyst comprises the steps: that (1) is with silicon source and the mixing of aluminium source solution, the formation mixed solution that stirs is regulated the pH value to 7.5-9, and mixed solution is transferred to hydrothermal reaction kettle, and place microwave reactor to utilize heating using microwave to 150～250 ℃ microwave hydrothermal to handle 0.5～3h, naturally cool to room temperature after the taking-up, with the product centrifugation that obtains, deionized water washing 3 times, in 80-120 ℃ of dry 12h, obtain sieve and silica-sesquioxide 500-700 ℃ of roasting; (2) prepare the precursor solution of active component respectively, wherein contain weight percentage in the precursor solution of vanadium and cerium and be 1% OP-10 surfactant, adopt infusion process to flood active component at sieve and silica-sesquioxide, the sequencing of dipping is niobium, vanadium, sodium, phosphorus, cerium, and each dipping back is at 80-120 ℃ of dry 12h; (3) catalyst after will flooding obtained catalyst at 600-800 ℃ of roasting 4-6 hour.Described silicon source is Ludox, and described aluminium source is aluminum sulfate.The precursor solution of vanadium is ammonium metavanadate solution, and the precursor solution of phosphorus is phosphoric acid, and the precursor solution of cerium is cerous nitrate, and the precursor solution of sodium is sodium chloride, and the precursor solution of niobium is niobium oxalate.When being used for the n-hexane isomerization reaction, reaction temperature is 250 ℃, and the conversion ratio of n-hexane reaches 90.4%, and the yield of isomeric compound can reach 82.5%.
More than show and described basic principle of the present invention, principal character and advantage.The technical staff of the industry should understand, and above-described embodiment does not limit the present invention in any form, and all employings are equal to replaces or technical scheme that the mode of equivalent transformation obtains, all drops in protection scope of the present invention.
Claims (4)
1. the preparation method of a hydroisomerisation catalysts is characterized in that: comprise the steps:
(1) silicon source and aluminium source solution are mixed, the formation mixed solution stirs, regulate the pH value to 7.5-9, mixed solution is transferred to hydrothermal reaction kettle, and places microwave reactor to utilize heating using microwave to 150～250 ℃ microwave hydrothermal to handle 0.5～3h, naturally cool to room temperature after the taking-up, with the product centrifugation that obtains, deionized water washing 3 times in 80-120 ℃ of dry 12h, obtains sieve and silica-sesquioxide 500-700 ℃ of roasting;
(2) prepare the precursor solution of active component respectively, wherein contain weight percentage in the precursor solution of vanadium and cerium and be 1% OP-10 surfactant, adopt infusion process to flood active component at sieve and silica-sesquioxide, the sequencing of dipping is niobium, vanadium, sodium, phosphorus, cerium, and each dipping back is at 80-120 ℃ of dry 12h;
(3) catalyst after will flooding obtained catalyst at 600-800 ℃ of roasting 4-6 hour.
2. the preparation method of a kind of hydroisomerisation catalysts according to claim 1, it is characterized in that: described silicon source is ethyl orthosilicate or Ludox, described aluminium source is aluminum sulfate or aluminum nitrate.
3. the preparation method of a kind of hydroisomerisation catalysts according to claim 1, it is characterized in that: the precursor solution of vanadium is ammonium metavanadate solution, the precursor solution of phosphorus is phosphoric acid, the precursor solution of cerium is cerous nitrate, the precursor solution of sodium is sodium chloride, and the precursor solution of niobium is niobium oxalate.
4. the preparation method of a kind of hydroisomerisation catalysts according to claim 1, be characterised in that: described catalyst adopts sieve and silica-sesquioxide as carrier, the mol ratio of silicon/aluminium is 2:1-1:4, described catalyst activity component and weight percentage are: the vanadic anhydride of 3-5%, the niobium of 2-4%, the cerium of 2-4%, the sodium of 1-2% and the phosphorus of 2-5%, surplus is sieve and silica-sesquioxide.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201310181372 CN103285898A (en) | 2013-05-16 | 2013-05-16 | Preparation method of hydrogenization isomerization catalyst |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201310181372 CN103285898A (en) | 2013-05-16 | 2013-05-16 | Preparation method of hydrogenization isomerization catalyst |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN103285898A true CN103285898A (en) | 2013-09-11 |
Family
ID=49087738
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 201310181372 Pending CN103285898A (en) | 2013-05-16 | 2013-05-16 | Preparation method of hydrogenization isomerization catalyst |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103285898A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105582972A (en) * | 2014-10-24 | 2016-05-18 | 中国石油化工股份有限公司 | Isomerization pour point depression catalyst, preparation method and application thereof, and a Fischer-Tropsch synthetic wax isomerization pour point depression method |
| US20230038263A1 (en) * | 2017-11-14 | 2023-02-09 | Umicore Ag & Co. Kg | SCR Catalyst |
-
2013
- 2013-05-16 CN CN 201310181372 patent/CN103285898A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105582972A (en) * | 2014-10-24 | 2016-05-18 | 中国石油化工股份有限公司 | Isomerization pour point depression catalyst, preparation method and application thereof, and a Fischer-Tropsch synthetic wax isomerization pour point depression method |
| CN105582972B (en) * | 2014-10-24 | 2017-11-28 | 中国石油化工股份有限公司 | A kind of isomerization-visbreaking catalyst and its preparation method and application and a kind of Fischer Tropsch waxes isomerization-visbreaking method |
| US20230038263A1 (en) * | 2017-11-14 | 2023-02-09 | Umicore Ag & Co. Kg | SCR Catalyst |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102112228B (en) | Catalyst comprising at least one IZM-2 zeolite and use thereof for the conversion of hydrocarbon-based feedstocks | |
| CN104028307B (en) | A kind of magnetic solid super acidic catalyst and preparation method | |
| CN102458657B (en) | Catalyst for producing monocyclic aromatic hydrocarbons, and method for producing monocyclic aromatic hydrocarbons | |
| US8101809B2 (en) | Base oil composition comprising oligomerized olefins | |
| TWI639692B (en) | Catalyst for hydrogenation decomposition treatment and method for seeking hydrocarbon | |
| CN101823728B (en) | Method for preparing small-crystal-size SAPO-34 zeolite | |
| CN106082257A (en) | A kind of hollow molecular sieve, preparation method and applications | |
| CN103285898A (en) | Preparation method of hydrogenization isomerization catalyst | |
| CN105289712B (en) | The catalyst preparing propylene transformed for coupling between methanol C_4 hydrocarbon and its application | |
| CN105983439A (en) | Preparation method of molecular sieve catalyst for benzene alkylation, catalyst and application | |
| CN110354874A (en) | The preparation method of the sial phosphorus carrier hydrogenation catalyst of porous structure and preparing the application in bio-fuel | |
| CN108129252B (en) | Cycloalkylnaphthalene, process for producing the same and use thereof | |
| CN103897753B (en) | A kind of method of the biological Aviation Fuel of mesopore molecular sieve preparation | |
| CN103937276B (en) | Low temperature sensitization special type Wax special and preparation method thereof | |
| CN101955849B (en) | Biological lubricant prepared with ionic liquid as catalyst and preparation method | |
| CN107398290A (en) | catalyst for synthesizing thymol | |
| CN102631940B (en) | Composite catalyst and application thereof in preparing pale rosin glyceride | |
| CN105541612A (en) | Method for catalyzed synthesis of lubricating base oil from supported ionic liquid | |
| CN105195186A (en) | Preparation method of wear-resistant microsphere catalyst for acrylic acid (ester) fluidized bed | |
| CN103613761A (en) | Method for preparing polyhydrazide with effects on lowering viscosity, lowering coagulability and inhibiting corrosion and application thereof | |
| CN104447173B (en) | The method for producing sec-butylbenzene | |
| CN101550357A (en) | Method for phase-change wax decoloring | |
| Nuithitikul et al. | Catalytic activity of sulfated iron-tin mixed oxide for esterification of free fatty acids in crude palm oil: effects of iron precursor, calcination temperature and sulfate concentration | |
| CN101805013A (en) | Synthesis method for grenade-shaped nanometer zinc oxide with low-temperature control | |
| CN104107711A (en) | Fluidized bed catalyst for preparing propylene from methanol and preparation method of fluidized bed catalyst |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20130911 |