CN105582981B - A kind of naphtha isomerization catalyst and preparation method - Google Patents
A kind of naphtha isomerization catalyst and preparation method Download PDFInfo
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Abstract
The invention discloses a kind of naphtha isomerization catalyst and preparation method thereof, on the basis of catalyst weight, the content of the molecular sieves of MCM 36 is 20% ~ 80%, the content of zirconium oxide is 1% ~ 20%, the content of sulfate radical is 1% ~ 10%, and the content of Group IIA metal oxide is 0.2% ~ 3%, and the content of ferrous oxide is 0.1% ~ 5%, hydrogenation active metal component counts content as 0.05% ~ 2% using element, and surplus is aluminum oxide.Preparation method is as follows：The molecular sieves of MCM 36 through Group IIA metal and modified zirconia, are mixed with aluminium hydroxide, add sulfuric acid and/or ammonium sulfate solution, kneading extruded moulding, catalyst carrier is obtained by dry and roasting, then load active component, dried, roasting obtains naphtha isomerization catalyst.The catalyst has higher activity, under the process conditions for comparing mitigation, can increase substantially the octane number of naphtha.
Description
Technical field
It is specifically a kind of containing super acids the present invention relates to a kind of naphtha isomerization catalyst and preparation method
Naphtha conversion carries high-octane catalyst and preparation method thereof.
Background technology
Oil is the blood of modern industry, and petrochemical industry is very important basic chemical industry, the Atmospheric vacuum technique life of refinery
The gasoline fraction of production（That is naphtha）Octane number（RON）Typically between 45 ~ 60, it is necessary to by catalytic reforming, alkylation or
The reaction such as isomerization changes molecular structure, increase isoparaffin and arene content, while straight chain hydrocarbon content is reduced, to reach raising
The purpose of octane number.But clean gasoline proposes strict limitation to arene content therein now, and alkylation process meeting
Serious environmental pollution is produced, its large-scale production is extremely limited, isomerization process is to solve to be produced by naphtha
The economic and efficient technology path of high-knock rating gasoline blend component.
Acid catalyst plays an important role in petrochemical industry, and conventional acid catalyst has liquid acid catalyst, such as sulphur
Acid, hydrofluoric acid and halogen-containing solid acid catalyst.The problems such as this two classes catalyst all has pollution environment, etching apparatus,
Halogen-containing solid acid catalyst, because halogen is easily lost in, therefore has harsh control, in addition it is also necessary to often mend halogen to raw material reclaimed water.
SO4 2-/ZrO2Solid super acid catalyst it is active it is high, selectivity it is good, easily with reactant be separated, it is environmentally friendly,
Not etching apparatus, the advantages of can regenerate, such catalyst can be such that isomerization reaction carries out at a lower temperature, and with higher
Activity, it is considered to be have very much the isomerization catalyst using future, but there is the catalyst easily deficiency such as inactivation.
CN1229368A discloses a kind of solid acid catalyst and preparation method thereof, by mediating aluminium hydroxide and hydroxide
Zirconium and sulfur-containing compound, are allowed to be molded and are calcined the zirconium oxide of generation tetragonal phase, are loading a kind of the 8th, 9 or 10 race of being selected from
Metal, preferably platinum, though the catalyst introduces aluminum oxide by kneading method, stabilize tetragonal-phase zirconia, it is used for alkane
During isomerization, C1 ~ C4 of generation low-carbon alkanes are more, and isomerisation selectivity is still not ideal enough.
US5095169 and US5107054 disclose the straight chain for using beta zeolites and MCM-22 molecular sieves as catalyst
The hygrogenating isomerization reaction process of alkane.US6080904 discloses a kind of hygrogenating isomerization reaction process of linear paraffin, wherein
Used catalyst is Pt-W/ZrO2.Above-mentioned catalyst still suffers from reaction temperature height, the problems such as octane number has much room for improvement.
The content of the invention
In view of the shortcomings of the prior art, the present invention provides a kind of naphtha isomerization catalyst and preparation method thereof, and this is urged
Agent has higher activity, under the process conditions for comparing mitigation, can increase substantially the octane number of naphtha.
The composition of naphtha isomerization catalyst of the present invention is：MCM-36 molecular sieves, Group IIA metal oxide, zirconium oxide,
Sulfate radical, aluminum oxide, iron oxide and hydrogenation active metal component, on the basis of catalyst weight, the content of MCM-36 molecular sieves
For 20% ~ 80%, the content of zirconium oxide is 1% ~ 20%, and the content of sulfate radical is 1% ~ 10%, and the content of Group IIA metal oxide is
0.2% ~ 3%, the content of ferrous oxide is 0.1% ~ 5%, and hydrogenation active metal component counts content as 0.05% ~ 2% using element, and surplus is
Aluminum oxide.
Naphtha isomerization catalyst of the present invention preferably constitute for：On the basis of catalyst weight, MCM-36 molecular sieves
Content be 30% ~ 70%, the content of zirconium oxide is 2% ~ 15%, the content of sulfate radical is 2% ~ 8%, and Group IIA metal oxide contains
Measure as 0.5% ~ 2%, the content of ferrous oxide is 0.2% ~ 3%, and hydrogenation active metal component counts content as 0.1% ~ 1.5% using element,
Surplus is aluminum oxide.
The silica of described MCM-36 molecular sieves and the mol ratio of aluminum oxide arrive total silicon for 50.
Described Group IIA metal is the one or more in beryllium, magnesium, calcium, strontium or barium, preferably magnesium.
Described hydrogenation active metal component is one or more in ruthenium, palladium, platinum, rhodium, preferably palladium and/or
Platinum.
The preparation method of naphtha isomerization catalyst of the present invention, including following content：
（1）MCM-36 molecular sieves are added to the mixed solution containing soluble Group IIA metal compound and zirconium compounds
In, the MCM-36 molecular sieves of Group IIA metal and modified zirconia are prepared using coprecipitation；
（2）By step（1）The MCM-36 molecular sieves of obtained Group IIA metal and modified zirconia are sufficiently mixed with aluminium hydroxide,
Add sulfuric acid and/or ammonium sulfate solution, kneading extruded moulding, by drying and obtaining catalyst carrier after calcination process；
（3）Compound loaded by iron content arrives step（2）Obtained carrier, by drying, calcination process, obtains iron modification
Catalyst carrier；
（4）The compound containing hydrogenation active metal component is loaded into step（3）Obtained iron modified catalyst supports, warp
Dry, calcination process is crossed, naphtha isomerization catalyst is obtained.
Step（1）Group IIA metal and the specific mistake of method of the MCM-36 molecular sieves of modified zirconia prepared by the coprecipitation
Cheng Wei：MCM-36 molecular sieves are added to containing in zirconium and Group IIA metal soluble compound solution, in the condition being stirred vigorously
The lower solution ph that dropped to ammoniacal liquor is 7.0 ~ 12, stands 0.5 ~ 4 hour, separation of solid and liquid is dried, obtains Group IIA metal and zirconium changes
The MCM-36 molecular sieves of property.
Wherein, the soluble-salt of Group IIA metal is its chloride or nitrate；Soluble compound containing zirconium is Zr
(NO3)4、ZrCl4Or ZrOCl2In one or more.
Step（2）Described sulfuric acid and/or the concentration of ammonium sulfate solution is calculated as 0.1 ~ 2.0mol/L with sulfate radical, adds
Material kneading that can be defined by amount into plasticity paste.
Step（3）Described iron containing compoundses are one or both of frerrous chloride or ferrous sulfate, iron containing compoundses
The specific concentration of solution can be according to depending on the tenor on final catalyst；Mode of loading can be spraying, coating or soak
The modes such as stain, preferably impregnate, preferred saturation dipping in impregnation method.
Step（4）Described hydrogenation active component compound is one or both of chloroplatinic acid or palladium bichloride, and hydrogenation is lived
The specific concentration of property component composition solution can be according to depending on the active metallic content on final catalyst；Mode of loading can be with
For mode of loading commonly used in the prior art, such as saturation dipping, ion exchange.
Drying and roasting condition described in above step can be the same or different, described drying temperature for 25 ~
300 DEG C, drying time is 0.5 ~ 24 hour；Described sintering temperature is 300 ~ 700 DEG C, and roasting time is 0.5 ~ 8 hour.
Catalyst of the present invention is used for the conversion process of naphtha, the process conditions of reaction：Fixed bed reactors, temperature 150 ~
300 DEG C, 0.1 ~ 10MPa of pressure, 0.5 ~ 10h of volume space velocity-1, hydrogen to oil volume ratio 100 ~ 2000.
The present invention has the following advantages that compared with prior art：
The carrier of catalyst of the present invention is MCM-36 molecular sieves, is a kind of molecular sieve of layer pole structure, with micropore and Jie
The dual pore structure in hole, its intermediary hole is located at interlayer, is by the polymeric postization formation of interlevel inorganic oxide.Existing micropore
The acidity and stability of molecular sieve, while it is preferable its active sites is had for reactant molecule due to the mesoporous of interlayer again
Accessibility.In addition, MCM-36 specific surface area is very big, and its surface is made up of 12 yuan of rings holes being relatively large in diameter,
Therefore, it is possible to provide substantial amounts of active sites for reaction, it is ensured that the high activity of catalyst.
Zirconium oxide is tetragonal phase in catalyst of the present invention.Simple zirconium oxide starts monocline occur in 400 DEG C of roastings
Crystalline phase, specific surface area decreases 100m2/ below g.After sulfuric acid oxide impregnation zirconium, there is monoclinic crystal in 600 DEG C of roastings
Phase, specific surface area significantly declines therewith.The present invention makes it by being introduced into Group IIA metal in the periodic table of elements into zirconium oxide
With zirconium oxide formation solid solution, so as to suppress zirconium oxide from metastable state tetragonal phase to the transformation of stable monocline crystalline phase, make to urge
Agent is at high temperature（750~800℃）Remain to keep larger specific surface area, improve the heat endurance of catalyst, can prevent from urging
Influence of the high temperature accidentally occurred during agent use to catalyst performance, the addition of sulfate radical can form super with zirconium oxide
Strong acid center, improves catalyst activity.
Catalyst of the present invention is modified with iron and noble metal respectively, and super acidic catalyst is different low-carbon n-alkane
Have the advantages that catalytic activity is high and selectivity is high in terms of structureization, but easily occur carbon deposit there is also catalyst and inactivate, be hydrogenated with
Active component is due to raising hydrogenation activity from noble metal, reduces the stroke of the predecessor of carbon deposit, is modified and reduced by iron
The activity of the part in superpower acid site extremely active active sites, improves catalyst stability.
Embodiment
The present invention is described in detail below by embodiment, but the present invention is not limited thereto.
Wherein, MCM-36 molecular sieves are according to document disclosed in Wang Baoyu etc.（" MCM-36 Zeolite under Ultrasonic Treatment it is fast
Speed synthesis ", catalysis journal, volume 28, the 5th phase, page 398 ~ 400,）Method synthesis, obtain MCM-36 silica alumina ratio（nSiO2/
nAl2O3）125, specific surface area 820m2, average pore size 4.8nm.
The performance evaluation condition of catalyst is as follows：On continuously flowing fixed bed midget plant, 20 milliliters of catalyst are loaded,
With naphtha after hydrofinishing（RON=53）For raw material, 210 DEG C, 2.0MPa, volume space velocity 2.0h-1, hydrogen to oil volume ratio 500
Under the conditions of react, reaction for every eight hours for one it is constant, the research octane number (RON) of different constant samples is detected respectively（RON）.
Embodiment 1
A kind of preparation method of catalyst of the present invention
（1）Take 100 grams of powderies MCM-36 molecular sieves be added to 300 milliliters it is water-soluble containing magnesium nitrate and zirconium oxychloride
In liquid, with vigorous stirring, it is 8.5 that 25% concentrated ammonia liquor to solution ph, which is added dropwise, stands 2 and was as a child isolated afterwards by centrifugal process
Precipitation, is dried 8 hours by 120 DEG C, and the MCM-36 molecular sieves of magnesium and modified zirconia are made；
（2）By step（1）The MCM-36 molecular sieves of obtained magnesium and modified zirconia are sufficiently mixed with aluminium hydroxide, add concentration
For 1.0M sulfuric acid solution, kneading extrusion dries that to be calcined 3 within 4 hours and 350 DEG C small by 100 DEG C into the strip of 1.5 millimeters of diameter
When processing after obtain catalyst carrier；
（3）With sulfur acid ferrous iron solution impregnation steps（2）Obtained carrier, dries by 110 DEG C and roasts for 6 hours and 420 DEG C
Iron modified catalyst supports are obtained after burning processing in 2 hours.
（4）With the solution impregnation steps containing chloroplatinic acid（3）Obtained iron modified catalyst supports, dry 12 small by 80 DEG C
When and 380 DEG C roasting 4 hours processing after obtain catalyst of the present invention, its composition is shown in Table 1, and reactivity worth is shown in Table 2.
Embodiment 2 ~ 10
The method that catalyst is prepared according to embodiment 1, different part is that the composition of catalyst is different, obtains catalyst
Composition be shown in Table 1, reactivity worth is shown in Table 2.
Comparative example 1
The method that catalyst is prepared according to embodiment 1, different parts are step（1）Without molecular sieve, catalyst
Composition is different, and the composition for obtaining catalyst is shown in Table 1, and reactivity worth is shown in Table 2.
Comparative example 2
The method that catalyst is prepared according to comparative example 1, different parts are step（1）Without magnesium-containing compound, catalysis
The composition of agent is different, and the composition for obtaining catalyst is shown in Table 1, and reactivity worth is shown in Table 2.
Comparative example 3
The method that catalyst is prepared according to comparative example 2, cancellation step（3）, i.e., not iron content, the composition of catalyst in catalyst
Difference, the composition for obtaining catalyst is shown in Table 1, and reactivity worth is shown in Table 2.
Each embodiment of table 1（Comparative example）Catalyst is constituted.
Note：1 calcium oxide, 2 strontium oxide strontias, 3 barium barium monoxide, 4 beryllium oxide：Magnesia=1:1（Mass ratio）, 5 palladiums, 6 rhodiums, 7 palladiums：
Platinum=1:1（Mass ratio）, 8 rutheniums.
Each embodiment of table 2（Comparative example）The reactivity worth of catalyst.
Note：Raw material RON=53, each Time constant is 8 hours.
The result of table 2 is shown, compared with comparative example, and catalyst of the present invention is not only lived initial stage in naphtha conversion process
Property it is high, and catalyst stability more preferably, show good effect.
Claims (15)
1. a kind of naphtha isomerization catalyst, it is characterised in that：Catalyst is constituted：MCM-36 molecular sieves, Group IIA metal oxygen
Compound, zirconium oxide, sulfate radical, aluminum oxide, iron oxide and hydrogenation active metal component, on the basis of catalyst weight, MCM-36
The content of molecular sieve is 20% ~ 80%, and the content of zirconium oxide is 1% ~ 20%, and the content of sulfate radical is 1% ~ 10%, Group IIA metal oxidation
The content of thing is 0.2% ~ 3%, and the content of ferrous oxide is 0.1% ~ 5%, and hydrogenation active metal component counts content as 0.05% using element
~ 2%, surplus is aluminum oxide；The preparation method of described catalyst, including following content：（1）MCM-36 molecular sieves are added to
In mixed solution containing soluble Group IIA metal compound and zirconium compounds, Group IIA metal and zirconium are prepared using coprecipitation
Modified MCM-36 molecular sieves；（2）By step（1）The MCM-36 molecular sieves and hydroxide of obtained Group IIA metal and modified zirconia
Aluminium is sufficiently mixed, and adds sulfuric acid and/or ammonium sulfate solution, kneading extruded moulding, by drying and being urged after calcination process
Agent carrier；（3）Compound loaded with iron content arrives step（2）Obtained carrier, by drying, calcination process, obtains iron and changes
Property catalyst carrier；（4）Hydrogenation active metal component will be contained compound loaded to step（3）Obtained iron modified catalyst is carried
Body, by drying, calcination process, obtains naphtha isomerization catalyst.
2. according to the catalyst described in claim 1, it is characterised in that：On the basis of catalyst weight, MCM-36 molecular sieves
Content is 30% ~ 70%, and the content of zirconium oxide is 2% ~ 15%, and the content of sulfate radical is 2% ~ 8%, the content of Group IIA metal oxide
For 0.5% ~ 2%, the content of ferrous oxide is 0.2% ~ 3%, and hydrogenation active metal component counts content as 0.1% ~ 1.5% using element, remaining
Measure as aluminum oxide.
3. according to the catalyst described in claim 1 or 2, it is characterised in that：The silica and oxygen of described MCM-36 molecular sieves
The mol ratio for changing aluminium is 50 to 125.
4. according to the catalyst described in claim 1 or 2, it is characterised in that：Described Group IIA metal be selected from beryllium, magnesium, calcium,
One or more in strontium or barium.
5. according to the catalyst described in claim 1 or 2, it is characterised in that：Described Group IIA metal is magnesium.
6. according to the catalyst described in claim 1 or 2, it is characterised in that：Described hydrogenation active metal component be selected from ruthenium,
One or more in palladium, platinum, rhodium.
7. the preparation method of the catalyst described in a kind of claim 1 or 2, it is characterised in that including following content：（1）By MCM-
36 molecular sieves are added in the mixed solution containing soluble Group IIA metal compound and zirconium compounds, using co-precipitation legal system
The MCM-36 molecular sieves of standby Group IIA metal and modified zirconia；（2）By step（1）The MCM-36 of obtained Group IIA metal and modified zirconia
Molecular sieve is sufficiently mixed with aluminium hydroxide, adds sulfuric acid and/or ammonium sulfate solution, kneading extruded moulding, by drying and roasting
Catalyst carrier is obtained after burning processing；（3）Compound loaded with iron content arrives step（2）Obtained carrier, by drying, roasting
Processing, obtains iron modified catalyst supports；（4）Hydrogenation active metal component will be contained compound loaded to step（3）Obtained iron
Modified catalyst supports, by drying, calcination process, obtain naphtha isomerization catalyst.
8. in accordance with the method for claim 7, it is characterised in that：Step（1）Group IIA metal prepared by the coprecipitation and
The method detailed process of the MCM-36 molecular sieves of modified zirconia is：MCM-36 molecular sieves are added to can containing zirconium and Group IIA metal
In soluble compound solution, it is 7.0 ~ 12 to drop to solution ph with ammoniacal liquor under conditions of being stirred vigorously, and stands 0.5 ~ 4 hour,
Separation of solid and liquid, dries, obtains the MCM-36 molecular sieves of Group IIA metal and modified zirconia.
9. in accordance with the method for claim 7, it is characterised in that：Step（1）The soluble-salt of the Group IIA metal is IIA
One or more in the chloride or nitrate of race's metal.
10. in accordance with the method for claim 7, it is characterised in that：Step（1）The soluble compound containing zirconium is Zr
(NO3)4、ZrCl4Or ZrOCl2In one or more.
11. in accordance with the method for claim 7, it is characterised in that：Step（2）Described sulfuric acid and/or ammonium sulfate solution
Concentration 0.1 ~ 2.0mol/L is calculated as with sulfate radical.
12. in accordance with the method for claim 7, it is characterised in that：Step（3）Described iron containing compoundses be frerrous chloride or
One or both of ferrous sulfate.
13. in accordance with the method for claim 7, it is characterised in that：Step（4）Described hydrogenation active component compound is chlorine
One or both of platinic acid or palladium bichloride.
14. in accordance with the method for claim 7, it is characterised in that：Described drying temperature is 25 ~ 300 DEG C, and drying time is
0.5 ~ 24 hour；Described sintering temperature is 300 ~ 700 DEG C, and roasting time is 0.5 ~ 8 hour.
15. application of the catalyst in naphtha conversion process described in a kind of claim 1 or 2, it is characterised in that：Reaction
Process conditions：Fixed bed reactors, 150 ~ 300 DEG C of temperature, 0.1 ~ 10MPa of pressure, 0.5 ~ 10h of volume space velocity-1, hydrogen to oil volume ratio
100~2000。
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| CN111804330B (en) * | 2020-07-09 | 2023-04-25 | 中国石油大学(北京) | Sulfate radical/zirconia@SAPO-11 composite material, hydrocarbon isomerization catalyst and application |
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| CN101035618A (en) * | 2004-09-07 | 2007-09-12 | Abb路慕斯全球股份有限公司 | Hydroprocessing catalyst with zeolite and high mesoporosity |
| CN101116827A (en) * | 2006-07-31 | 2008-02-06 | 中国石油化工股份有限公司 | Catalyzer for preparing low carbon olefinic hydrocarbon through hydrocarbons catalytic oxidation cracking |
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| US6797849B2 (en) * | 2002-11-01 | 2004-09-28 | Exxonmobil Chemical Patents Inc. | Xylene isomerization |
| US7456329B2 (en) * | 2005-11-30 | 2008-11-25 | Exxonmobil Chemical Patents Inc. | Polyolefins from non-conventional feeds |
| US8227654B2 (en) * | 2009-09-08 | 2012-07-24 | Exxonmobil Chemical Patents Inc. | Aromatic hydrocarbon purification method |
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| CN101035618A (en) * | 2004-09-07 | 2007-09-12 | Abb路慕斯全球股份有限公司 | Hydroprocessing catalyst with zeolite and high mesoporosity |
| CN101116827A (en) * | 2006-07-31 | 2008-02-06 | 中国石油化工股份有限公司 | Catalyzer for preparing low carbon olefinic hydrocarbon through hydrocarbons catalytic oxidation cracking |
| CN102066292A (en) * | 2008-05-07 | 2011-05-18 | 出光兴产株式会社 | Method for producing compound having adamantane structure |
| CN102794181A (en) * | 2011-05-27 | 2012-11-28 | 中科合成油技术有限公司 | Hydrodeoxygenation catalyst for Fischer Tropsch synthesis oil and preparation method and application of hydrodeoxygenation catalyst |
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