CN106672997A - Modified Y type molecular sieve and preparation method thereof - Google Patents
Modified Y type molecular sieve and preparation method thereof Download PDFInfo
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- CN106672997A CN106672997A CN201510761543.XA CN201510761543A CN106672997A CN 106672997 A CN106672997 A CN 106672997A CN 201510761543 A CN201510761543 A CN 201510761543A CN 106672997 A CN106672997 A CN 106672997A
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- C01B39/00—Compounds having molecular sieve and base-exchange properties, e.g. crystalline zeolites; Their preparation; After-treatment, e.g. ion-exchange or dealumination
- C01B39/02—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof; Direct preparation thereof; Preparation thereof starting from a reaction mixture containing a crystalline zeolite of another type, or from preformed reactants; After-treatment thereof
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
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Abstract
The invention discloses a modified Y type molecular sieve and a preparation method thereof. The molecular sieve has the following properties: the total pore volume is 0.76-1.25ml/g, wherein the mesoporous volume is 0.55-1.05ml/g and the mesoporous volume is 65-90% of the total pore volume; the mole ratio of silicon oxide to aluminum oxide is 10-35; and the specific surface area is 680-1050m<2>/g. The preparation method comprises the following steps: under a stirring condition, adding the Y type molecular sieve into a pressure container filled with organic aqueous alkali; closing the system; increasing the pressure to 0.2-1.0MPa, and then increasing temperature to 50-90 DEG C and treating for 0.5-3 hours under constant temperature; and relieving pressure, performing suction filtration, drying and roasting, thereby acquiring the modified Y type molecular sieve. The molecular sieve has larger-size mesoporous distribution and can supply much more reaction space for macromolecules; the catalytic performance of the molecular sieve is promoted; and the preparation method is simple and is suitable for industrial application.
Description
Technical field
The present invention relates to a kind of Modified Zeolite Y and preparation method thereof.
Background technology
Y type molecular sieve is mutually communicated by octahedral molecular sieve cage along three crystalline axis directions by twelve-ring and is formed,
It is a kind of excellent catalyst activity component, not only cracking activity is high, and it is selective good.Therefore the discovery of Y type molecular sieve and
There is epoch-making meaning using in catalytic field.
Due to the Y type molecular sieve of low silica-alumina ratio（Silica than aluminum oxide mol ratio between 3 ~ 4.2）Without good
Hydrothermal stability, therefore, extensive research and universal attention are not obtained in actual building-up process and in application.And high silicon
Aluminum ratio Y type molecular sieve（Silica than aluminum oxide mol ratio more than 4.3）Because it has good hydrothermal stability and acid steady
It is qualitative, playing in the catalytic cracking of PETROLEUM PROCESSING and during being hydrocracked etc. as a kind of catalysis material through modified
Irreplaceable effect.
All the time, the modified work with regard to Y type molecular sieve has obtained the extensive concern of numerous scientific research personnel.Y type molecules
The study on the modification of sieve mainly is modified to carry out desiliconization dealuminzation by conventional acid, alkali and hydro-thermal process, while producing a large amount of
Secondary mesopore structure.The a large amount of secondary pores for producing are conducive to the reaction and diffusion of macromolecular.Current modified method is mainly
First pass through and carry out after the hydro-thermal process of uniform temperature acid treatment, not only dealuminzation has been carried out to molecular sieve, improve hydrothermal stability,
Simultaneously substantial amounts of secondary pore structure can be produced.But molecular sieve secondary pore prepared by the method is concentrated mainly on surface and amount
Limited, the amount for wanting to improve secondary pore is accomplished by advanced treating molecular sieve, and this can cause the excessive dealuminzation of molecular sieve, the acid of molecular sieve
Amount reduction cannot meet requirement.In recent years, huge progress is achieved by the research of aqueous slkali desiliconization, by pickling laggard
Step carries out alkali process can greatly increase the amount of secondary pore, while the acid amount of molecular sieve, just right solution can also be improved
The problem of the acid amount deficiency that originally advanced treating is brought.Although but by first hydro-thermal process, then pickling dealuminzation, further
Alkali cleaning desiliconization can bring up substantial amounts of secondary pore structure, while acid amount can also meet requirement.But the secondary pore structure for preparing
Aperture is concentrated mainly on 3 ~ 5nm, for the conversion of some two rings and its aromatic hydrocarbons macromolecular of the above or helpless, therefore makes
The molecular sieve of more macroporous structure of getting everything ready is a critically important direction of scientific rersearch.
The content of the invention
For the deficiencies in the prior art, the present invention provides a kind of Modified Zeolite Y and preparation method thereof.The molecular sieve
There is larger sized mesoporous distribution, more reaction compartments can be provided for macromolecular, improve the catalytic performance of molecular sieve, make
Preparation Method is simple, it is adaptable to commercial Application.
The Modified Zeolite Y of the present invention, with following property：Total pore volume be 0.76 ~ 1.25ml/g, preferably 0.80 ~
1.10ml/g；Its intermediary hole pore volume is 0.55 ~ 1.05ml/g, more preferably preferably 0.60 ~ 0.95ml/g, 0.68 ~ 0.90ml/g；
Mesoporous pore volume accounts for the 65% ~ 90% of total pore volume, and preferably 70% ~ 85%；Silica is 10 ~ 35 with the mol ratio of aluminum oxide, preferably
12~30；Specific surface area is 680 ~ 1050m2/ g, preferably 800 ~ 950m2/g。
The preparation method of the Modified Zeolite Y of the present invention, including following content：Under agitation, by Y type molecular sieve
It is in being added to the pressure vessel equipped with organic alkali solution and system is closed, 0.2 ~ 1.0MPa is boosted to, then heat to 50 ~
90 DEG C, constant temperature is processed 0.5 ~ 3 hour, and release, suction filtration, drying and roasting obtain Modified Zeolite Y.
In the inventive method, it is Hydrogen to be added to Y type molecular sieve in organic alkali solution, silica/alumina molar ratio
For 10 ~ 55, preferably 18 ~ 45；Specific surface area is 650 ~ 950m2/ g, preferably 750 ~ 900m2/g；The addition of Y type molecular sieve with have
Water quality ratio in machine aqueous slkali is 1:5 ~ 20, preferably 1：7.5~1：15.
In the inventive method, described organic base is tetraethyl ammonium hydroxide, TPAOH or tetrabutyl hydrogen-oxygen
Change one or more in ammonium, the concentration of organic alkali solution is 0.05 ~ 0.35mol/L, preferably 0.10 ~ 0.30mol/L.
Tetraethyl ammonium halide, tetrapropyl ammonium halide or tetrabutyl ammonium halide can also be directly added into the inventive method to pass through
It generates tetraethyl ammonium hydroxide, TPAOH or TBAH with NaOH reaction.
In the inventive method, boosting is realized using compressed air, nitrogen or inert gas etc. is passed through in pressure vessel.
In the inventive method, suction filtration to pH value is less than 9, and drying condition is to be dried 6 ~ 24 hours under the conditions of 80 ~ 120 DEG C.
In the inventive method, roasting condition is roasting 2 ~ 8 hours under the conditions of 450 ~ 650 DEG C.
The Modified Zeolite Y of the present invention can be used for the hydrocracking catalyst for preparing hydrocracking catalyst, obtaining
It is particularly well-suited to the conversion of condensed ring macromolecular in hydrocracking process.
The inventive method using high pressure alkali process have been carried out to Y type molecular sieve in organic alkali solution, both filled by organic base
The duct of molecular sieve also plays the destruction to molecular sieve structure limited extent simultaneously, and the destruction of exactly this limited extent exists
Bigger mesoporous formation is promoted under certain pressure.Destroy original 4nm or so in molecular sieve the method limited extent
Mesoporous hole wall so as to run through the mesoporous pore structure for defining 8nm or so, while organic in organic base during this
The radical protection microcellular structure of molecular sieve.Y type molecular sieve with macropore volume structure prepared by this method can directly be made
It is used to prepare catalyst for acid carrier.More traditional method of modifying is compared, Y type molecular sieve prepared by the present invention has bigger
Meso-hole structure is distributed, while reducing the silica alumina ratio of molecular sieve during alkali process, substantially increases the acid amount of molecular sieve, because
Catalysis activity and diffusion that molecular sieve prepared by this this method has had, while also there is very strong anti-carbon deposition ability,
Can be had broad application prospects with preferential conversion condensed ring macromolecular in hydrocracking process.
Description of the drawings
Fig. 1 is the graph of pore diameter distribution of Y type molecular sieve prepared by embodiment 1.
Fig. 2 is the XRD diffraction patterns of Y type molecular sieve prepared by embodiment 1.
Specific embodiment
The preparation process of the present invention is further illustrated with reference to embodiment, but following examples are not constituted to present invention side
The restriction of method.The Hydrogen Y type molecular sieve added in preparation process, with following property：The silica of Y-1 and aluminum oxide mole
Than for 18, specific surface area is 827m2/g；The silica of Y-2 is 35 with the mol ratio of aluminum oxide, and specific surface area is 871m2/g.This
Pressure vessel described in invention is autoclave, and it is 15MPa that maximum bears pressure, and maximum temperature is 300 DEG C.
Embodiment 1
Under agitation, Y-1 and TPAOH solution are mixed in autoclave, is passed through nitrogen control
System pressure then heats to 70 DEG C in 0.4MPa, continues constant temperature and stirs 2 hours, and release, cooling, suction filtration to pH value is less than 9,
It is dried 12 hours under the conditions of 120 DEG C, in 500 DEG C of roastings 3 hours, obtains Modified Zeolite Y.TPAOH solution
Concentration be the mass ratio of water in 0.12mol/L, Y-1 and solution be 1:9.Molecular sieve volume property is as shown in table 1.
Embodiment 2
Under agitation, Y-1 and TBAH solution are mixed in autoclave, is passed through air control
System pressure then heats to 80 DEG C in 0.6MPa, continues constant temperature and stirs 1 hour, and release, cooling, suction filtration to pH value is less than 9,
It is dried 18 hours under the conditions of 110 DEG C, in 550 DEG C of roastings 4 hours, obtains Modified Zeolite Y.TBAH solution
Concentration be the mass ratio of water in 0.15mol/L, Y-1 and solution be 1:11.Molecular sieve volume property is as shown in table 1.
Embodiment 3
Under agitation, Y-1 and tetraethyl ammonium hydroxide solution are mixed in autoclave, is passed through nitrogen control
System pressure then heats to 60 DEG C in 0.2MPa, continues constant temperature and stirs 3 hours, and release, cooling, suction filtration to pH value is less than 9,
It is dried 24 hours under the conditions of 100 DEG C, in 520 DEG C of roastings 6 hours, obtains Modified Zeolite Y.Tetraethyl ammonium hydroxide solution
Concentration be the mass ratio of water in 0.14mol/L, Y-1 and solution be 1:10.Molecular sieve volume property is as shown in table 1.
Embodiment 4
Under agitation, Y-2 and TBAH solution are mixed in autoclave, is passed through air control
System pressure then heats to 65 DEG C in 0.7MPa, continues constant temperature and stirs 2 hours, and release, cooling, suction filtration to pH value is less than 9,
It is dried 18 hours under the conditions of 90 DEG C, in 580 DEG C of roastings 3 hours, obtains Modified Zeolite Y.TPAOH solution
Concentration be the mass ratio of water in 0.18mol/L, Y-1 and solution be 1:15.Molecular sieve volume property is as shown in table 1.
Embodiment 5
Under agitation, Y-2 and TPAOH solution are mixed in autoclave, is passed through nitrogen control
System pressure then heats to 68 DEG C in 0.8MPa, continues constant temperature and stirs 2 hours, and release, cooling, suction filtration to pH value is less than 9,
It is dried 12 hours under the conditions of 120 DEG C, in 620 DEG C of roastings 3 hours, obtains Modified Zeolite Y.TPAOH solution
Concentration be the mass ratio of water in 0.14mol/L, Y-1 and solution be 1:15.Molecular sieve volume property is as shown in table 1.
Comparative example 1
With embodiment 1, simply course of reaction is carried out in atmospheric conditions.
Comparative example 2
With embodiment 1, TPAOH solution is simply replaced with the sodium hydroxide solution of 0.25mol/L（I.e. high pressure without
Machine alkali process）.
The application of catalyst carrier：
Ion exchange：Molecular sieve prepared by embodiment 1 and comparative example 1 is washed to neutrality, drying, then in 80 DEG C of water bath conditions
Under, ion exchange is carried out with 1mol/L ammonium nitrate, sodium oxide content is made less than 0.5%, washing, drying, in 550 DEG C of roasting 3h, is obtained
To hydrogen type molecular sieve.
Hydro-thermal process：By hydrogen type molecular sieve, respectively constant temperature processes 2h under the conditions of hydrothermal temperature is for 580 DEG C, obtains at hydro-thermal
Molecular sieve after reason.
Catalyst preparation：Alumina powder, amorphous silicon aluminium, modified molecular screen powder are well mixed, acid is subsequently adding molten
Liquid, fully rolls aftershaping, is then dried 8 hours under the conditions of 100 DEG C, and finally roasting 8 hours under the conditions of 600 DEG C, obtain
Catalyst carrier；The catalyst carrier that the metal impregnation solution impregnation of W and Ni is obtained is prepared, 6 are then dried under the conditions of 120 DEG C
Hour, finally roasting 6 hours under the conditions of 470 DEG C, obtain hydrocracking catalyst.Catalyst property such as table 2.
Evaluating catalyst condition：Evaluating apparatus are carried out using 200m1 small hydrogenation devices, and catalyst is entered before activity rating
Row presulfurization.Evaluate the raw materials used oil nature of catalyst activity and reaction process condition is shown in Table 3 and table 4, catalyst reaction performance
Comparing result is shown in Table 5.When evaluating catalyst, feedstock oil first passes through Hydrobon catalyst bed and then immediately proceeds to be hydrocracked
Beds, the organic nitrogen content controlled when Hydrobon catalyst bed in feedstock oil is less than 10ppm.
The physico-chemical property of the Modified Zeolite Y of table 1.
The composition of the catalyst of table 2.
The process conditions of table 3.
The feedstock property of table 4.
The catalyst reaction performance of table 5.
| Catalyst | Catalyst 1 | Catalyst 2 | Catalyst 3 |
| Reaction temperature, DEG C | 388 | 381 | 385 |
| Two ring above naphthene contents, wt% | 26 | 20 | 23 |
| BMCI values | 11.2 | 8.6 | 9.8 |
Hydrocracking reaction result shows that the molecular sieve of the present invention when conversion ratio is identical, reacts compared with other molecular sieves
Temperature is low 4 ~ 7 DEG C, and the BMCI values of tail oil product and two ring above naphthene contents are lower.Illustrate dividing for the inventive method preparation
The active sites accessibility of son sieve more preferably, is conducive to the hydrogenation open loop of polycyclic aromatic hydrocarbon so that the BMCI values of hydrocracked product with
Naphthene contents more than two rings is lower.
Claims (8)
1. a kind of Modified Zeolite Y, it is characterised in that with following property：Total pore volume be 0.76 ~ 1.25ml/g, its intermediary
Hole pore volume is 0.55 ~ 1.05ml/g, and mesoporous pore volume accounts for the 65% ~ 90% of total pore volume；The mol ratio of silica and aluminum oxide
For 10 ~ 35；Specific surface area is 680 ~ 1050m2/g。
2. according to the Modified Zeolite Y described in claim 1, it is characterised in that with following property：Total pore volume be 0.80 ~
1.10ml/g, its intermediary hole pore volume is 0.60 ~ 0.95ml/g, and mesoporous pore volume accounts for the 70% ~ 85% of total pore volume；Silica with
The mol ratio of aluminum oxide is 12 ~ 30；Specific surface area is 800 ~ 950m2/g。
3. the preparation method of the Modified Zeolite Y described in a kind of claim 1 or 2, it is characterised in that including following content：
Under stirring condition, Y type molecular sieve is added in the pressure vessel equipped with organic alkali solution, and system is closed, boost to 0.2
~ 1.0MPa, then heats to 50 ~ 90 DEG C, and constant temperature is processed 0.5 ~ 3 hour, release, suction filtration, drying and roasting, obtains modified Y types
Molecular sieve.
4. in accordance with the method for claim 3, it is characterised in that：The Y type molecular sieve being added in organic alkali solution is Hydrogen,
Silica/alumina molar ratio is 10 ~ 55, and specific surface area is 650 ~ 950m2/g；The addition of Y type molecular sieve and organic alkali soluble
Water quality ratio in liquid is 1:5~20.
5. according to the method described in claim 3 or 4, it is characterised in that：Described organic base be tetraethyl ammonium hydroxide, 4 third
One or more in base ammonium hydroxide or TBAH, the concentration of organic alkali solution is 0.05 ~ 0.35mol/L.
6. according to the method described in claim 3 or 4, it is characterised in that：The concentration of described organic alkali solution be 0.10 ~
0.30mol/L。
7. in accordance with the method for claim 3, it is characterised in that：Described drying condition is to be dried under the conditions of 80 ~ 120 DEG C
6 ~ 24 hours.
8. in accordance with the method for claim 3, it is characterised in that：Roasting condition is that roasting 2 ~ 8 is little under the conditions of 450 ~ 650 DEG C
When.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109574831A (en) * | 2017-09-29 | 2019-04-05 | 中国石油化工股份有限公司 | A method of preparing phenylacetate |
| CN109775718A (en) * | 2017-11-14 | 2019-05-21 | 中国石油化工股份有限公司 | A kind of modified Y-Y isomorphous molecular sieve and its preparation method and application |
| CN109775716A (en) * | 2017-11-14 | 2019-05-21 | 中国石油化工股份有限公司 | A kind of multi-stage porous Y type molecular sieve and preparation method thereof rich in L acid |
| CN112121849A (en) * | 2020-10-12 | 2020-12-25 | 天长市润源催化剂有限公司 | Preparation method of molecular sieve catalyst for power plant tail gas purification |
| CN112723370A (en) * | 2019-10-28 | 2021-04-30 | 中国石油化工股份有限公司 | High-acid-content modified Y-type molecular sieve and preparation method and application thereof |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109574831A (en) * | 2017-09-29 | 2019-04-05 | 中国石油化工股份有限公司 | A method of preparing phenylacetate |
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| CN109775718A (en) * | 2017-11-14 | 2019-05-21 | 中国石油化工股份有限公司 | A kind of modified Y-Y isomorphous molecular sieve and its preparation method and application |
| CN109775716A (en) * | 2017-11-14 | 2019-05-21 | 中国石油化工股份有限公司 | A kind of multi-stage porous Y type molecular sieve and preparation method thereof rich in L acid |
| CN109775716B (en) * | 2017-11-14 | 2020-07-03 | 中国石油化工股份有限公司 | Hierarchical pore Y-type molecular sieve rich in L acid and preparation method thereof |
| CN112723370A (en) * | 2019-10-28 | 2021-04-30 | 中国石油化工股份有限公司 | High-acid-content modified Y-type molecular sieve and preparation method and application thereof |
| CN112121849A (en) * | 2020-10-12 | 2020-12-25 | 天长市润源催化剂有限公司 | Preparation method of molecular sieve catalyst for power plant tail gas purification |
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