CN108751223A - A kind of AEL structure CeAPO-11 molecular sieves and preparation method - Google Patents
A kind of AEL structure CeAPO-11 molecular sieves and preparation method Download PDFInfo
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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
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Abstract
A kind of AEL structure CeAPO-11 molecular sieves of the present invention and preparation method, CeAPO-11 molecular sieves are synthesized by solid-phase grinding, it is to weigh metal salt, silicon source, phosphorus source, Fluorine source and organic amine template to improve according to a certain percentage to move to the mortar progress uniform mixed grindings of 10-30 min first, mixture state carries out crystallization by being fitted into reaction kettle after viscous wet desiccation powder or particle；It is rapid cooling after the completion of crystallization, solid product is washed to neutrality with deionized water, molecular screen primary powder is obtained after 80-120 DEG C of air drying；Molecular screen primary powder is roasted into 5h in 550 DEG C of air, obtains final products.The preferable CeAPO-11 molecular sieves of crystallinity can be made through the invention, which relates only to the mixing of primary raw materials, and synthesis step is simple compared with conventional method, and yield and one-pot utilization rate are all higher, greatly reduce production cost, energy-saving and emission-reduction, prospects for commercial application is wide.
Description
Technical field
The invention belongs to molecular sieve preparation fields, and in particular to a kind of AEL structure CeAPO-11 molecular sieves and preparation method.
Background technology
Aluminum phosphate equimolecular sieves poromerics due to having well-regulated pore passage structure and big specific surface area, the spirit of aluminium skeleton
Active and higher thermal stability can be applied to the fields such as catalysis, absorption, separation, host-guest chemistry.Metal heteroatom phosphoric acid
The one kind of aluminum molecular screen MeAPO as phosphate aluminium molecular sieve family has certain ion-exchange capacity, acidity and oxidation susceptibility,
In addition their various structures and peculiar property, have been widely used in the fields such as catalysis industry.MeAPO-11 molecular sieves are because of it
Suitable one-dimensional ten-ring structure and mild Acidity are widely used in fields such as hydroisomerizations, new
The exploration of synthetic route becomes the hot spot that researchers pay close attention to.
The characteristics of earliest Zeolite synthesis route synthesizes for solvent method, the route is using a large amount of water, amine or alcohol etc.
It is synthesized as solvent.Then, researcher studies its synthetic method, xerogel conversion method, F ion revulsion,
These methods such as ionothermal synthesis, eutectic mixing method, crystal seed method have pushed the development of molecular sieve.However it at present can be extensive
It is still hydro-thermal method route applied to industrial synthetic route, because other synthetic routes are directed to making for organic solvent
With making that increased production cost, and applicable synthesis range is relatively narrow.If the aqueous solvent of high consumption can be reduced to greatest extent
Amount and the step of synthesis of molecular sieve, is simplified, not only will significantly reduce the production cost of molecular sieve, but also can also save
The about energy all has positive effect for reducing waste discharge.
Rare earth element ce is widely used due to its unique performance in material preparation, the Ce- of ion exchange
SAPO-11 molecular sieves have higher catalytic activity in long chain alkane hydrocracking.And CeAPO-11 molecular sieves be it is a kind of by
The molecular sieve with AEL topological structures of cerium, phosphorus, aluminium and oxygen composition, due to its unique pore structure, suitable acid and oxygen
Change activity, so that it is had preferable catalytic activity in catalytic hydrogenation, isomerization reaction, the high cost based on existing level, high energy
Defect is consumed, explores at low cost, less energy consumption, safe synthetic method, it will make the application value of CeAPO-11 molecular sieves
More extensively.
Invention content
Goal of the invention：To solve problems of the prior art, the present invention provides a kind of AEL structure CeAPO-11 molecules
Sieve and preparation method.
To achieve the above object, the technical solution adopted by the present invention is：
A kind of AEL structure CeAPO-11 molecular sieves, by metal salt, silicon source, phosphorus source, cerium source, Fluorine source and organic amine template through mixed
It is prepared after carrying out crystallization, drying and roasting successively after synthesis dried powder or particle.
Further, the additive amount of the metal salt, silicon source, phosphorus source, cerium source, Fluorine source and organic amine template should make crystallization
The mol ratio of each ingredient when reaction is：A12O3：P205：CeO2：F-：R=0.9-1.1：1：0-0.2：1：0.6-1, wherein R
It refer to organic amine template.
A kind of preparation method of AEL structure CeAPO-11 molecular sieves, includes the following steps：
Step 1: being shifted after according to a certain percentage weighing metal salt, silicon source, phosphorus source, cerium source, Fluorine source and organic amine template
The uniform mixed grindings of 10-30 min are carried out to mortar, object state to be mixed after gluing wet desiccation powder or particle by being packed into reaction
Crystallization is carried out in kettle；
Step 2: room temperature cools down rapidly after the completion of crystallization, solid crystallized product is detached with mother liquor, with deionized water by solid knot
Brilliant product is washed to neutrality, and molecular screen primary powder is obtained after 80-120 DEG C of air drying；
Step 3: the molecular screen primary powder that step 2 obtains is roasted 5h in 550 DEG C of air, final products are obtained.
Further, in step 1, according to a certain percentage by metal salt, silicon source, phosphorus source, cerium source, Fluorine source and organic amine mould
Plate agent be transferred to after weighing mortar carry out the uniform mixed grindings of 10-30 min, mixture state by glue wet desiccation powder or
It is fitted into after particle in reaction kettle and carries out crystallization, subsequently complete step 2 and step 3, required molecular sieve is prepared.
Further, in step 1, metal salt, silicon source, phosphorus source, cerium source, Fluorine source and organic amine template additive amount answer
The mol ratio of each ingredient when crystallization is set to be：A12O3：P205：CeO2：F-：R=0.9-1.1：1：0-0.2：1：0.6-1,
Wherein, R refers to organic amine template.
Further, in step 1, the reaction temperature of crystallization is 150-200 DEG C, reaction time 8-48h.
Further, the metal salt is nitrate, chloride, acetate or sulfate, and silicon source is aluminium isopropoxide, phosphorus source
For one kind in phosphoric acid, ammonium dihydrogen phosphate, diammonium hydrogen phosphate, Fluorine source is hydrofluoric acid HF or ammonium fluoride NH3F, organic amine template
For one kind in diisopropylamine, di-n-propylamine.
Compared with prior art, beneficial effects of the present invention are：
The invention discloses a kind of AEL structure CeAPO-11 molecular sieves and preparation methods, and CeAPO-11 molecular sieves are by metal salt, aluminium
Source, phosphorus source, cerium source, Fluorine source and organic amine template carry out crystallization, drying successively after being mixed into dried powder or particle
It is prepared with after roasting, specifically, according to a certain percentage by metal salt, silicon source, phosphorus source, cerium source, Fluorine source and organic amine mould
Plate agent weigh improve moves to mortar carry out the uniform mixed grindings of 10-30 min, mixture state by glue wet desiccation powder or
It is fitted into reaction kettle after grain and carries out crystallization；It is rapid cooling after the completion of crystallization, solid crystallized product is detached with mother liquor, is spent
Ionized water washs solid crystallized product to neutrality, and molecular screen primary powder is obtained after 80-120 DEG C of air drying；By molecular sieve
Original powder roasts 5 hours in 550 DEG C of air, obtains final products.AEL structure CeAPO-11 molecular sieves provided by the invention and system
The crystallinity of Preparation Method, the CeAPO-11 flake nano grade molecular sieves synthesized by simple solid-phase grinding is preferable, pattern size
It is uniform, it is pure phase, inorganic atoms utilization rate is high, which relates only to the mixing of each non-silicon reaction raw materials, synthesis step
More simple compared with prior synthesizing method, solvent-free in synthesis and water eliminates influence of the pressure to material preparation in synthesis, no longer
Using traditional hydrothermal synthesis method, avoid because containing water in synthesis, high temperature leads to the security risk that reactor pressure height occurs, and closes
At safety, the problem of largely waste there is no water source, and the synthetic yield of product and one-pot utilization rate are high, greatly reduce production
Cost, energy-saving and emission-reduction can be applied to long chain alkane cracking, there is huge prospects for commercial application.
Description of the drawings
Fig. 1 is the XRD spectra of the present invention；
Fig. 2 is the SEM figures of the magnification at high multiple of the present invention；
Fig. 3 is the SEM figures of the low power amplification of the present invention；
Fig. 4 is the nitrogen adsorption isotherm of the embodiment of the present invention 1.
Specific implementation mode
With reference to specific embodiment, the present invention is described in detail.
Embodiment 1
As shown in Figs 1-4, a kind of AEL structure CeAPO-11 molecular sieves, by metal salt, silicon source, phosphorus source, cerium source, Fluorine source and organic
Amine template is prepared after carrying out crystallization, drying and roasting successively after being mixed into dried powder or particle.
A kind of preparation method of AEL structure CeAPO-11 molecular sieves d, includes the following steps：
First by solid reaction raw material：2.084g aluminium isopropoxides, 1.153g phosphoric acid, 0.087g cerous nitrates, 0.205g hydrofluoric acid and
0.607g diisopropylamines pour into mortar after weighing, and uniformly grind 10-30 min, and mixture state is made wet to become xeraphium by viscous
End or particle are fitted into after the completion of grinding in reaction kettle, after the completion of 150 DEG C of crystallization 8h, crystallization, room temperature cooling, by solid crystal
After product is detached with mother liquor, adopts and solid crystallized product is washed with deionized to neutrality, divided after 80 DEG C of air dryings
Son sieve powder, then roasts 5h in 550 DEG C of air by molecular screen primary powder, obtains final products.
In this method, crystallization should be made by controlling the additive amount of metal salt, silicon source, phosphorus source, cerium source, Fluorine source and organic amine template
The mol ratio of each ingredient when reaction is：A12O3：P2O5：CeO2：F-：R = 1：1：0.02：1：1, wherein R refers to organic amine
Template.
Fig. 1 is the XRD characterization result of product, it can be seen that product is typical CeAPO-11 structures, and with preferable
Crystallinity；Fig. 2 and Fig. 3 is SEM stereoscan photograph of the product under different amplification, the production that electromicroscopic photograph shows
Product are pure phase；Fig. 4 is the nitrogen adsorption isotherm of product, in relative pressure 0.4<P/P0<1, there is hysteresis loop in centre, shows product
It is a kind of multistage porous molecular sieve.
Embodiment 2
The preparation method of CeAPO-11 molecular sieves and aluminium isopropoxide, phosphoric acid, cerous nitrate, hydrofluoric acid and the diisopropylamine of embodiment 1
Charging sequence and milling time it is identical, the chemical mol ratio of the system is：A12O3：P2O5：CeO2：F-：R = 1：1：
0.04：1：1, it is fitted into reaction kettle after the completion of grinding, after the completion of 150 DEG C of crystallization 12h, crystallization, room temperature cooling, by solid crystal
After product is detached with mother liquor, adopts and solid crystallized product is washed with deionized to neutrality, obtained product is filled with deionized water
Divide washing, and dry at 80 DEG C, inorganic atoms utilization rate is 85.5%.
Remaining same embodiment 1.
Embodiment 3
The preparation method of CeAPO-11 molecular sieves and aluminium isopropoxide, phosphoric acid, cerous nitrate, hydrofluoric acid and the diisopropylamine of embodiment 1
Charging sequence and milling time it is identical, under the stoicheiometry of the system：A12O3：P2O5：CeO2：F-：R = 1：1：0：1：1, in
150 DEG C of crystallization 12h.After the completion of reaction, obtained product is fully washed with deionized water, and dry at 80 DEG C.
Remaining same embodiment 1.
Embodiment 4
Charging sequence and milling time prepared by CeAPO-11 sieve samples is the same as embodiment 1.Under the stoicheiometry of the system：
A12O3：P2O5：CeO2：F-：R = 1：1：0.02：1：1, in 150 DEG C of crystallization 2d.After the completion of reaction, by obtained product spend from
Sub- water fully washs, and dry at 80 DEG C.
Remaining same embodiment 1.
Embodiment 5
Charging sequence and milling time prepared by CeAPO-11 sieve samples is the same as embodiment 1.Under the stoicheiometry of the system：
A12O3：P2O5：CeO2：F-：R = 0.9：1：0.05：1：1, in 150 DEG C of crystallization 1d.After the completion of reaction, obtained product is spent
Ionized water fully washs, and dry at 80 DEG C.
Remaining same embodiment 1.
Embodiment 6
Charging sequence and milling time prepared by CeAPO-11 sieve samples is the same as embodiment 1.Under the stoicheiometry of the system：
A12O3：P2O5：CeO2：F-：R = 0.9：1：0.01：1：1, in 150 DEG C of crystallization 1d.After the completion of reaction, obtained product is spent
Ionized water fully washs, and dry at 80 DEG C.
Remaining same embodiment 1.
Embodiment 7
Charging sequence and milling time prepared by CeAPO-11 sieve samples is the same as embodiment 1.Under the stoicheiometry of the system：
A12O3：P2O5：CeO2：F-：R= 1：1：0.02：1：0.6, in 150 DEG C of crystallization 1d.After the completion of reaction, obtained product is spent
Ionized water fully washs, and dry at 80 DEG C.
Remaining same embodiment 1.
Embodiment 8
Charging sequence and milling time prepared by CeAPO-11 sieve samples is the same as embodiment 1.Under the stoicheiometry of the system：
A12O3：P2O5：CeO2：F-：R = 1.1：1：0.02：1：0.6, in 150 DEG C of crystallization 1d.After the completion of reaction, obtained product is used
Deionized water is fully washed, and dry at 80 DEG C.
Remaining same embodiment 1.
Embodiment 9
Charging sequence and milling time prepared by CeAPO-11 sieve samples is the same as embodiment 1.Under the stoicheiometry of the system：
A12O3：P2O5：CeO2：F-：R = 1：1：0.1：1：0.8, in 150 DEG C of crystallization 2d.After the completion of reaction, obtained product is spent
Ionized water fully washs, and dry at 80 DEG C.
Remaining same embodiment 1.
Embodiment 10
Charging sequence and milling time prepared by CeAPO-11 sieve samples is the same as embodiment 1.Under the stoicheiometry of the system：
A12O3：P2O5：CeO2：F-：R = 1：1：0. 2：1：1, in 150 DEG C of crystallization 2d.After the completion of reaction, by obtained product spend from
Sub- water fully washs, and dry at 80 DEG C.
Remaining same embodiment 1.
The above is only a preferred embodiment of the present invention, it should be pointed out that：For the ordinary skill people of the art
For member, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications are also answered
It is considered as protection scope of the present invention.
Claims (7)
1. a kind of AEL structure CeAPO-11 molecular sieves, which is characterized in that by metal salt, silicon source, phosphorus source, cerium source, Fluorine source and organic
Amine template is prepared after carrying out crystallization, drying and roasting successively after being mixed into dried powder or particle.
2. a kind of AEL structure CeAPO-11 molecular sieves according to claim 1, which is characterized in that the metal salt, aluminium
Source, phosphorus source, cerium source, Fluorine source and organic amine template additive amount the mol ratio of each ingredient when crystallization should be made to be 0.9-
1.1：1：0-0.2：1：0.6-1, wherein R refers to organic amine template.
3. a kind of preparation method of AEL structure CeAPO-11 molecular sieves, which is characterized in that include the following steps：
It is ground Step 1: being transferred to after according to a certain percentage weighing metal salt, silicon source, phosphorus source, Fluorine source and organic amine template
Alms bowl carries out the uniform mixed grindings of 10-30 min, mixture state by glue be fitted into reaction kettle after wet desiccation powder or particle into
Row crystallization；
Step 2: it is rapid cooling after the completion of crystallization, solid crystallized product is detached with mother liquor, is produced solid crystal with deionized water
Object is washed to neutrality, and molecular screen primary powder is obtained after 80-120 DEG C of air drying；
Step 3: the molecular screen primary powder that step 2 obtains is roasted a period of time in air, final products are obtained.
4. a kind of preparation method of AEL structure CeAPO-11 molecular sieves according to claim 3, which is characterized in that step
In one, mortar is transferred to after according to a certain percentage weighing metal salt, silicon source, phosphorus source, cerium source, Fluorine source and organic amine template
The uniform mixed grindings of 10-30 min are carried out, mixture state is carried out by being fitted into reaction kettle after viscous wet desiccation powder or particle
Crystallization subsequently completes step 2 and step 3, and required molecular sieve is prepared.
5. a kind of preparation method of AEL structure CeAPO-11 molecular sieves according to claim 3, which is characterized in that step
In one, metal salt, silicon source, phosphorus source, cerium source, Fluorine source and organic amine template each ingredient of additive amount when should make crystallization
Mol ratio is：A12O3：P205：CeO2：F-：R=0.9-1.1：1：0-0.2：1：0.6-1, wherein R refers to organic amine template.
6. a kind of preparation method of AEL structure CeAPO-11 molecular sieves according to claim 3, which is characterized in that step
In one, the reaction temperature of crystallization is 150-200 DEG C, reaction time 8-48h.
7. a kind of preparation method of AEL structure CeAPO-11 molecular sieves according to claim 3, which is characterized in that described
Metal salt is nitrate, chloride, acetate or sulfate, and silicon source is aluminium isopropoxide, and phosphorus source is phosphoric acid, ammonium dihydrogen phosphate, phosphorus
One kind in sour hydrogen diammonium, Fluorine source are hydrofluoric acid or ammonium fluoride, and organic amine template is one in diisopropylamine, di-n-propylamine
Kind.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112456513A (en) * | 2020-12-10 | 2021-03-09 | 聊城大学 | Open system solid phase synthesis AEL structure aluminum phosphate based molecular sieve, preparation method and application |
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