CN108128786B - A kind of method that ultrasonic wave added prepares multi-stage porous SAPO-11 molecular sieve - Google Patents
A kind of method that ultrasonic wave added prepares multi-stage porous SAPO-11 molecular sieve Download PDFInfo
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Abstract
The invention discloses a kind of methods that ultrasonic wave added prepares multi-stage porous SAPO-11 molecular sieve.This method are as follows: after mixing silicon source, phosphorus source, silicon source, deionized water, micropore template agent and mesoporous template in proportion, it is ultrasonically treated, then it is stirred at room temperature to mixture and becomes colloidal sol, it is dry, grinding, hydrothermal crystallizing, roasting removal micropore template agent, obtains multi-stage porous SAPO-11 molecular sieve after product separation drying.The condition of the ultrasonic treatment are as follows: ultrasonic power 200-400w, supersonic frequency 20-60kHz, ultrasonic time 0.5-4h.The multi-stage porous SAPO-11 zeolite product that the present invention prepares not only has the AEL structure and higher crystallinity of complete SAPO-11 molecular sieve, and there are more meso-hole structures, in addition only with minimal amount of water in sieve synthesis procedure, reduce the generation of waste water in production process, yield and one-pot yield are all enhanced.
Description
Technical field
The invention belongs to molecule sieve porous material technical fields, and in particular to a kind of ultrasonic wave added prepares multi-stage porous SAPO-
The method of 11 molecular sieves.
Background technique
Silicon phosphate aluminium base SAPO-11 molecular sieve has been constantly subjected to study and pay close attention to extensively, be known as since the eighties researches and develops
" third generation novel molecular sieve ".The skeleton structure of SAPO-11 molecular sieve is different from traditional Si-Al zeolite ZSM-5, by aluminium and phosphorus
It is alternately arranged as main element, the silicon atom of introducing has broken the electroneutral balance of phosphorus aluminium skeleton, makes it have commutative
Charge, form the acidity and catalytic applications of unique molecular sieve.SAPO-11 molecular sieve is in the means of nonzeolitic of AEL structure
Porous molecular sieve belongs to orthorhombic system, has one-dimensional ten-ring cellular structure, oval duct (0.64 × 0.39nm).Cause
Make SAPO-11 molecular sieve extensive in the isomerization of normal hydrocarbon class, alkylation, gasoline isomery with suitable acid site and cellular structure
The multiple petrochemical industries such as octane number and lubricating oil isomerization dewaxing are widely applied.
Multistage porous molecular sieve can reduce micropore diffusional resistance to mass transfer since it has micropore and mesoporous feature simultaneously
Bring adverse effect, to improve the mass transfer rate of catalyst.Generally it is by the definition that aperture is less than 2nm in multistage porous molecular sieve
Micropore, aperture are mesoporous in 2-50nm.For multistage porous molecular sieve, pore structure is more flourishing, and pore morphology is more complicated, especially micro-
When hole and bigger mesoporous ratio, the specific surface area of material is bigger, therefore the amount of the gas of the material absorption of unit mass will be got over
Greatly, the adsorption function of material for gaseous is stronger.The primary synthetic methods for the multi-stage porous SAPO-11 molecular sieve reported at present have water
Thermal method, dry gum method and solvent-thermal method etc., but these methods are limited for mesoporous increase degree.
Ultrasonic technology can generate a series of close to pole as a kind of physical means and tool in chemical reaction medium
The condition at end, such as electric discharge sharply, the high temperature of moment for generating part, high pressure, this energy can not only excite or promote
Many chemical reactions accelerate reaction speed, or even can also change the direction of certain chemical reactions.Sonochemistry is in catalyst
Preparation and field of catalytic reactions using increasing.But there is presently no apply sonochemistry in SAPO-11 molecular sieve
Prepare the relevant report of aspect.
Summary of the invention
It is an object of the present invention to provide a kind of methods that ultrasonic wave added prepares multi-stage porous SAPO-11 molecular sieve, solve existing
The not high technical problem of the mesoporous increase degree of SAPO-11 molecular sieve preparation method in technology.
Used technical solution is as follows to solve above-mentioned technical problem by the present invention:
A kind of method that ultrasonic wave added prepares multi-stage porous SAPO-11 molecular sieve, this method are as follows: by silicon source, phosphorus source, silicon source,
It after deionized water, micropore template agent and mesoporous template mix in proportion, is ultrasonically treated, is then stirred at room temperature to mixing
Object becomes colloidal sol, dry, grinding, hydrothermal crystallizing, and roasting removal micropore template agent, obtains multi-stage porous SAPO- after product separation drying
11 molecular sieves.
Preferably, source of aluminium is boehmite or aluminium isopropoxide；The silicon source is silica gel or ethyl orthosilicate.
Preferably, the mesoporous template is surfactant cetyl trimethylammonium bromide or cetyl front three
Ammonium chloride or hard template active carbon.
Preferably, the micropore template agent is di-n-propylamine.
Preferably, the molar ratio between the silicon source, silicon source, phosphorus source, micropore template agent and mesoporous template are as follows: (0.05-
0.48): 1:(0.7-1.2): (0.8-2): (0.01-0.2).
Preferably, the condition of the ultrasonic treatment are as follows: ultrasonic power 200-400w, supersonic frequency 20-60kHz surpass
The sound time is 0.5-4h.
Preferably, the temperature of the hydrothermal crystallizing of the colloidal sol is 160-220 DEG C, and the time of hydrothermal crystallizing is 12-36h.
It is 500-600 DEG C that the maturing temperature of template agent removing is removed in roasting after the product drying.
The present invention also provides a kind of multi-stage porous SAPO-11 molecular sieve, which is prepared by the above method.
Preferably, the partial size of the multi-stage porous SAPO-11 molecular sieve is 2-10 microns, external surface area 89m2/g。
The present invention also provides application of the multi-stage porous SAPO-11 molecular sieve in the reaction of n-dodecane hydroisomerizing.
Compared with prior art, beneficial effects of the present invention are as follows:
1, compared with prior art, the multi-stage porous SAPO-11 zeolite product that the present invention prepares not only has completely
SAPO-11 molecular sieve AEL structure and higher crystallinity, and have more meso-hole structures.In addition with hydrothermal synthesis
It compares, only reduces the generation of waste water in production process, yield and list with minimal amount of water in sieve synthesis procedure
Kettle yield is all enhanced.
2, multi-stage porous SAPO-11 molecular sieve prepared by the present invention can to the hydroisomerizing maximum isomers yield of n-dodecane
With reach 81% (reaction condition: 320 DEG C, 4.5MPa, WHSV=1h-1, nH2: nC12=15).
Detailed description of the invention
Fig. 1 is the XRD spectra of product multi-stage porous SAPO-11 molecular sieve made from the embodiment of the present invention 2.
Fig. 2 is the stereoscan photograph of product multi-stage porous SAPO-11 molecular sieve made from the embodiment of the present invention 2.
Fig. 3 is the nitrogen adsorption isotherm of product multi-stage porous SAPO-11 molecular sieve made from the embodiment of the present invention 2.
Fig. 4 is the XRD spectra of product multi-stage porous SAPO-11 molecular sieve made from comparative example 1 of the present invention.
Fig. 5 is the stereoscan photograph of product multi-stage porous SAPO-11 molecular sieve made from comparative example 1 of the present invention.
Fig. 6 is the nitrogen adsorption isotherm of product multi-stage porous SAPO-11 molecular sieve made from comparative example 1 of the present invention.
Fig. 7 is the embodiment of the present invention 1, and product made from 2,3 becomes the isomers yield that n-dodecane hydroisomerizing reacts
Change curve.
Specific embodiment
Technical solution of the present invention is described in detail below with reference to embodiment.Raw materials and reagents used in the present invention
It is commercially available.
Embodiment 1
The present embodiment provides a kind of methods that ultrasonic wave added method prepares SAPO-11 multistage porous molecular sieve, specifically include: first
4.085g aluminium isopropoxide and 3.16g deionized water are mixed, are added later by 1.7mL phosphoric acid and 3.16g deionized water group
At mixed solution in；Then 0.45mL ethyl orthosilicate, 1.6mL di-n-propylamine and 0.018g cetyl front three are added successively
Base ammonium bromide, later by mixing liquid room temperature ultrasound 1h (ultrasonic power 53KHz, 350W).Continue to stir, 80 DEG C of dryings, 200
For 24 hours, template agent removing is removed in high-temperature roasting (600 DEG C) for DEG C hydrothermal crystallizing.
The specific surface area for the multi-stage porous SAPO-11 molecular sieve that the present embodiment obtains is 296.4m2/ g, external surface area are
80.6m2/ g, total pore volume 0.225cm3/ g, mesoporous Kong Rongwei 0.139cm3/g。
Embodiment 2
The present embodiment provides a kind of methods that ultrasonic wave added method prepares SAPO-11 multistage porous molecular sieve, specifically include: first
4.085g aluminium isopropoxide and 3.16g deionized water are mixed, are added later by 1.7mL phosphoric acid and 3.16g deionized water group
At mixed solution in；Then 0.45mL tetraethyl orthosilicate, 1.6mL di-n-propylamine and 0.018g cetyl three are added successively
Methyl bromide ammonium, later by mixing liquid room temperature ultrasound 2h (ultrasonic power 53KHz, 350W).Continue to stir, 80 DEG C of dryings,
For 24 hours, template agent removing is removed in high-temperature roasting (600 DEG C) to 200 DEG C of hydrothermal crystallizings.
Fig. 1 is shown as the XRD characterization result of multi-stage porous SAPO-11 molecular sieve synthesized by the present embodiment, it can be seen that produces
Product are typical AEL structure, have preferable crystallinity.Fig. 2 is shown as multi-stage porous SAPO-11 molecule synthesized by the present embodiment
The stereoscan photograph of sieve, it can be seen that the ball that product is about 2 microns of partial size, and be hollow structure.Fig. 3 is shown as this reality
Apply the nitrogen adsorption isotherm of multi-stage porous SAPO-11 molecular sieve synthesized by example.The multi-stage porous SAPO-11 that the present embodiment obtains points
The specific surface area of son sieve is 333.4m2/ g, external surface area 89.4m2/ g, total pore volume 0.237cm3/ g, mesoporous Kong Rongwei
0.139cm3/g。
The present embodiment also provides a kind of application method of multi-stage porous SAPO-11 molecular sieve, the multi-stage porous SAPO-11 molecule
The hydroisomerizing that sieve is applied to long chain alkane reacts.As an example, the long chain alkane includes n-dodecane.It is prepared in the present invention
Multi-stage porous SAPO-11 molecular sieve be 81% (reaction condition: 320 to the isomers yield of the hydroisomerizing of n-dodecane reaction
DEG C, 4.5MPa, WHSV=1h-1, nH2: nC12=15).
Embodiment 3
The present embodiment provides a kind of methods that ultrasonic wave added method prepares SAPO-11 multistage porous molecular sieve, specifically include: first
4.085g aluminium isopropoxide and 3.16g deionized water are mixed, are added later by 1.7mL phosphoric acid and 3.16g deionized water group
At mixed solution；0.45mL tetraethyl orthosilicate, 1.6mL di-n-propylamine and 0.018g cetyl trimethyl bromine are added successively
Change ammonium, later by mixing liquid room temperature ultrasound 3h (ultrasonic power 53KHz, 350W).Continue to stir, 80 DEG C of dryings, 200 DEG C of water
For 24 hours, template agent removing is removed in high-temperature roasting (600 DEG C) to thermal crystallisation.
The specific surface area for the multi-stage porous SAPO-11 molecular sieve that the present embodiment obtains is 286.4m2/ g, external surface area are
64.8m2/ g, total pore volume 0.231cm3/ g, mesoporous Kong Rongwei 0.143cm3/g。
Embodiment 4
The present embodiment provides a kind of methods that ultrasonic wave added method prepares SAPO-11 multistage porous molecular sieve, specifically include: first
4.085g aluminium isopropoxide and 3.16g deionized water are mixed, are added later by 1.7mL phosphoric acid and 3.16g deionized water group
At mixed solution；0.45mL tetraethyl orthosilicate, 1.6mL di-n-propylamine and 0.018g active carbon are added successively, will mix later
It closes liquid room temperature ultrasound 1h (ultrasonic power 53KHz, 350W).Continue to stir, 80 DEG C of dryings, 200 DEG C of hydrothermal crystallizings are for 24 hours, high
Template agent removing is removed in temperature roasting (500 DEG C).
The specific surface area for the multi-stage porous SAPO-11 molecular sieve that the present embodiment obtains is 280.5m2/ g, external surface area are
62.3m2/ g, total pore volume 0.22cm3/ g, mesoporous Kong Rongwei 0.14cm3/g。
Embodiment 5
The present embodiment provides a kind of methods that ultrasonic wave added method prepares SAPO-11 multistage porous molecular sieve, specifically include: first
4.085g aluminium isopropoxide and 3.16g deionized water are mixed, are added later by 1.7mL phosphoric acid and 3.16g deionized water group
At mixed solution；0.45mL tetraethyl orthosilicate, 1.6mL di-n-propylamine and 0.018g cetyl trimethyl bromine are added successively
Change ammonium, later by mixing liquid room temperature ultrasound 4h (ultrasonic power 20KHz, 200W).Continue to stir, 80 DEG C of dryings, 200 DEG C of water
For 24 hours, template agent removing is removed in high-temperature roasting (500 DEG C) to thermal crystallisation.
The specific surface area for the multi-stage porous SAPO-11 molecular sieve that the present embodiment obtains is 278.2m2/ g, external surface area are
60.5m2/ g, total pore volume 0.20cm3/ g, mesoporous Kong Rongwei 0.135cm3/g。
Embodiment 6
The present embodiment provides a kind of methods that ultrasonic wave added method prepares SAPO-11 multistage porous molecular sieve, specifically include: first
4.085g aluminium isopropoxide and 3.16g deionized water are mixed, are added later by 1.7mL phosphoric acid and 3.16g deionized water group
At mixed solution；0.45mL tetraethyl orthosilicate, 1.6mL di-n-propylamine and 0.018g cetyl trimethyl bromine are added successively
Change ammonium, later by mixing liquid room temperature ultrasound 0.5h (ultrasonic power 60KHz, 400W).Continue to stir, 80 DEG C of dryings, 200 DEG C
For 24 hours, template agent removing is removed in high-temperature roasting (500 DEG C) to hydrothermal crystallizing.
The specific surface area for the multi-stage porous SAPO-11 molecular sieve that the present embodiment obtains is 282.5m2/ g, external surface area are
63.2m2/ g, total pore volume 0.225cm3/ g, mesoporous Kong Rongwei 0.140cm3/g。
Comparative example 1
As a comparison, the SAPO-11 multi-stage porous molecular sieve methods prepared without the method for ultrasonic treatment are as follows: first will
4.085g aluminium isopropoxide and 3.16g deionized water are mixed, and are added are made of 1.7mL phosphoric acid and 3.16g deionized water later
Mixed solution；0.45mL tetraethyl orthosilicate, 1.6mL di-n-propylamine and 0.018g cetyl trimethyl bromination are added successively
Ammonium.Continue to stir, 80 DEG C of dryings, for 24 hours, template agent removing is removed in high-temperature roasting to 200 DEG C of hydrothermal crystallizings.
The specific surface area for the multi-stage porous SAPO-11 molecular sieve that the present embodiment obtains is 266.6m2/ g, external surface area are
55.9m2/ g, total pore volume 0.199cm3/ g, mesoporous Kong Rongwei 0.115cm3/g。
Fig. 4 is shown as the XRD characterization result of multi-stage porous SAPO-11 molecular sieve synthesized by this comparative example, in figure 5 it can be seen that with
Sieve sample in Fig. 1 by ultrasonic treatment is compared, and the SAPO-11 molecular sieve of ultrasonic treatment 1h preparation still has SAPO-11
Crystal form, and crystal type is fine.
Fig. 5 is shown as the stereoscan photograph of multi-stage porous SAPO-11 molecular sieve synthesized by this comparative example, in figure 5 it can be seen that
Not plus ultrasonic obtained sieve sample pattern is spherical shape, and apparent hollow structure occurs in the sample of ultrasound 1h preparation.Therefore,
The SAPO-11 sieve sample obtained after ultrasonic treatment, pore structure is more flourishing, and the specific surface area of molecular sieve is bigger, therefore
The molecular screen material of unit mass is stronger to the adsorption function of gas.
Fig. 6 is shown as the nitrogen adsorption isotherm of multi-stage porous SAPO-11 molecular sieve synthesized by this comparative example.It can see
To: compared with the sieve sample in Fig. 3 by ultrasonic treatment, the SAPO-11 molecular sieve of ultrasonic treatment 1h preparation is to nitrogen
Absorption property is more preferable.
As described above, SAPO-11 multistage porous molecular sieve and its ultrasonic wave added synthetic method of the invention, have beneficial below
Effect:
The multi-stage porous SAPO-11 molecular sieve prepared in 1-3 of the embodiment of the present invention reacts the hydroisomerizing of n-dodecane
Isomers yield is up to 81% (reaction condition: 320 DEG C, 4.5MPa, WHSV=1h-1, nH2:nC12=15).Fig. 7 is the present invention
Embodiment 1,2, the isomers yield change curve that product made from 3 reacts n-dodecane hydroisomerizing.It can from Fig. 7
To: the sieve sample of preparation is ultrasonically treated in the hydroisomerizing reaction of catalysis n-dodecane, and isomers yield is higher.And
For the sieve sample that comparative example 1 obtains in the hydroisomerizing reaction of catalysis n-dodecane, isomers yield only has 70%.Cause
This, the SAPO-11 sieve sample being ultrasonically treated, in the hydroisomerizing reaction of catalysis n-dodecane, Ke Yiti
The isomers yield of high hydroisomerizing reaction.
Compared with prior art, products obtained therefrom not only have complete SAPO-11 molecular sieve AEL structure and higher knot
Brilliant degree, and there are more meso-hole structures, in addition water consumption is seldom in sieve synthesis procedure, reduces in production process and gives up
The generation of water, yield and one-pot yield are all enhanced.
So the present invention effectively overcomes various shortcoming in the prior art and has high industrial utilization value.
It above are only part preferred embodiment of the invention, the present invention is not limited in the content of embodiment.For ability
For technical staff in domain, can there are various change and change in the conception range of technical solution of the present invention, made
What changes and change, within that scope of the present invention.
Claims (10)
1. a kind of method that ultrasonic wave added prepares multi-stage porous SAPO-11 molecular sieve, this method are as follows: by silicon source, phosphorus source, silicon source, go
It after ionized water, micropore template agent and mesoporous template mix in proportion, is ultrasonically treated, is then stirred at room temperature to mixture
Become colloidal sol, dry, grinding, hydrothermal crystallizing, roasting removal micropore template agent, obtains multi-stage porous SAPO-11 after product separation drying
Molecular sieve.
2. a kind of method that ultrasonic wave added prepares multi-stage porous SAPO-11 molecular sieve as described in claim 1, it is characterised in that:
Source of aluminium is boehmite or aluminium isopropoxide；The silicon source is silica gel or ethyl orthosilicate.
3. a kind of method that ultrasonic wave added prepares multi-stage porous SAPO-11 molecular sieve as described in claim 1, it is characterised in that:
The mesoporous template is cetyl trimethylammonium bromide or hexadecyltrimethylammonium chloride or active carbon.
4. a kind of method that ultrasonic wave added prepares multi-stage porous SAPO-11 molecular sieve as described in claim 1, it is characterised in that:
Molar ratio between the silicon source, silicon source, phosphorus source, micropore template agent and mesoporous template are as follows: (0.05-0.48): 1:(0.7-
1.2): (0.8-2): (0.01-0.2).
5. a kind of method that ultrasonic wave added prepares multi-stage porous SAPO-11 molecular sieve as described in claim 1, which is characterized in that
The condition of the ultrasonic treatment are as follows: ultrasonic power 200-400w, supersonic frequency 20-60kHz, ultrasonic time 0.5-4h.
6. a kind of method that ultrasonic wave added prepares multi-stage porous SAPO-11 molecular sieve as described in claim 1, it is characterised in that:
The temperature of the hydrothermal crystallizing of the colloidal sol is 160-220 DEG C, and the time of hydrothermal crystallizing is 12-36h.
7. a kind of method that ultrasonic wave added prepares multi-stage porous SAPO-11 molecular sieve as described in claim 1, it is characterised in that:
Maturing temperature is 500-600 DEG C after the product drying.
8. a kind of multi-stage porous SAPO-11 molecular sieve, which is obtained by the described in any item method preparations of claim 1-7
?.
9. multi-stage porous SAPO-11 molecular sieve as claimed in claim 8, it is characterised in that: the multi-stage porous SAPO-11 molecular sieve
Partial size be 2-10 microns, external surface area 89m2/g。
10. multi-stage porous SAPO-11 molecular sieve as claimed in claim 8, it is characterised in that: the multi-stage porous SAPO-11 molecule
Sieve the application in the reaction of n-dodecane hydroisomerizing.
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| CN109663509B (en) * | 2019-01-18 | 2022-01-21 | 中国科学院上海高等研究院 | Preparation method of hierarchical pore SAPO-34 molecular sieve membrane |
| CN109939729B (en) * | 2019-04-16 | 2021-07-27 | 中国科学院上海高等研究院 | Preparation method and application of Pt/SAPO-11 bifunctional catalyst |
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| CN110182826A (en) * | 2019-05-17 | 2019-08-30 | 大连理工大学 | A method of synthesizing hollow SSZ-13 molecular sieve |
| CN111410207B (en) * | 2020-03-12 | 2022-11-25 | 青岛科技大学 | Normal-pressure synthesis method of SAPO-11 molecular sieve |
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