CN109019621A - The preparation method of nanometer sodalite under a kind of low temperature - Google Patents
The preparation method of nanometer sodalite under a kind of low temperature Download PDFInfo
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- CN109019621A CN109019621A CN201811188376.4A CN201811188376A CN109019621A CN 109019621 A CN109019621 A CN 109019621A CN 201811188376 A CN201811188376 A CN 201811188376A CN 109019621 A CN109019621 A CN 109019621A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/20—Silicates
- C01B33/26—Aluminium-containing silicates, i.e. silico-aluminates
- C01B33/28—Base exchange silicates, e.g. zeolites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C01—INORGANIC CHEMISTRY
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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Abstract
The present invention provides a kind of preparation methods of nanometer sodalite under low temperature, comprising the following steps: weighs silicon source and highly basic first, stirs evenly after deionized water is added, obtain the alkaline slurry A containing aluminium;Then silicon source is added in the alkaline slurry A containing aluminium, is added while stirring, continued 30~45min of stirring after the completion of being added, obtain silica-alumina gel;Silica-alumina gel then carries out at 25~35 DEG C to crystallization in sealed environment, crystallization time is 4~for 24 hours;Finally the product after crystallization is filtered, and will filter product to be washed to pH is 8~9, in 60~120 DEG C of dry 12~48h, obtains a nanometer sodalite.The present invention prepares nanometer sodalite by the lower crystallization of low temperature; preparation process is simple; mild condition, it is low in cost, and it is not added with any organic additive; obtained nanometer sodalite good crystallinity; purity is high, partial size are 20~30nm, are suitable for absorption and hydrogen storage material aspect; it is suitble to large-scale production, there is certain economic benefit and realistic meaning.
Description
Technical field
The present invention relates to technical field of inorganic nano-material preparation, the preparation side of nanometer sodalite under specially a kind of low temperature
Method.
Background technique
Sodalite is a kind of porous silicoaluminate zeolite with small-bore, its aluminum-oxygen tetrahedron and oxygen-octahedron phase
Interconnection structure can fill small molecule, non-stoichiometric salt at the three-dimensional framework with cube hole (referred to as SOD cage), in cage
Class and metal " cluster ".Since it is with unique space structure and physicochemical properties, sodalite is used as hydrogen storage extensively
Material, photochromic material and adsorbent.
Nanometer sodalite has the characteristics that molecule is easy to diffusion and large specific surface area and is closed since its crystallite dimension is small
Note has bigger application value in terms of adsorbing with hydrogen storage.In recent years, the researchers conjunction to nanometer sodalite always
At being explored, have some pertinent literature reports.Ma Yingchong etc. (Chemical Journal of Chinese Universities, 2006,27:739~741) with
1- ethyl-3-methylimidazole bromide ([emim] Br) ionic liquid is solvent, is made crystal grain about 200~500nm's under normal pressure
Sodalite crystal, research think that solvent or template different in system causes the difference of zeolite crystal growth environment, lead to shape
At crystal morphology it is different.On this basis, Zang Lijun etc. (2013,32 (3): 220~223) adopt by Dalian Polytechnic University's journal
With the mode of microwave heating, the sodalite nano powder of high-crystallinity, narrow particle size distribution is synthesized under the open ionic liquid system of normal pressure
Body, average grain diameter are only 20nm or so.This method is compared with the ionothermal synthesis of conventional heating, and the dosage of ionic liquid reduces
20%, crystallization time shortens 90%, reduces costs, improves combined coefficient.Both methods is required with ionic liquid
As crystallization medium, cost is too high, it is therefore necessary to find other more effective experimental methods.Yang little Yue etc. (science and technology with
2015,15 (20): engineering 249~251) under normal-pressure open system, is taken water as a solvent, is synthesized in the way of microwave heating
Crystallinity is high, partial size 30nm or so nanometer sodalite.The method greatly reduces the cost that ionothermal synthesis uses ionic liquid.
Ji Yuanyuan etc. (CN201510347496.4) reports one kind without condition existing for any organic additive and structure directing agent
Under, the method for preparing nanoscale sodalite.This method is synthesized using two steps, by the alkaline mixed serum of silicon-aluminum containing 40~100
DEG C 2~10h of crystallization, then in 70~200 DEG C of 1~5h of aging, sodalite crystalline form obtained is having a size of 200~800nm.Jiang Yang etc.
A kind of method that (CN 201510021734.2) reports low temperature controlledly synthesis SOD type sodalite, it is molten that this method prepares mixing first
Then liquid clay mineral is added in mixed solution under agitation, stir 0.5~4h, it is anti-that mixture is sealed in hydro-thermal
Answer in kettle 12~36h of hydro-thermal reaction under the conditions of 60~120 DEG C.The sodalite of this method preparation is by diameter close to 2um, thickness
For the stereochemical structure that the round sheet crystal of 30~50nm assembles, these round sheet crystal have common center (former
Point), they are mutually inlayed centered on origin is staggeredly assembled into frame structure.
In conclusion the method for existing synthesis nanometer sodalite mainly has hydrothermal synthesis method, ionothermal synthesis etc., but close
At method there are still higher cost, preparation process is complicated the disadvantages of.Therefore, it is necessary to find it is a kind of at low cost, quickly and easily
Nanometer sodalite synthetic method.
Summary of the invention
The purpose of the present invention is to solve the deficiency of above-mentioned technology, a kind of preparation side of nanometer sodalite under low temperature is provided
Method, a crystallization generates at low temperature for this method reaction, and crystallization time is short, and crystallization condition is mild, and synthesis procedure is simple, and equipment is wanted
Ask low, it is at low cost.
To achieve the above object, the technical solution adopted by the present invention is that:
The preparation method of nanometer sodalite under a kind of low temperature, comprising the following steps:
Step 1 weighs silicon source and highly basic, stirs evenly after deionized water is added, obtains the alkaline slurry A containing aluminium;
In step 2, the alkaline slurry A containing aluminium for obtaining silicon source addition step 1, it is added while stirring, after the completion of addition
Continue 30~45min of stirring, obtains silica-alumina gel;
Step 3, the silica-alumina gel for obtaining step 2 carry out crystallization, crystallization time in sealed environment at 25~35 DEG C
For 4~for 24 hours;
Step 4 filters the product after step 3 crystallization, and will filter product to be washed to pH is 8~9, then in 60
~120 DEG C of dry 12~48h, finally obtain a nanometer sodalite.
Preferably, step 1 silicon source is b propanol aluminium.
Preferably, step 1 highly basic is sodium hydroxide.
Preferably, step 2 silicon source is one of silica solution, solid silicone or white carbon black, wherein titanium dioxide in silica solution
The mass fraction of silicon is 30%.
Preferably, by the dosage of silicon source with SiO2Meter, by the dosage of silicon source with Al2O3Meter, the dosage of highly basic is with Na2O meter,
The molar ratio of each substance is Na in silica-alumina gel described in step 32O:Al2O3: SiO2: H2O=2.0~7.8:0.3~1.2:1.0:
60~200.
Compared with prior art, beneficial effects of the present invention are as follows:
1, nanometer sodalite is generated in the lower crystallization of 25~35 DEG C of low temperature in the present invention, and reaction condition is mild, synthesizes work
Sequence is simple, and it is short to expend the time;
2, the present invention directly prepares nanometer sodalite under conditions of not using any organic additive, meets Green Chemistry
Development need;
3, nanometer sodalite good crystallinity prepared by the present invention, purity is high, the sodalite partial size of preparation is on the left side 20~30nm
The right side is more suitable and applies in terms of adsorbing with hydrogen storage material, be suitble to large-scale production, has certain economic benefit.
Detailed description of the invention
Fig. 1 is X-ray diffraction (XRD) spectrogram for the nanometer sodalite powder that in the present invention prepared by embodiment 1;
Fig. 2 is transmission electron microscope (TEM) photo for the nanometer sodalite powder that in the present invention prepared by embodiment 1.
Specific embodiment
Below by specific embodiment example, the present invention will be described in detail.The scope of the present invention is not limited to the tool
Body embodiment.
Embodiment 1
Step 1 weighs in 7.46g b propanol aluminium and 9.56g sodium hydroxide addition beaker, adds 59.50g deionization
Water, stirring are completely dissolved raw material, the alkaline slurry A containing aluminium are made;
Step 2 weighs the silica solution that 5.22g silica quality score is 30%, is slowly added into silica solution under stirring
In the alkaline slurry A containing aluminium that step 1 obtains, continues to stir 30min after addition, form silica-alumina gel;
Step 3, the silica-alumina gel for obtaining step 2 are transferred to close in the stainless steel synthesis reactor with polytetrafluoroethyllining lining
Envelope, is placed in water-bath, sets water bath temperature as 25 DEG C, crystallization 6h;
Step 4, after the reaction was completed takes out synthesis reactor, reaction mixture is filtered, and with deionized water to filter cake into
Row washing, until washing pH value of solution to 9;By filter cake, for 24 hours, white nanometer sodalite powder is can be obtained in drying at 100 DEG C.
Embodiment 2
Step 1 weighs in 9.48g b propanol aluminium and 12.25g sodium hydroxide addition beaker, adds 69.75g deionization
Water, stirring are completely dissolved raw material, the alkaline slurry A containing aluminium are made;
Step 2 weighs the silica solution that 6.16g silica quality score is 30%, is slowly added into silica solution under stirring
In the alkaline slurry A containing aluminium that step 1 obtains, continues to stir 30min after addition, form silica-alumina gel;
Step 3, the silica-alumina gel for obtaining step 2 are transferred to close in the stainless steel synthesis reactor with polytetrafluoroethyllining lining
Envelope, is placed in water-bath, sets water bath temperature as 25 DEG C, crystallization 12h;
Step 4, after the reaction was completed takes out synthesis reactor, reaction mixture is filtered, and with deionized water to filter cake into
Row washing, until washing pH value of solution to 8;By filter cake, for 24 hours, white nanometer sodalite powder is can be obtained in drying at 100 DEG C.
Embodiment 3
Step 1 weighs in 10.58g b propanol aluminium and 11.05g sodium hydroxide addition beaker, adds 55.25g deionization
Water, stirring are completely dissolved raw material, the alkaline slurry A containing aluminium are made;
Step 2 weighs the silica solution that 5.78g silica quality score is 30%, is slowly added into silica solution under stirring
In the alkaline slurry A containing aluminium that step 1 obtains, continues to stir 45min after addition, form silica-alumina gel;
Step 3, the silica-alumina gel for obtaining step 2 are transferred to close in the stainless steel synthesis reactor with polytetrafluoroethyllining lining
Envelope, is placed in water-bath, sets water bath temperature as 25 DEG C, crystallization is for 24 hours;
Step 4, after the reaction was completed takes out synthesis reactor, reaction mixture is filtered, and with deionized water to filter cake into
Row washing, until washing pH value of solution to 8;Filter cake is dried into 48h at 60 DEG C, white nanometer sodalite powder can be obtained.
Embodiment 4
Step 1 weighs in 8.90g b propanol aluminium and 10.16g sodium hydroxide addition beaker, adds 65.50g deionization
Water, stirring are completely dissolved raw material, the alkaline slurry A containing aluminium are made;
Step 2 weighs 1.28g solid silicone, is slowly added into the alkaline slurry A containing aluminium that step 1 obtains, adds under stirring
Continue to stir 30min after entering, forms silica-alumina gel;
Step 3, the silica-alumina gel for obtaining step 2 are transferred to close in the stainless steel synthesis reactor with polytetrafluoroethyllining lining
Envelope, is placed in water-bath, sets water bath temperature as 25 DEG C, crystallization 6h;
Step 4, after the reaction was completed takes out synthesis reactor, reaction mixture is filtered, and with deionized water to filter cake into
Row washing, until washing pH value of solution to 9;Filter cake is dried into 12h at 120 DEG C, white sodalite powder can be obtained.
Embodiment 5
Step 1 weighs in 9.45g b propanol aluminium and 10.78g sodium hydroxide addition beaker, adds 60.55g deionization
Water, stirring are completely dissolved raw material, the alkaline slurry A containing aluminium are made;
Step 2 weighs 1.48g solid silicone, is slowly added into the alkaline slurry A containing aluminium that step 1 obtains, adds under stirring
Continue to stir 30min after entering, forms silica-alumina gel;
Step 3, the silica-alumina gel for obtaining step 2 are transferred to close in the stainless steel synthesis reactor with polytetrafluoroethyllining lining
Envelope, is placed in water-bath, sets water bath temperature as 25 DEG C, crystallization 12h;
Step 4, after the reaction was completed takes out synthesis reactor, reaction mixture is filtered, and with deionized water to filter cake into
Row washing, until washing pH value of solution to 9;Filter cake is dried into 36h at 80 DEG C, white nanometer sodalite powder can be obtained.
Embodiment 6
Step 1 weighs in 9.05g b propanol aluminium and 13.12g sodium hydroxide addition beaker, adds 70.25g deionization
Water, stirring are completely dissolved raw material, the alkaline slurry A containing aluminium are made;
Step 2 weighs 1.25g white carbon black, is slowly added into the alkaline slurry A containing aluminium that step 1 obtains under stirring, is added
After continue stir 30min, formed silica-alumina gel;
Step 3, the silica-alumina gel for obtaining step 2 are transferred to close in the stainless steel synthesis reactor with polytetrafluoroethyllining lining
Envelope, is placed in water-bath, sets water bath temperature as 25 DEG C, crystallization 6h;
Step 4, after the reaction was completed takes out synthesis reactor, reaction mixture is filtered, and with deionized water to filter cake into
Row washing, until washing pH value of solution to 8;By filter cake, for 24 hours, white nanometer sodalite powder is can be obtained in drying at 100 DEG C.
Embodiment 7
Step 1 weighs in 9.65g b propanol aluminium and 13.47g sodium hydroxide addition beaker, adds 65.25g deionization
Water, stirring are completely dissolved raw material, the alkaline slurry A containing aluminium are made;
Step 2 weighs 1.42g white carbon black, is slowly added into the alkaline slurry A containing aluminium that step 1 obtains under stirring, is added
After continue stir 45min, formed silica-alumina gel;
Step 3, the silica-alumina gel for obtaining step 2 are transferred to close in the stainless steel synthesis reactor with polytetrafluoroethyllining lining
Envelope, is placed in water-bath, sets water bath temperature as 25 DEG C, crystallization 12h;
Step 4, after the reaction was completed takes out synthesis reactor, reaction mixture is filtered, and with deionized water to filter cake into
Row washing, until washing pH value of solution to 9;Filter cake is dried into 12h at 120 DEG C, white nanometer sodalite powder can be obtained.
Embodiment 8
Step 1 weighs in 7.46g b propanol aluminium and 9.56g sodium hydroxide addition beaker, adds 59.50g deionization
Water, stirring are completely dissolved raw material, the alkaline slurry A containing aluminium are made;
Step 2 weighs the silica solution that 5.22g silica quality score is 30%, is slowly added into silica solution under stirring
In the alkaline slurry A containing aluminium that step 1 obtains, continues to stir 30min after addition, form silica-alumina gel;
Step 3, the silica-alumina gel for obtaining step 2 are transferred to close in the stainless steel synthesis reactor with polytetrafluoroethyllining lining
Envelope, is placed in water-bath, sets water bath temperature as 30 DEG C, crystallization 5h;
Step 4, after the reaction was completed takes out synthesis reactor, reaction mixture is filtered, and with deionized water to filter cake into
Row washing, until washing pH value of solution to 9;By filter cake, for 24 hours, white nanometer sodalite powder is can be obtained in drying at 100 DEG C.
Embodiment 9
Step 1 weighs in 7.46g b propanol aluminium and 9.56g sodium hydroxide addition beaker, adds 59.50g deionization
Water, stirring are completely dissolved raw material, the alkaline slurry A containing aluminium are made;
Step 2 weighs the silica solution that 5.22g silica quality score is 30%, is slowly added into silica solution under stirring
In the alkaline slurry A containing aluminium that step 1 obtains, continues to stir 30min after addition, form silica-alumina gel;
Step 3, the silica-alumina gel for obtaining step 2 are transferred to close in the stainless steel synthesis reactor with polytetrafluoroethyllining lining
Envelope, is placed in water-bath, sets water bath temperature as 35 DEG C, crystallization 4h;
Step 4, after the reaction was completed takes out synthesis reactor, reaction mixture is filtered, and with deionized water to filter cake into
Row washing, until washing pH value of solution to 9;By filter cake, for 24 hours, white nanometer sodalite powder is can be obtained in drying at 100 DEG C.
The white nanometer sodalite powder that we obtain embodiment 1 carries out X-ray diffraction test (XRD) and transmitted electron
Microscope tests (TEM), and Fig. 1 is the X-ray diffraction spectrogram of 1 sample of embodiment, and synthetic product is pure as can see from Figure 1
SOD structure, i.e., pure sodalite.Fig. 2 is the transmission electron microscope photo of 1 sample of embodiment, as seen from Figure 2 synthetic product
For nanometer-size die deposit, size of microcrystal is 20~30nm.
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, without departing from the principle of the present invention, it can also make several improvements and retouch, these improvements and modifications are also answered
It is considered as protection scope of the present invention.
Claims (5)
1. the preparation method of nanometer sodalite under a kind of low temperature, which comprises the following steps:
Step 1 weighs silicon source and highly basic, stirs evenly after deionized water is added, obtains the alkaline slurry A containing aluminium;
It in step 2, the alkaline slurry A containing aluminium for obtaining silicon source addition step 1, is added, continues after the completion of being added while stirring
30~45min is stirred, silica-alumina gel is obtained;
Step 3, the silica-alumina gel for obtaining step 2 carry out crystallization in sealed environment at 25~35 DEG C, and crystallization time is 4~
24h;
Step 4 filters the product after step 3 crystallization, and will filter product to be washed to pH is 8~9, then in 60~
120 DEG C of dry 12~48h, finally obtain a nanometer sodalite.
2. the preparation method of nanometer sodalite under a kind of low temperature according to claim 1, which is characterized in that described in step 1
Silicon source is b propanol aluminium.
3. the preparation method of nanometer sodalite under a kind of low temperature according to claim 1, which is characterized in that described in step 1
Highly basic is sodium hydroxide.
4. the preparation method of nanometer sodalite under a kind of low temperature according to claim 1, which is characterized in that described in step 2
Silicon source is one of silica solution, solid silicone or white carbon black, and the mass fraction of silica is 30% in the silica solution.
5. the preparation method of nanometer sodalite under a kind of low temperature according to claim 1, which is characterized in that by the use of silicon source
Amount is with SiO2Meter, by the dosage of silicon source with Al2O3Meter, the dosage of highly basic is with Na2O is counted, each substance in silica-alumina gel described in step 3
Molar ratio be Na2O:Al2O3: SiO2: H2O=2.0~7.8:0.3~1.2:1.0:60~200.
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