CN115432712A - Nano-crystal material based on steric hindrance regulation and control and preparation method thereof - Google Patents
Nano-crystal material based on steric hindrance regulation and control and preparation method thereof Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 239000000463 material Substances 0.000 title claims description 22
- 239000002159 nanocrystal Substances 0.000 title claims description 20
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 22
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000002707 nanocrystalline material Substances 0.000 claims abstract description 19
- 238000006243 chemical reaction Methods 0.000 claims abstract description 17
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 13
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 13
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 13
- 238000000034 method Methods 0.000 claims abstract description 12
- 238000001035 drying Methods 0.000 claims abstract description 11
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 10
- 230000032683 aging Effects 0.000 claims abstract description 10
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 10
- 239000010703 silicon Substances 0.000 claims abstract description 10
- 239000008367 deionised water Substances 0.000 claims abstract description 9
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 9
- 238000003756 stirring Methods 0.000 claims abstract description 8
- 238000002425 crystallisation Methods 0.000 claims abstract description 7
- 230000008025 crystallization Effects 0.000 claims abstract description 7
- 238000005406 washing Methods 0.000 claims abstract description 6
- 239000000376 reactant Substances 0.000 claims abstract description 5
- HPXRVTGHNJAIIH-UHFFFAOYSA-N cyclohexanol Chemical compound OC1CCCCC1 HPXRVTGHNJAIIH-UHFFFAOYSA-N 0.000 claims description 7
- 239000011734 sodium Substances 0.000 claims description 7
- HZAXFHJVJLSVMW-UHFFFAOYSA-N 2-Aminoethan-1-ol Chemical compound NCCO HZAXFHJVJLSVMW-UHFFFAOYSA-N 0.000 claims description 6
- 239000002202 Polyethylene glycol Substances 0.000 claims description 6
- CBTVGIZVANVGBH-UHFFFAOYSA-N aminomethyl propanol Chemical compound CC(C)(N)CO CBTVGIZVANVGBH-UHFFFAOYSA-N 0.000 claims description 6
- 229920001223 polyethylene glycol Polymers 0.000 claims description 6
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 6
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 6
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 5
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims description 5
- 229910052708 sodium Inorganic materials 0.000 claims description 5
- 239000003112 inhibitor Substances 0.000 claims description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical group O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 3
- SMZOGRDCAXLAAR-UHFFFAOYSA-N aluminium isopropoxide Chemical compound [Al+3].CC(C)[O-].CC(C)[O-].CC(C)[O-] SMZOGRDCAXLAAR-UHFFFAOYSA-N 0.000 claims description 3
- DIZPMCHEQGEION-UHFFFAOYSA-H aluminium sulfate (anhydrous) Chemical compound [Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O DIZPMCHEQGEION-UHFFFAOYSA-H 0.000 claims description 3
- 229910021485 fumed silica Inorganic materials 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims description 3
- XKMRRTOUMJRJIA-UHFFFAOYSA-N ammonia nh3 Chemical compound N.N XKMRRTOUMJRJIA-UHFFFAOYSA-N 0.000 abstract description 18
- 238000001179 sorption measurement Methods 0.000 abstract description 16
- 230000000694 effects Effects 0.000 abstract description 9
- -1 ammonium ions Chemical class 0.000 abstract description 6
- 230000015572 biosynthetic process Effects 0.000 abstract description 5
- 239000013078 crystal Substances 0.000 abstract description 5
- 238000003786 synthesis reaction Methods 0.000 abstract description 5
- 239000002245 particle Substances 0.000 abstract description 4
- 238000009792 diffusion process Methods 0.000 abstract description 3
- 230000008569 process Effects 0.000 abstract description 2
- 238000010899 nucleation Methods 0.000 abstract 1
- 230000006911 nucleation Effects 0.000 abstract 1
- 239000002808 molecular sieve Substances 0.000 description 18
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 18
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- 238000001914 filtration Methods 0.000 description 3
- 239000010881 fly ash Substances 0.000 description 3
- 239000011148 porous material Substances 0.000 description 3
- 239000002351 wastewater Substances 0.000 description 3
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 2
- 241001465754 Metazoa Species 0.000 description 2
- CSDREXVUYHZDNP-UHFFFAOYSA-N alumanylidynesilicon Chemical compound [Al].[Si] CSDREXVUYHZDNP-UHFFFAOYSA-N 0.000 description 2
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- 238000012512 characterization method Methods 0.000 description 2
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- 230000004048 modification Effects 0.000 description 2
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 2
- 239000004810 polytetrafluoroethylene Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 150000003384 small molecules Chemical class 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229910052908 analcime Inorganic materials 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000000149 chemical water pollutant Substances 0.000 description 1
- 238000004939 coking Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 239000003651 drinking water Substances 0.000 description 1
- 235000020188 drinking water Nutrition 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 238000012851 eutrophication Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 210000003608 fece Anatomy 0.000 description 1
- 239000003337 fertilizer Substances 0.000 description 1
- 150000002605 large molecules Chemical class 0.000 description 1
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- 239000012528 membrane Substances 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- 235000015097 nutrients Nutrition 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 239000002910 solid waste Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
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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
- 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
- C01B39/14—Type A
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/16—Alumino-silicates
- B01J20/18—Synthetic zeolitic molecular sieves
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- 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
- C01B39/14—Type A
- C01B39/145—Type A using at least one organic template directing agent
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4806—Sorbents characterised by the starting material used for their preparation the starting material being of inorganic character
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4812—Sorbents characterised by the starting material used for their preparation the starting material being of organic character
-
- 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
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/16—Nitrogen compounds, e.g. ammonia
Abstract
The invention discloses a nano-crystalline material based on steric hindrance regulation and control and a preparation method thereof, wherein the preparation method comprises the following steps: adding an aluminum source, sodium hydroxide, a silicon source and a steric hindrance agent M into deionized water, and uniformly stirring to obtain mixed gel; and placing the mixed gel in a reaction kettle, placing reactants in a high-pressure reaction kettle for crystallization reaction after water bath aging, and washing and drying a product to obtain the nano-crystalline material based on steric hindrance regulation and control. According to the invention, the spatial position resisting agent is added in the synthesis process of the nanocrystalline material, so that the crystal nucleation and growth rate is slowed, the crystal dispersity is improved, the nanocrystalline material with small particle size and large specific surface area is generated, the smaller particle size means that the diffusion length in adsorption can be effectively reduced, the adsorption performance is increased, the larger specific surface area can provide more adsorption sites, more ammonium ions can be adsorbed, and the adsorption effect on ammonia nitrogen is enhanced.
Description
Technical Field
The invention relates to the technical field of water pollution treatment, in particular to a nano-crystal material based on steric hindrance regulation and control and a preparation method thereof.
Background
The sources of the ammonia nitrogen wastewater can be divided into a natural source and an artificial source. The natural sources mainly include degradation of some nitrogenous organic matters in nature, such as animal excreta, animal and plant debris and loss of plant nitrogen nutrients, although a large amount of ammonia nitrogen comes from the natural sources every year, the ammonia nitrogen is highly dispersed and has low concentration, and the degree of harming human health is not reached; the artificial sources mainly include: although the total ammonia nitrogen content of metallurgy, coking, pharmacy, food, chemical fertilizer, landfill leachate and the like is less than that of natural sources, the concentration is generally higher due to high concentration, water eutrophication is caused, the quality of drinking water is reduced, and direct damage is caused to human health.
The NaA molecular sieve has strong ion exchange capacity due to the low silicon-aluminum ratio, and is a potential nano-crystal material for treating ammonia nitrogen wastewater through adsorption. The invention with publication number CN104291348B discloses a method for preparing novel analcite by adding a spatial steric inhibitor by using fly ash as a raw material, which can reduce the synthesis cost of analcite, realize the resource utilization of solid waste and improve the added value of fly ash, but the fly ash can be used as the raw material for synthesizing analcite through a complicated treatment process, which is not beneficial to mass production.
Disclosure of Invention
In view of the above, the invention provides a nano-crystalline material based on steric hindrance regulation and control and a preparation method thereof, so as to solve the problems that the existing analcime is not high in purity and is not beneficial to mass production.
In order to achieve the purpose, the technical scheme of the invention is realized as follows:
a preparation method of a nano-crystal material based on steric hindrance regulation comprises the following steps:
s1, adding an aluminum source, sodium hydroxide, a silicon source and a steric hindrance agent M into deionized water, and uniformly stirring to obtain mixed gel;
s2, placing the mixed gel in a reaction kettle, placing reactants in a high-pressure reaction kettle for crystallization reaction after water bath aging, and washing and drying a product to obtain the nano-crystal material based on steric hindrance regulation and control.
According to the scheme, in the step S1, in the mixed gel, according to the molar ratio, a silicon source/aluminum source =1.0-1.2, and a steric hindrance agent M/aluminum source =1.0-5.0.
According to the scheme, in the step S1, the aluminum source comprises one of aluminum sulfate, sodium metaaluminate and aluminum isopropoxide, and the silicon source is fumed silica or liquid silica sol.
According to the scheme, the spatial position resisting agent M comprises one of 2-amino-2-methyl-propanol (AMP), ethanolamine (MEA), polyvinylpyrrolidone (PVP), polyethylene glycol (PEG) and cyclohexanol (CyOH).
According to the scheme, the pH value of the mixed gel is 9-12.
According to the scheme, in the step S2, the temperature of the water bath aging is 30-60 ℃, and the time is 2-6h.
According to the scheme, in the step S2, the temperature of the crystallization reaction is 70-100 ℃, and the time is 4-8h.
According to the scheme, in the step S2, the drying temperature is 80-100 ℃, and the drying time is 12-24h.
On the basis of the scheme, the second purpose of the invention is to provide a nano-crystal material based on steric hindrance regulation and control, which is prepared by adopting the preparation method of the nano-crystal material based on steric hindrance regulation and control.
Compared with the prior art, the invention has the following advantages:
(1) The method utilizes the steric hindrance effect to regulate and control the synthesis of the nano-crystalline material, the prepared nano-crystalline material has large specific surface area, more ammonia nitrogen adsorbed in unit area and small crystal size, can effectively reduce diffusion length in adsorption, increases adsorption performance, and can provide more adsorption sites with larger specific surface area, thereby adsorbing more ammonium ions and enhancing the adsorption effect on the ammonia nitrogen.
(2) The preparation method provided by the invention is simple to operate, low in cost and wide in application prospect.
Drawings
In order to more clearly illustrate the technical solutions of the present invention or the prior art, some brief descriptions will be given below to the drawings used in the description of the embodiments or the prior art, and it is obvious that the drawings in the following description are some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings based on these drawings without creative efforts.
FIG. 1 is a scanning electron microscope SEM image of a nano-crystalline material based on steric hindrance control according to an embodiment of the present invention.
Detailed Description
In order to make the aforementioned objects, features and advantages of the present invention comprehensible, embodiments accompanied with figures are described in detail below.
It should be noted that in the description of the embodiments herein, the description of the term "some embodiments" means that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. Throughout this specification, the schematic representations of the terms used above do not necessarily refer to the same implementation or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The term "in.. Range" as used herein includes both ends, such as "in the range of 1 to 100" including both ends of 1 and 100.
The NaA type molecular sieve is a cubic crystal formed by mutually communicating alpha cages through eight-membered rings, the effective aperture is 0.42nm and is almost the same as the kinetic diameter of small molecules, so the NaA type molecular sieve has high separation and selection performance on the small molecules and the large molecules; meanwhile, the silicon-aluminum ratio is small, the hydrophilicity is strong, and the separation of polar molecules and non-polar molecules, water and organic matters and the like can be realized. How to utilize steric hindrance effect to regulate and control nanocrystalline materials so as to enable the nanocrystalline materials to be better applied to ammonia nitrogen wastewater treatment is a very valuable subject at present.
In order to solve the problems, the preparation method of the nano-crystalline material based on steric hindrance regulation comprises the following steps:
s1, adding an aluminum source into deionized water, uniformly stirring, sequentially adding sodium hydroxide (NaOH) and a silicon source, and uniformly stirring; adding a spatial position resistance agent M, and stirring at a low speed for 1-2h to obtain mixed gel;
s2, placing the mixed gel into a reaction kettle, placing reactants into a high-pressure reaction kettle for crystallization reaction after water bath aging, wherein the aging has the function of limiting the growth of the molecular sieve and reducing the size of the molecular sieve. And filtering the reactant, washing with deionized water and absolute ethyl alcohol, and drying to obtain the nano-crystal material based on steric hindrance regulation.
Specifically, in step S1, in the mixed gel, a silicon source/aluminum source =1.0 to 1.2, and a steric hindrance agent M/aluminum source =1.0 to 5.0 in terms of a molar ratio. That is, the molar ratio of each substance in the mixed gel is: siO 2 2 /Al 2 O 3 ＝1.0-1.2，Na 2 O/Si 2 O＝1.5-2.0，H 2 O/Na 2 O＝30-45，M/Al 2 O 3 ＝1.0-5.0。
The aluminum source comprises one of aluminum sulfate, sodium metaaluminate and aluminum isopropoxide, and the silicon source is fumed silica or liquid silica sol. The steric inhibitor M includes one of 2-amino-2-methyl-propanol (AMP), ethanolamine (MEA), z (PVP), polyethylene glycol (PEG), and cyclohexanol (CyOH).
Further, naOH is added to adjust the pH of the mixed solution, and in this example, the pH of the mixed gel is adjusted to 9-12.
Specifically, in the step S2, the temperature of the water bath aging is 30-60 ℃, and the time is 2-6h; the temperature of the crystallization reaction is 70-100 ℃, and the time is 4-8h; the drying temperature is 80-100 deg.C, and the drying time is 12-24h.
The NaA molecular sieve prepared by the method for regulating and controlling the synthesis of the nanocrystalline material through the steric hindrance effect has the advantages of large specific surface area, more ammonia nitrogen adsorbed in unit area, small crystal size, effective reduction of diffusion length in adsorption, increase of adsorption performance, larger specific surface area and capability of providing more adsorption sites, so that more ammonium ions can be adsorbed, and the adsorption effect on the ammonia nitrogen is enhanced.
On the basis of the scheme, the invention further provides a nano-crystal material based on steric hindrance regulation and control, and the nano-crystal material is prepared by adopting the preparation method of the nano-crystal material based on steric hindrance regulation and control.
The NaA molecular sieve with small particle size and high specific surface area is prepared by using a method for regulating and controlling the synthesis of a nanocrystalline material by using a steric hindrance effect, has larger specific surface area and pore volume, and has stronger adsorption effect on ammonia nitrogen; the removal rate of the ammonia nitrogen in the ammonia nitrogen wastewater reaches 80 to 95 percent.
On the basis of the above embodiments, the present invention is further illustrated by the following specific examples. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. The following examples are examples of experimental procedures not specified under specific conditions, generally according to the conditions recommended by the manufacturer. Unless otherwise indicated, percentages and parts are by mass.
Example 1
The embodiment provides a preparation method of a nano-crystal material based on steric hindrance regulation, which comprises the following steps:
1) 1.968 adding sodium metaaluminate into 21mL of deionized water, uniformly stirring, sequentially adding 3g of NaOH and 4mL of liquid silica sol, and stirring for 15min to obtain mixed gel;
2) And transferring the mixed gel into a polytetrafluoroethylene container, aging in a water bath for 4h, setting the temperature at 60 ℃, then putting the mixed gel into a high-pressure reaction kettle, heating to 90 ℃, crystallizing for 4h, filtering, washing with deionized water and absolute ethyl alcohol, and drying at 100 ℃ for 12h to obtain the NaA molecular sieve label L1.
Example 2
The embodiment provides a preparation method of a nano-crystal material based on steric hindrance regulation, which comprises the following steps:
1) 1.968 sodium metaaluminate is added into 21mL of deionized water and stirred uniformly, 3g of NaOH and 4mL of liquid silica sol are sequentially added and stirred for 15min, 4.6mL of AMP as a steric hindrance agent is added, and the mixture is stirred at a low speed for 1h to obtain mixed gel;
2) And transferring the mixed gel into a polytetrafluoroethylene container, aging in water bath for 4h at the temperature of 60 ℃, then putting the mixed gel into a high-pressure reaction kettle, heating to 90 ℃, crystallizing for 4h, filtering, washing with deionized water and absolute ethyl alcohol, and drying at 100 ℃ for 12h to obtain the NaA molecular sieve labeled as L2.
Example 3
The embodiment provides a preparation method of a nano-crystal material based on steric hindrance regulation, which is different from the embodiment 2 in that:
in the step 1), adding 2.9mL of MEA (membrane electrode assembly) as a spatial position resisting agent;
the remaining steps and parameters were the same as in example 2. The NaA molecular sieve is marked as L3.
Example 4
The embodiment provides a preparation method of a nano-crystal material based on steric hindrance regulation, which is different from the embodiment 2 in that:
in the step 1), adding 8.5mL of PEG as a spatial retarder;
the remaining steps and parameters were the same as in example 2. The NaA molecular sieve is marked as L4.
Example 5
The embodiment provides a preparation method of a nano-crystalline material based on steric hindrance control, which is different from the preparation method of the embodiment 2 in that:
in the step 1), 9.4mL PVP (polyvinyl pyrrolidone) of spatial retarder is added;
the remaining steps and parameters were the same as in example 2. The NaA molecular sieve is marked as L5.
Example 6
The embodiment provides a preparation method of a nano-crystal material based on steric hindrance regulation, which is different from the embodiment 2 in that:
in the step 1), adding a spatial retarder 5mL of CyOH;
the remaining steps and parameters were the same as in example 2. The NaA molecular sieve is obtained and marked as L6.
Taking the nano-crystal material NaA molecular sieve prepared in example 2 based on steric hindrance regulation as an example, the morphology and the structure of the nano-crystal material NaA molecular sieve are characterized, and a result graph shown in fig. 1 is obtained. As can be seen from FIG. 1, the NaA molecular sieve has uniform size and regular appearance.
Performance characterization of the nanocrystalline materials prepared in examples 1-6 resulted in specific surface areas (m) 2 G), pore volume (cm) 3 In terms of/g), size (nm) and ammonia nitrogen removal (%), as shown in Table 1:
TABLE 1 Performance characterization of nano-crystalline materials based on steric hindrance modulation
As can be seen from table 1, the NaA molecular sieve prepared after the spatial resistance agent is added has an increased specific surface area and a reduced particle size, and different spatial resistance agents have an influence on the specific surface area, the pore volume and the ammonia nitrogen adsorption performance of the NaA molecular sieve. It is understood from comparative examples 1 to 6 that the ammonia nitrogen adsorption effect is the best when the steric inhibitor, cyclohexanol, cyOH, is added, because the ion exchange capacity is large, and more ammonium ions can be adsorbed. That is, example 6 is the best example of the present invention, and has the best ammonia nitrogen removal rate.
Although the present disclosure has been described with reference to the above embodiments, the scope of the present disclosure is not limited thereto. Various changes and modifications may be effected therein by one of ordinary skill in the pertinent art without departing from the spirit and scope of the present disclosure, and these changes and modifications are intended to be within the scope of the present disclosure.
Claims (9)
1. A preparation method of a nano-crystalline material based on steric hindrance regulation is characterized by comprising the following steps:
s1, adding an aluminum source, sodium hydroxide, a silicon source and a steric hindrance agent M into deionized water, and uniformly stirring to obtain mixed gel;
s2, placing the mixed gel in a reaction kettle, placing reactants in a high-pressure reaction kettle for crystallization reaction after water bath aging, and washing and drying a product to obtain the nano-crystal material based on steric hindrance regulation and control.
2. The method according to claim 1, wherein in step S1, the mixed gel contains silicon source/aluminum source =1-1.2 and steric hindrance agent M/aluminum source =1-5 in terms of molar ratio.
3. The method of claim 2, wherein in step S1, the aluminum source comprises one of aluminum sulfate, sodium metaaluminate and aluminum isopropoxide, and the silicon source is fumed silica or liquid silica sol.
4. The production method according to claim 2 or 3, wherein the steric inhibitor M comprises one of 2-amino-2-methyl-propanol, ethanolamine, polyvinylpyrrolidone, polyethylene glycol, and cyclohexanol.
5. The method of claim 4, wherein the pH of the mixed gel is 9 to 12.
6. The preparation method according to claim 4, wherein in the step S2, the temperature of the water bath aging is 30-60 ℃ and the time is 2-6h.
7. The method according to claim 6, wherein the crystallization reaction is carried out at a temperature of 70-100 ℃ for 4-8 hours in step S2.
8. The method according to claim 7, wherein the drying is carried out at 80-100 ℃ for 12-24 hours in step S2.
9. A nano-crystalline material based on steric hindrance control, which is prepared by the method for preparing the nano-crystalline material based on steric hindrance control according to any one of claims 1 to 8.
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