CN107381591A - A kind of preparation method of the sodalite of petal-shaped at room temperature - Google Patents
A kind of preparation method of the sodalite of petal-shaped at room temperature Download PDFInfo
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- CN107381591A CN107381591A CN201710691649.6A CN201710691649A CN107381591A CN 107381591 A CN107381591 A CN 107381591A CN 201710691649 A CN201710691649 A CN 201710691649A CN 107381591 A CN107381591 A CN 107381591A
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- sodalite
- room temperature
- petal
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- 229910052665 sodalite Inorganic materials 0.000 title claims abstract description 57
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- 239000000203 mixture Substances 0.000 claims abstract description 32
- 238000002425 crystallisation Methods 0.000 claims abstract description 29
- 230000008025 crystallization Effects 0.000 claims abstract description 29
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 27
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 27
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 26
- 239000010703 silicon Substances 0.000 claims abstract description 26
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 22
- 239000002994 raw material Substances 0.000 claims abstract description 21
- 239000012065 filter cake Substances 0.000 claims abstract description 18
- 239000008367 deionised water Substances 0.000 claims abstract description 16
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 16
- 238000010438 heat treatment Methods 0.000 claims abstract description 16
- 238000003756 stirring Methods 0.000 claims abstract description 16
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 19
- 238000013019 agitation Methods 0.000 claims description 10
- 239000004115 Sodium Silicate Substances 0.000 claims description 9
- 239000000376 reactant Substances 0.000 claims description 9
- 235000019795 sodium metasilicate Nutrition 0.000 claims description 9
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 9
- 229910052911 sodium silicate Inorganic materials 0.000 claims description 9
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 claims description 5
- 229910021502 aluminium hydroxide Inorganic materials 0.000 claims description 5
- 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
- ANBBXQWFNXMHLD-UHFFFAOYSA-N aluminum;sodium;oxygen(2-) Chemical compound [O-2].[O-2].[Na+].[Al+3] ANBBXQWFNXMHLD-UHFFFAOYSA-N 0.000 claims description 2
- 229910001388 sodium aluminate Inorganic materials 0.000 claims description 2
- 239000000126 substance Substances 0.000 claims description 2
- 238000002242 deionisation method Methods 0.000 claims 1
- 230000015572 biosynthetic process Effects 0.000 abstract description 11
- 238000003786 synthesis reaction Methods 0.000 abstract description 10
- 238000000034 method Methods 0.000 abstract description 6
- 239000000047 product Substances 0.000 abstract description 6
- 230000009286 beneficial effect Effects 0.000 abstract description 5
- 239000000463 material Substances 0.000 abstract description 5
- 238000005406 washing Methods 0.000 abstract description 5
- 239000006259 organic additive Substances 0.000 abstract description 4
- 238000006243 chemical reaction Methods 0.000 abstract description 2
- 238000011031 large-scale manufacturing process Methods 0.000 abstract description 2
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 14
- 239000004810 polytetrafluoroethylene Substances 0.000 description 14
- 239000003643 water by type Substances 0.000 description 14
- 239000000843 powder Substances 0.000 description 11
- -1 sodium aluminates Chemical class 0.000 description 10
- 235000011121 sodium hydroxide Nutrition 0.000 description 9
- 239000010457 zeolite Substances 0.000 description 8
- 229910021536 Zeolite Inorganic materials 0.000 description 7
- 239000013078 crystal Substances 0.000 description 7
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 7
- 229910052708 sodium Inorganic materials 0.000 description 5
- 239000011734 sodium Substances 0.000 description 5
- 230000004048 modification Effects 0.000 description 4
- 238000012986 modification Methods 0.000 description 4
- 238000010189 synthetic method Methods 0.000 description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 3
- 230000008901 benefit Effects 0.000 description 3
- JYIMWRSJCRRYNK-UHFFFAOYSA-N dialuminum;disodium;oxygen(2-);silicon(4+);hydrate Chemical compound O.[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[Na+].[Na+].[Al+3].[Al+3].[Si+4] JYIMWRSJCRRYNK-UHFFFAOYSA-N 0.000 description 3
- 238000005265 energy consumption Methods 0.000 description 3
- 239000001257 hydrogen Substances 0.000 description 3
- 229910052739 hydrogen Inorganic materials 0.000 description 3
- 239000011232 storage material Substances 0.000 description 3
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-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
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000003292 glue Substances 0.000 description 2
- 238000001027 hydrothermal synthesis Methods 0.000 description 2
- 239000004575 stone Substances 0.000 description 2
- HZAXFHJVJLSVMW-UHFFFAOYSA-N 2-Aminoethan-1-ol Chemical compound NCCO HZAXFHJVJLSVMW-UHFFFAOYSA-N 0.000 description 1
- KKCBUQHMOMHUOY-UHFFFAOYSA-N Na2O Inorganic materials [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 description 1
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- NWGKJDSIEKMTRX-MDZDMXLPSA-N Sorbitan oleate Chemical compound CCCCCCCC\C=C\CCCCCCCC(=O)OCC(O)C1OCC(O)C1O NWGKJDSIEKMTRX-MDZDMXLPSA-N 0.000 description 1
- LWZFANDGMFTDAV-BURFUSLBSA-N [(2r)-2-[(2r,3r,4s)-3,4-dihydroxyoxolan-2-yl]-2-hydroxyethyl] dodecanoate Chemical compound CCCCCCCCCCCC(=O)OC[C@@H](O)[C@H]1OC[C@H](O)[C@H]1O LWZFANDGMFTDAV-BURFUSLBSA-N 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 150000001340 alkali metals Chemical class 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 235000006708 antioxidants Nutrition 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 229910052593 corundum Inorganic materials 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- ONCZQWJXONKSMM-UHFFFAOYSA-N dialuminum;disodium;oxygen(2-);silicon(4+);hydrate Chemical compound O.[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[Na+].[Na+].[Al+3].[Al+3].[Si+4].[Si+4].[Si+4].[Si+4] ONCZQWJXONKSMM-UHFFFAOYSA-N 0.000 description 1
- 230000008034 disappearance Effects 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 238000002389 environmental scanning electron microscopy Methods 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000002808 molecular sieve Substances 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 235000010482 polyoxyethylene sorbitan monooleate Nutrition 0.000 description 1
- 229920000053 polysorbate 80 Polymers 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 150000003384 small molecules Chemical class 0.000 description 1
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 1
- 229940080314 sodium bentonite Drugs 0.000 description 1
- 229910000280 sodium bentonite Inorganic materials 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 235000011067 sorbitan monolaureate Nutrition 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 238000010408 sweeping Methods 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
- 229910001845 yogo sapphire Inorganic materials 0.000 description 1
Classifications
-
- 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
-
- 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
- C01B33/2807—Zeolitic silicoaluminates with a tridimensional crystalline structure possessing molecular sieve properties; Isomorphous compounds wherein a part of the aluminium ore of the silicon present may be replaced by other elements such as gallium, germanium, phosphorus; Preparation of zeolitic molecular sieves from molecular sieves of another type or from preformed reacting mixtures
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Silicates, Zeolites, And Molecular Sieves (AREA)
Abstract
The invention discloses a kind of preparation method of the sodalite of petal-shaped at room temperature, belong to zeolitic material technical field.This method comprises the following steps：Sodium hydroxide and silicon source are weighed, adds deionized water, and heating stirring is completely dissolved raw material, and solution A is made；Silicon source is weighed, adds deionized water, and heating stirring is completely dissolved raw material, and solution B is made；Solution A and solution B are well mixed；Mixture is subjected to crystallization in room temperature；After crystallization, filter cake is dried 12 36h, you can obtain sodalite by washing until wash solution pH to 89 at 80 120 DEG C.The preparation method reaction of the present invention is carried out at room temperature, and mild condition is pollution-free without using organic additive；Synthesis procedure is simple, and time-consuming short, cost is low；Product good crystallinity, purity is high, and the sodalite of synthesis has petal-shaped pattern, is more beneficial for its suction-operated, is adapted to large-scale production.
Description
Technical field
The present invention relates to zeolitic material technical field, and in particular to a kind of preparation method of the sodalite of petal-shaped at room temperature.
Background technology
Sodalite is the zeolite that the SOD cages of body-centered cubic arrangement are formed by connecting by Dan Si and single hexatomic ring, is to enter first
Enter the zeolite molecular sieve of inorganic functional material field.Aluminum-oxygen tetrahedron has cube hole with interconnected form of silicon-oxy tetrahedron
(it is referred to as SOD cages, volume about 0.150nm3) three-dimensional framework, small molecule, non-stoichiometric salt and gold can be filled in cage
Belong to " cluster ".If be filled with the sodalite of non-stoichiometry alkali metal with the radiation exposure of high-energy, it is excited to produce
Photochromism.Sodalite hydrogen-sucking amount is higher than other zeolites, can theoretically reach the volume target of hydrogen storage material, while certainly
Body has anti-oxidant good with moisture resistance energy, stability well.Sodalite is used extensively with its unique cage structure and performance
Make photochromic material, hydrogen storage material, adsorbent etc., people increasingly pay close attention to the synthesis of sodalite.
Sodalite reserves are limited in nature, synthesized frequently with manual method.Traditional synthetic method is hydro-thermal method and molten
The hot method of agent.Hydro-thermal method is simple to operate, but the temperature needed for its synthesis is higher, energy consumption is larger, and pressure, temperature and equipment are wanted
Ask higher.The chemical reagent and organic additive of costliness are needed to use in solvent-thermal method, cost is higher.In addition, in experimentation
System composition, crystallization temperature and crystallization time etc. be also the factor for influenceing sodalite crystal morphology.(the chemistry of fuel such as Dou Tao
Report, 1996,24 (4)：It is in cube shape 372-374) to be reported in the sodalite obtained in glycol system, and using monoethanolamine as
The crystal morphology of the sodalite synthesized during decentralized medium is elliposoidal.Conclude its reason be in synthesis there is solvent effect,
Crystal Growth Mechanism has differences in different synthetic systems.(artificial lens journal, 2014,43 (2) such as He Qian：426-431) with
Sodium bentonite is raw material, and alkaline aqueous systems investigate the influence of crystallization temperature at ambient pressure.As a result it is 60 DEG C to show crystallization temperature
During with 70 DEG C, the sample of synthesis is the mixture of A types, P type zeolite and a small amount of sodalite composition；Crystallization temperature is 80 DEG C, sample
Middle P type zeolite disappears, and type A zeolite peak intensity substantially weakens, the enhancing of sodalite diffraction peak intensity；And during 100 DEG C of crystallization temperature, product
For the sodalite of single thing phase, its crystal mutually surrounds a central growth, forms the more uniform spheroidal aggravation of size, bulb diameter is about
0.5-0.8μm.(silicate journal, 2016,44 (8) such as Hu little Qiang：1200-1206) research shows crystallization time to synthetic product
There is a significant impact, crystallization generation at initial stage product be cube type A zeolite, during crystallization 10h, type A zeolite disappearance, the square sodium of formation
Stone is the aggregate that spindle crystal grain is agglomerated into, and average grain diameter is about 0.88 μm.(the Materials such as M.K.Naskar
Letters, 2011,65 (3)：436-438) report is respectively using Tween 80, span 20 and sorbester p17 as template, 90 DEG C of crystallization 10h,
The sodalite crystal morphology of synthesis, which distinguishes spherical in shape, column and petal-shaped, this petal-shaped pattern, can further increase zeolite
Surface area, be more beneficial for its suction-operated.To sum up narrate, existing synthetic method there is temperature is higher, energy consumption is larger,
The shortcomings of cost is higher.Therefore, it is necessary to find it is a kind of can reduce cost and product has the synthetic method of high surface area,
Laid the foundation in terms of so as to which absorption and hydrogen storage material can be better utilized in for sodalite.
The content of the invention
The present invention is for the shortcomings of temperature is higher, energy consumption is larger, cost is higher present in existing production, there is provided one kind is not
Use the preparation method of organic additive, at room temperature petal-shaped sodalite.The sodalite crystal of synthesis is in petal-shaped pattern, this
Pattern can further increase the surface area of zeolite, be more beneficial for its suction-operated.Synthetic method meets the development of Green Chemistry
It is required that there is certain economic benefit and social benefit.
The invention provides a kind of preparation method of the sodalite of petal-shaped at room temperature, comprise the following steps：
(1) sodium hydroxide and silicon source are weighed, adds deionized water, and heating stirring is completely dissolved raw material, and solution is made
A；
(2) silicon source is weighed, adds deionized water, and heating stirring is completely dissolved raw material, and solution B is made；
(3) solution A and solution B are well mixed, form silica-alumina gel mixture；
(4) above-mentioned silica-alumina gel mixture is subjected to crystallization at room temperature；
(5) reactant mixture after crystallization is washed after the completion of reacting, until wash solution pH to 8-9, by filter cake
12-36h is dried at 80-120 DEG C, you can obtain sodalite.
It is preferred that the room temperature is 25 DEG C.
It is preferred that filter cake is dried into 24h at 100 DEG C in step (5).
It is preferred that silicon source described in step (1) is one kind in sodium aluminate, aluminum sulfate, aluminium hydroxide.
It is preferred that silicon source described in step (2) is nine water sodium metasilicate.
It is preferred that hybrid mode is carried out by any one following mode in step (3)：
A. solution A is slowly added into solution B under agitation；
B. solution B is slowly added into solution A under agitation；
C. solution A and solution B are added dropwise in container jointly under agitation.
It is preferred that step (4) described crystallization time is 8-20h.
It is preferred that the crystallization time is 10h.
It is preferred that the silicon source dosage is in terms of Si, in terms of Al, the silicon source, silicon source and sodium hydroxide rub silicon source dosage
You are than being 1.0:0.4-2.0:2.8-16.0, the mol ratio of silicon source and deionized water in step (1) is 0.4-2.0:20-80,
The mol ratio of silicon source and deionized water in step (2) is 1.0:20-80.
Compared with prior art, the invention has the advantages that:
(1) reaction is carried out at room temperature, and mild condition is pollution-free without using organic additive, meets the hair of Green Chemistry
Exhibition requires；
(2) synthesis procedure is simple, and time-consuming short, cost is low；
(3) product good crystallinity, purity is high, and the sodalite of synthesis has petal-shaped pattern, is more beneficial for its absorption and makees
With suitable large-scale production.
Brief description of the drawings
Fig. 1 is X-ray diffraction (XRD) spectrogram for the sodalite powder that the embodiment of the present invention 1 obtains；
Fig. 2 is ESEM (SEM) photo for the sodalite powder that the embodiment of the present invention 1 obtains.
Embodiment
The embodiment of the present invention is described in detail below, it is to be understood that protection scope of the present invention is not
Limited by embodiment.Based on the embodiment in the present invention, those of ordinary skill in the art are not making creativeness
The every other embodiment obtained on the premise of work, belongs to the scope of protection of the invention.
Embodiment 1：
The preparation method of the sodalite of petal-shaped at room temperature of the present invention, comprises the following steps：
(1) 2.21g sodium aluminates are weighed and 4.56g sodium hydroxides are added in beaker, add 20.50g deionized waters, and add
Thermal agitation is completely dissolved raw material, and solution A is made；
(2) weigh the water sodium metasilicate of 5.68g nine to add in another beaker, add 25.12g deionized waters, and heating stirring
Raw material is completely dissolved, solution B is made；
(3) solution B is slowly added into solution A, and quickly stirred, made it well mixed, form silica-alumina gel mixture；
(4) silica-alumina gel mixture is transferred in the reactor of polytetrafluoroethylene (PTFE), be positioned in water-bath, set water-bath
Pot temperature is 25 DEG C, crystallization 10h；
(5) after the completion of reacting, reactor is taken out, the reactant mixture after crystallization is filtered, and with deionized water pair
Filter cake is washed, until wash solution pH to 8-9, dries 24h, you can obtain white sodalite powder by filter cake at 100 DEG C
Body.
Embodiment 2：
The preparation method of the sodalite of petal-shaped at room temperature of the present invention, comprises the following steps：
(1) weigh 3.76g aluminum sulfate and 4.78g sodium hydroxides are added in beaker, add 20.50g deionized waters, and add
Thermal agitation is completely dissolved raw material, and solution A is made；
(2) weigh the water sodium metasilicate of 5.39g nine to add in another beaker, add 20.85g deionized waters, and heating stirring
Raw material is completely dissolved, solution B is made；
(3) solution B is slowly added into solution A, and is quickly stirred, and is made it well mixed, is formed silica-alumina gel mixture；
(4) silica-alumina gel mixture is transferred in the reactor of polytetrafluoroethylene (PTFE), be positioned in water-bath, set water-bath
Pot temperature is 25 DEG C, crystallization 10h；
(5) after the completion of reacting, reactor is taken out, reactant mixture is filtered, and filter cake is carried out with deionized water
Washing, until wash solution pH to 8-9, filter cake dries 24h at 100 DEG C, you can obtains white sodalite powder.
Embodiment 3：
The preparation method of the sodalite of petal-shaped at room temperature of the present invention, comprises the following steps：
(1) 1.72g aluminium hydroxides are weighed and 4.78g sodium hydroxides are added in beaker, add 20.50g deionized waters, and
Heating stirring is completely dissolved raw material, and solution A is made；
(2) weigh the water sodium metasilicate of 5.68g nine to add in another beaker, add 24.68g deionized waters, and heating stirring
Raw material is completely dissolved, solution B is made；
(3) solution B is slowly added into solution A, and is quickly stirred, and is made it well mixed, is formed silica-alumina gel mixture；
(4) silica-alumina gel mixture is transferred in the reactor of polytetrafluoroethylene (PTFE), be positioned in water-bath, set water-bath
Pot temperature is 25 DEG C, crystallization 10h；
(5) after the completion of reacting, reactor is taken out, reactant mixture is filtered, and filter cake is carried out with deionized water
Washing, until wash solution pH to 8-9, filter cake dries 24h at 100 DEG C, you can obtains white sodalite powder.
Embodiment 4：
The preparation method of the sodalite of petal-shaped at room temperature of the present invention, comprises the following steps：
(1) 2.48g aluminium hydroxides are weighed and 5.56g sodium hydroxides are added in beaker, add 24.53g deionized waters, and
Heating stirring is completely dissolved raw material, and solution A is made；
(2) weigh the water sodium metasilicate of 5.68g nine to add in another beaker, add 22.12g deionized waters, and heating stirring
Raw material is completely dissolved, solution B is made；
(3) solution A is slowly added into solution B, and is quickly stirred, and is made it well mixed, is formed silica-alumina gel mixture；
(4) silica-alumina gel mixture is transferred in the reactor of polytetrafluoroethylene (PTFE), be positioned in water-bath, set water-bath
Pot temperature is 25 DEG C, crystallization 10h；
(5) after the completion of reacting, reactor is taken out, reactant mixture is filtered, and filter cake is carried out with deionized water
Washing, until wash solution pH to 8-9；Filter cake dries 24h at 100 DEG C, you can obtains white sodalite powder.
Embodiment 5：
The preparation method of the sodalite of petal-shaped at room temperature of the present invention, comprises the following steps：
(1) 2.18g sodium aluminates are weighed and 5.26g sodium hydroxides are added in beaker, add 21.50g deionized waters, and add
Thermal agitation is completely dissolved raw material, and solution A is made；
(2) weigh the water sodium metasilicate of 6.28g nine to add in another beaker, add 26.82g deionized waters, and heating stirring
Raw material is completely dissolved, solution B is made；
(3) solution A and solution B are added dropwise in beaker jointly, and quickly stirred, make it well mixed, formed sial and coagulate
Glue mixture；
(4) silica-alumina gel mixture is transferred in the reactor of polytetrafluoroethylene (PTFE), be positioned in water-bath, set water-bath
Pot temperature is 25 DEG C, crystallization 10h；
(5) after the completion of reacting, reactor is taken out, the reactant mixture after crystallization is filtered, and with deionized water pair
Filter cake is washed, until wash solution pH to 8-9, filter cake dries 24h at 100 DEG C, you can obtains white sodalite powder.
Embodiment 6：
The preparation method of the sodalite of petal-shaped at room temperature of the present invention, comprises the following steps：
(1) 2.18g sodium aluminates are weighed and 5.26g sodium hydroxides are added in beaker, add 21.50g deionized waters, and add
Thermal agitation is completely dissolved raw material, and solution A is made；
(2) weigh the water sodium metasilicate of 6.28g nine to add in another beaker, add 26.82g deionized waters, and heating stirring
Raw material is completely dissolved, solution B is made；
(3) solution A and solution B are added dropwise in beaker jointly, and quickly stirred, make it well mixed, formed sial and coagulate
Glue mixture；
(4) silica-alumina gel mixture is transferred in the reactor of polytetrafluoroethylene (PTFE), be positioned in water-bath, set water-bath
Pot temperature is 25 DEG C, crystallization 12h；
(5) after the completion of reacting, reactor is taken out, the reactant mixture after crystallization is filtered, and with deionized water pair
Filter cake is washed, until wash solution pH to 8-9, filter cake dries 36h at 80 DEG C, you can obtains white sodalite powder.
Embodiment 7：
The preparation method of the sodalite of petal-shaped at room temperature of the present invention, comprises the following steps：
(1) 2.48g aluminium hydroxides are weighed and 5.56g sodium hydroxides are added in beaker, add 24.53g deionized waters, and
Heating stirring is completely dissolved raw material, and solution A is made；
(2) weigh the water sodium metasilicate of 5.68g nine to add in another beaker, add 22.12g deionized waters, and heating stirring
Raw material is completely dissolved, solution B is made；
(3) solution A is slowly added into solution B, and is quickly stirred, and is made it well mixed, is formed silica-alumina gel mixture；
(4) silica-alumina gel mixture is transferred in the reactor of polytetrafluoroethylene (PTFE), be positioned in water-bath, set water-bath
Pot temperature is 25 DEG C, crystallization 16h；
(5) after the completion of reacting, reactor is taken out, reactant mixture is filtered, and filter cake is carried out with deionized water
Washing, until wash solution pH to 8-9, filter cake dries 12h at 120 DEG C, you can obtains white sodalite powder.
Wherein, the silica-alumina gel mixing chemical constituent silicon source amount described in step (3) is with SiO2Meter, silicon source amount is with Al2O3
Meter, alkali is with Na2O is counted, and silicon source in silica-alumina gel mixture, silicon source, the mol ratio of alkali and water are 1.0:0.2-1.0:1.4-8.0:
40-160。
Wherein, the sodalite powder obtained by embodiment 1 XRD as shown in figure 1, from figure 1 it appears that
13.8 °, 24.3 °, 31.4 °, 34.5 °, 42.6 ° appearance peaks and sodalite standard card correspond, it can be determined that produce
Thing is sodalite structure, and the sodalite belongs to typical cubic system, space group P-43n, space group number 218.Synthetic sample side
Sodium stone crystallinity is fine, almost high without impurity peaks, purity.
The surface sweeping electromicroscopic photograph of sodalite powder obtained by embodiment 1 is as shown in Fig. 2 figure it is seen that sodalite
Grain diameter has petal-shaped pattern at 0.3-0.6 μm, and this can further increase the surface area of zeolite, be more beneficial for inhaling
Attached effect.
Although preferred embodiments of the present invention have been described, but those skilled in the art once know basic creation
Property concept, then can make other change and modification to these embodiments.So appended claims be intended to be construed to include it is excellent
Select embodiment and fall into having altered and changing for the scope of the invention.
Obviously, those skilled in the art can carry out the essence of various changes and modification without departing from the present invention to the present invention
God and scope.So, if these modifications and variations of the present invention belong to the scope of the claims in the present invention and its equivalent technologies
Within, then the present invention is also intended to comprising including these changes and modification.
Claims (9)
1. a kind of preparation method of the sodalite of petal-shaped at room temperature, it is characterised in that comprise the following steps：
(1) sodium hydroxide and silicon source are weighed, adds deionized water, and heating stirring is completely dissolved raw material, and solution A is made；
(2) silicon source is weighed, adds deionized water, and heating stirring is completely dissolved raw material, and solution B is made；
(3) solution A and solution B are well mixed, form silica-alumina gel mixture；
(4) above-mentioned silica-alumina gel mixture is subjected to crystallization at room temperature；
(5) reactant mixture after crystallization is washed after the completion of reacting, until wash solution pH to 8-9, by filter cake in 80-
12-36h is dried at 120 DEG C, you can obtain sodalite.
2. the preparation method of petal-shaped sodalite at room temperature as claimed in claim 1, it is characterised in that the room temperature is 25
℃。
3. the preparation method of petal-shaped sodalite at room temperature as claimed in claim 1, it is characterised in that will filter in step (5)
Cake dries 24h at 100 DEG C.
4. the preparation method of petal-shaped sodalite at room temperature as claimed in claim 1, it is characterised in that described in step (1)
Silicon source is one kind in sodium aluminate, aluminum sulfate, aluminium hydroxide.
5. the preparation method of petal-shaped sodalite at room temperature as claimed in claim 1, it is characterised in that described in step (2)
Silicon source is nine water sodium metasilicate.
6. the preparation method of petal-shaped sodalite at room temperature as claimed in claim 1, it is characterised in that mixed in step (3)
Mode is carried out by any one following mode：
A. solution A is slowly added into solution B under agitation；
B. solution B is slowly added into solution A under agitation；
C. solution A and solution B are added dropwise in container jointly under agitation.
7. the preparation method of petal-shaped sodalite at room temperature as claimed in claim 1, it is characterised in that step (4) described crystalline substance
The change time is 8-20h.
8. the preparation method of petal-shaped sodalite at room temperature as claimed in claim 7, it is characterised in that the crystallization time is
10h。
9. the preparation method of the sodalite of petal-shaped at room temperature as described in claim 1-8 is any, it is characterised in that the silicon source
Dosage is in terms of Si, and for silicon source dosage in terms of Al, the mol ratio of the silicon source, silicon source and sodium hydroxide is 1.0:0.4-2.0:2.8-
16.0, the mol ratio of silicon source and deionized water in step (1) is 0.4-2.0:20-80, silicon source and deionization in step (2)
The mol ratio of water is 1.0:20-80.
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| CN109019621A (en) * | 2018-10-12 | 2018-12-18 | 许昌学院 | The preparation method of nanometer sodalite under a kind of low temperature |
| CN112850739A (en) * | 2021-03-12 | 2021-05-28 | 许昌学院 | Large-grain LTJ zeolite and preparation method thereof |
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