CN108101072A - The preparation method of micro--meso-hole structure analcime - Google Patents
The preparation method of micro--meso-hole structure analcime Download PDFInfo
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- CN108101072A CN108101072A CN201810056779.7A CN201810056779A CN108101072A CN 108101072 A CN108101072 A CN 108101072A CN 201810056779 A CN201810056779 A CN 201810056779A CN 108101072 A CN108101072 A CN 108101072A
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- C01B39/00—Compounds having molecular sieve and base-exchange properties, e.g. crystalline zeolites; Their preparation; After-treatment, e.g. ion-exchange or dealumination
- 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
- C01B39/04—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 using at least one organic template directing agent, e.g. an ionic quaternary ammonium compound or an aminated compound
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- C01P2006/16—Pore diameter
- C01P2006/17—Pore diameter distribution
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Abstract
The invention discloses a kind of preparation methods of micro- meso-hole structure analcime, with white carbon, sodium metaaluminate, sodium hydroxide is raw material, and asymmetric gemini quaternary ammonium salt cationic surfactant is directed agents, and solvent, detergent are done with deionized water, in a kettle crystallization, through quenching, separation, washing, vacuum drying, high-temperature roasting, multi-stage porous analcime is made, to improve the purity of multi-stage porous analcime, expands the application range of multi-stage porous analcime.This preparation method technique is advanced, and data are accurately full and accurate, and product is white powder, and product purity is the advanced method for preparing multi-stage porous analcime up to 99.8%.
Description
Technical field
The invention belongs to technical field of inorganic material, are specially a kind of preparation method of micro--meso-hole structure analcime.
Background technology
Analcime is with ANA topological structures, the micro porous molecular sieve in microporous three-dimensional duct.It is aluminosilicate zeolites synthesis
The common byproduct of system, but pure phase can also be artificial synthesized by way of hydro-thermal method or without organic formwork.Research shows
Analcime Development volue in terms of ion exchange, wastewater treatment and catalytic applications is huge, however its aperture is smaller, and duct is crisscross multiple
Miscellaneous, macromolecule reactant is larger in duct inside diffusional resistance, the mass transfer being unfavorable in reaction, easily leads to carbon distribution inactivation, makes
It obtains single micropore analcime to be restricted in practical applications, therefore the preparation of multi-stage porous analcime receives significant attention.
The preparation of multi-stage pore zeolite molecular sieve mainly has post treatment method, two major class of template.Post treatment method is typically to pass through
The methods of alkali, acid treatment or high-temperature water vapor are handled removes framework of molecular sieve element, but the method is with framework of molecular sieve structure
It destroys what is realized for cost, therefore is restricted in practice.Template is divided into two kinds of hard template method and soft template method, is sial
Species prepare multistage porous molecular sieve by template self assembly, however the templates such as nano carbon particle, mesoporous carbon in hard template method
Preparation be related to the carbonisation of high energy consumption, and process is complicated, is unfavorable for large-scale production.Soft template method is a kind of efficiently system
The method of standby multistage porous molecular sieve.
In recent years, in many soft templates, the use of gemini quaternary ammonium salt cationic surfactant receives significant attention, because
Its special construction, good degradability play effective mesoporous guiding role in the constructing of multistage porous molecular sieve.It is wherein not right
Claim the use of gemini quaternary ammonium salt cationic surfactant that can serve as the effect of difunctional directed agents, therefore this technology is for side
The characteristics of zeolite, using asymmetric gemini quaternary ammonium salt cationic surfactant, prepares multi-stage porous analcime.In existing synthesis side
In method, reaction condition requirement is high, raw material availability is low, without synthesising law, this technology is still in scientific research.
The content of the invention
The purpose of the present invention is being directed to the situation of background technology and deficiency, using white carbon, sodium metaaluminate, sodium hydroxide as original
Material, asymmetric gemini quaternary ammonium salt cationic surfactant are directed agents, solvent, detergent are done with deionized water, in reaction kettle
Middle crystallization, through quenching, separation, washing, vacuum drying, high-temperature roasting, multi-stage porous analcime is made, to improve multi-stage porous side
The purity of zeolite expands the application range of multi-stage porous analcime.
The present invention adopts the following technical scheme that realization：
A kind of preparation method of micro--meso-hole structure analcime, includes the following steps：
（1）Chemical substance material
The chemical substance material used is：Sodium metaaluminate, sodium hydroxide, deionized water, white carbon, asymmetric gemini quaternary ammonium salt sun
It is as follows to prepare dosage for ionic surface active agent：
Sodium metaaluminate：NaAlO2 0.630g
Sodium hydroxide：NaOH 0.480g
White carbon：SiO2 6.000g
Asymmetric gemini quaternary ammonium salt cationic surfactant：C33H72N2Br2 12.340g
Deionized water：H2O 12.25mL
C33H72N2Br2：Asymmetric gemini quaternary ammonium salt cationic surfactant, unique molecular structural formula are as follows：
（2）Configure sodium hydroxide solution
Sodium hydroxide 0.48g, deionized water 3mL are weighed, adds in beaker, is stirred with blender, mixing time 30min, is stirred
Afterwards into the sodium hydrate aqueous solution of 4mol/L；
（3）Prepare multi-stage porous analcime
1. configure multi-stage porous analcime mixed solution
Deionized water 9.25mL, sodium hydroxide solution 1.75mL are measured, weighs sodium metaaluminate 0.63g, asymmetric gemini quaternary ammonium salt
Cationic surfactant 12.34g, white carbon 6g, are added in polytetrafluoroethylcontainer container, using heat collecting type temperature constant magnetic stirring
Device heated at constant temperature stirs 1h, 25 DEG C of heating temperature, and agitation revolution 200r/min makes mixture fully dissolve, and forms white gels
Solution；
2. constant temperature is stood
The polytetrafluoroethylcontainer container for filling mixed solution is placed on electric heater, 50 DEG C of electric heater heating temperature, heating time is
40h；
3. heating crystallization
The polytetrafluoroethylcontainer container for filling mixed solution is placed in reaction kettle, and it is closed, reaction kettle is then put into insulating box
Middle heating, 140 DEG C of heating temperature, constant temperature, static crystallization reaction 96h；
4. quenching
Heating crystallization after reaction, closes insulating box, reaction kettle is placed in quenching slot, quick in 10 DEG C of deionized water
It is cooled to 20 DEG C；
5. deionized water dilution centrifuges
Reaction kettle is opened after cooling, the mixing turbid in polytetrafluoroethylcontainer container is poured into beaker, adds in deionized water
600mL stirs 30min on magnetic stirring apparatus, and turbid is mixed into dilution；
Dilution mixing turbid is placed in centrifugal separating tube, is centrifuged, revolution 5000r/min is centrifuged, during separation
Between 15min, solid sediment, abandoning supernatant are retained after centrifugation；
6. cleaning is scattered, centrifuges
Solid sediment after separation is placed in beaker, deionized water 500mL is added in, is subsequently placed in ultrasonic wave separating apparatus,
Carry out ultrasonic cleaning and dispersion, ultrasonic frequency 40Hz, jitter time 30min；
Then dispersion soln is placed in the centrifugal separating tube of centrifuge, be centrifuged, centrifuge revolution 5000r/
Min, disengaging time 15min retain solid sediment, abandoning supernatant after centrifugation；
Cleaning is scattered, and centrifugation repeats 3 times；
7. it is dried in vacuo
Solid sediment is placed in quartz container, is subsequently placed in drying in vacuum drying chamber, drying temperature is 100 DEG C, vacuum
2Pa, drying time 12h are spent, powder product is obtained after dry；
8. vacuum baking
The roasting of multi-stage porous analcime carries out in vacuum sintering furnace, heat, vacuumize, argon gas protection, outer water cycle
Cooling is lower to be completed；
A, solid sediment is placed in quartz container, be subsequently placed on the workbench in vacuum sintering furnace；
B, vacuum sintering furnace is closed, opens vacuum pump, extracts furnace air, pressure in stove is made to reach 5Pa；
C, argon bottle, tunger tube are opened, argon gas is passed through into stove, makes in stove invariablenes pressure of liquid in 0.9MPa；
D, outer water circulating cooling pipe is opened, carries out outer water circulating cooling；
E, opening resistor heater, 550 DEG C of heating temperature, is roasted, heating roasting time 360min；
F, cool down, stop heating after roasting, the product in quartz container cools to 25 DEG C with the furnace；
G, multi-stage porous analcime is obtained after cooling down；
（4）, grinding, sieving
Powder product after roasting is ground, is then sieved with 200 mesh screens；It is ground up, sieved and is repeated, obtain final product multistage
Hole analcime.
In the method for the present invention in the structure of asymmetric gemini quaternary ammonium salt cationic surfactant used, wrapped in connection chain
Containing 3 carbon atoms, when the connection chain carbon number of gemini quaternary ammonium salt cationic surfactant is 6 and is following, in water
Under the conditions of thermal synthesis, it may occur that Huffman eliminates the reaction reset, can shape after connection chain fracture just because of this design feature
Into an ammonium salt containing short hydrophobic chain and the ammonium salt of a long hydrophobic chain, in the crystallization building-up process of molecular sieve, send out respectively
Wave the effect of micropore template agent and mesoporous directed agents and occupy-place function.
Difficult situation is prepared the present invention be directed to multi-stage porous analcime, with white carbon, sodium metaaluminate, sodium hydroxide, not right
Gemini quaternary ammonium salt cationic surfactant is referred to as raw material, and solvent, detergent, formulated solution, reaction kettle are done with deionized water
Crystallization, heated at constant temperature, quenching, cleaning is scattered, centrifuge, washing, vacuum drying, high-temperature vacuum are roasted, be ground up, sieved,
Final product multi-stage porous analcime is made, this preparation method technique is advanced, and data are accurately full and accurate, and product is white powder, and product is pure
Degree is the advanced method for preparing multi-stage porous analcime up to 99.8%.
Present invention design is reasonable, has the application of good market and promotional value.
Description of the drawings
Fig. 1 shows multi-stage porous analcime X-ray diffraction intensity spectrograms.
Fig. 2 represents multi-stage porous analcime shape appearance figure.
Fig. 3 represents multi-stage porous analcime nitrogen adsorption desorption isotherm.
Fig. 4 represents the pore size distribution curve figure that multi-stage porous analcime is calculated according to NLDFT models.
Specific embodiment
Specific embodiments of the present invention are described in detail below in conjunction with the accompanying drawings.
A kind of preparation method of multi-stage porous analcime, the chemical substance material used are：Sodium metaaluminate, sodium hydroxide are gone
Ionized water, white carbon, asymmetric gemini quaternary ammonium salt cationic surfactant, it is as follows to prepare dosage：With gram, milliliter, centimetre3
For measurement unit
Sodium metaaluminate：NaAlO2 0.630g±0.001g
Sodium hydroxide：NaOH 0.480g ±0.001g
White carbon：SiO2 6.000g±0.001g
Asymmetric gemini quaternary ammonium salt cationic surfactant：C33H72N2Br2 12.340g±0.001g
Deionized water：H2O 12.25mL±0.01mL
Argon gas：Ar 100000cm3±100cm3
C33H72N2Br2：Asymmetric gemini quaternary ammonium salt cationic surfactant, unique molecular structural formula are as follows：
Specific preparation method is as follows
（1）, selected chemical substance material
The chemical substance material that uses of preparation to be carried out selected, and carry out quality purity control：
Sodium metaaluminate：Solid state 99.9%
Sodium hydroxide：Solid state 99.9%
White carbon：Solid state 97%
Deionized water：Liquid liquid 99.9%
Asymmetric gemini quaternary ammonium salt cationic surfactant：Liquid liquid 98%
Argon gas：Gaseous atmospheres 99.9%
（2）, configuration sodium hydroxide solution
Sodium hydroxide 0.48g ± 0.001g, deionized water 3mL ± 0.01mL are weighed, is added in beaker, is stirred, stirred with blender
Time 30min is mixed, into the sodium hydrate aqueous solution of 4mol/L after stirring；
（3）, prepare multi-stage porous analcime
Configure multi-stage porous analcime mixed solution
Measure deionized water 9.25mL ± 0.01mL, sodium hydroxide solution 1.75mL ± 0.01mL, weigh sodium metaaluminate 0.63g ±
0.001g, asymmetric gemini quaternary ammonium salt cationic surfactant 12.34g ± 0.001g, white carbon 6g ± 0.001g, are added to
In polytetrafluoroethylcontainer container, 1h is stirred using heat collecting type constant temperature blender with magnetic force heated at constant temperature, 25 DEG C ± 1 DEG C of heating temperature is stirred
Revolution 200r/min is mixed, mixture is made fully to dissolve, forms white gels solution；
Constant temperature is stood
The polytetrafluoroethylcontainer container for filling mixed solution is placed on electric heater, 50 DEG C ± 1 DEG C of electric heater heating temperature, during heating
Between be 40h；
Heating crystallization
The polytetrafluoroethylcontainer container for filling mixed solution is placed in reaction kettle, and it is closed, reaction kettle is then put into insulating box
Middle heating, 140 DEG C ± 2 DEG C of heating temperature, constant temperature, static crystallization reaction 96h；
Quenching
Heating crystallization after reaction, closes insulating box, reaction kettle is placed in quenching slot, quick in 10 DEG C of deionized water
It is cooled to 20 DEG C；
Deionized water dilution centrifuges
Reaction kettle is opened after cooling, the mixing turbid in polytetrafluoroethylcontainer container is poured into beaker, adds in deionized water
600mL stirs 30min on magnetic stirring apparatus, and turbid is mixed into dilution；
Dilution mixing turbid is placed in centrifugal separating tube, is centrifuged, revolution 5000r/min is centrifuged, during separation
Between 15min, solid sediment, abandoning supernatant are retained after centrifugation；
Cleaning is scattered, centrifuges
Solid sediment after separation is placed in beaker, deionized water 500mL is added in, is subsequently placed in ultrasonic wave separating apparatus,
Carry out ultrasonic cleaning and dispersion, ultrasonic frequency 40Hz, jitter time 30min；
Then dispersion soln is placed in the centrifugal separating tube of centrifuge, be centrifuged, centrifuge revolution 5000r/
Min, disengaging time 15min retain solid sediment, abandoning supernatant after centrifugation；
Cleaning is scattered, and centrifugation repeats 3 times；
Vacuum drying
Solid sediment is placed in quartz container, is subsequently placed in drying in vacuum drying chamber, drying temperature is 100 DEG C, vacuum
2Pa, drying time 12h are spent, powder product is obtained after dry；
Vacuum baking
The roasting of multi-stage porous analcime carries out in vacuum sintering furnace, heat, vacuumize, argon gas protection, outer water cycle
Cooling is lower to be completed；
A, solid sediment is placed in quartz container, be subsequently placed on the workbench in vacuum sintering furnace；
B, vacuum sintering furnace is closed, opens vacuum pump, extracts furnace air, pressure in stove is made to reach 5Pa；
C, argon bottle, tunger tube are opened, argon gas is passed through into stove, makes in stove invariablenes pressure of liquid in 0.9MPa；
D, outer water circulating cooling pipe is opened, carries out outer water circulating cooling；
E, opening resistor heater, 550 DEG C ± 2 DEG C of heating temperature, is roasted, heating roasting time 360min；
F, cool down, stop heating after roasting, the product in quartz container cools to 25 DEG C with the furnace；
G, multi-stage porous analcime is obtained after cooling down；
（4）, grinding, sieving
Powder product agate mortar, pestle after roasting is ground, is then sieved with 200 mesh screens；
It is ground up, sieved and is repeated, obtain final product multi-stage porous analcime；
（5）, detection, analyze, characterization
The multi-stage porous analcime crystal structure of preparation, pattern, color and luster, Chemical Physics performance are detected, analyzed, characterization；
A, crystal object phase and crystallinity analysis are carried out with X-ray diffractometer
Fig. 1 is multi-stage porous analcime X-ray diffraction intensity spectrogram, and as figure shows, the multi-stage porous analcime of synthesis shows that it is special
Some characteristic diffraction peaks, peak type is sharp and without other miscellaneous peaks, and diffracted intensity is higher, while small angular region has apparent diffraction maximum, card
Bright synthesized multi-stage porous analcime contains abundant orderly secondary pore passage structure.
B, crystalline product morphology analysis is carried out with scanning electron microscope
Fig. 2 is multi-stage porous analcime shape appearance figure, and as figure shows, the multi-stage porous analcime rough surface explanation of synthesis has largely
Meso-hole structure, while rich in abundant accumulation secondary pore structure.
C, Fig. 3 is multistage analcime nitrogen adsorption desorption curve, as shown in the figure, by N2Adsorption/desorption curve can be seen that
0.4<P/P0<1.0, there is apparent desorption hysteresis loop, this is because mesoporous presence, has occurred capillary condensation and show
As illustrating that there are substantial amounts of meso-hole structures in synthesized multi-stage porous analcime.
D, Fig. 4 is multi-stage porous analcime pore size distribution curve, the multistage of synthesis it can be seen from the pore volume distribution curve of aperture
Hole analcime molecular sieve has apparent micropore size to be distributed in 0 ~ 1nm sections, and point of a mesoporous pore size occurs again in 1 ~ 10nm
Cloth situation, it was demonstrated that there are transgranular mesoporous, and pore-size distribution is concentrated, and illustrates degree of order height.
Conclusion：The multi-stage porous analcime of preparation is white powder, and product purity is up to 99.8%；
（6）, product storage
The multi-stage porous analcime white powder of preparation is put into the glass container of amber transparent, sealing is protected from light storage, need are moisture-proof,
Sun-proof, anti-acid-alkali salt class corrodes, 20 DEG C of storage temperature, relative humidity 10%.
It should be noted last that the above embodiments are merely illustrative of the technical solutions of the present invention and it is unrestricted, although ginseng
It is described in detail according to the embodiment of the present invention, it will be understood by those of ordinary skill in the art that, to technical scheme
It is modified or replaced equivalently, without departure from the spirit and scope of technical scheme, should all cover the present invention's
In claims.
Claims (1)
1. a kind of preparation method of micro--meso-hole structure analcime, it is characterised in that：Include the following steps：
（1）, chemical substance material
The chemical substance material used is：Sodium metaaluminate, sodium hydroxide, deionized water, white carbon, asymmetric gemini quaternary ammonium salt sun
It is as follows to prepare dosage for ionic surface active agent：
Sodium metaaluminate：NaAlO2 0.630g
Sodium hydroxide：NaOH 0.480g
White carbon：SiO2 6.000g
Asymmetric gemini quaternary ammonium salt cationic surfactant：C33H72N2Br2 12.340g
Deionized water：H2O 12.25mL
C33H72N2Br2：Asymmetric gemini quaternary ammonium salt cationic surfactant, unique molecular structural formula are as follows：
Explanation:Explanation: F:It is military build 2018 Nian Yi Yue science and engineering great science and engineering king's poem Yaos of Yun it is micro--the Zhi Beifangfa surfactants .jpg of meso-hole structure analcime
（2）, configuration sodium hydroxide solution
Sodium hydroxide 0.48g, deionized water 3mL are weighed, adds in beaker, is stirred with blender, mixing time 30min, is stirred
Afterwards into the sodium hydrate aqueous solution of 4mol/L；
（3）, prepare multi-stage porous analcime
1. configure multi-stage porous analcime mixed solution
Deionized water 9.25mL, sodium hydroxide solution 1.75mL are measured, weighs sodium metaaluminate 0.63g, asymmetric gemini quaternary ammonium salt
Cationic surfactant 12.34g, white carbon 6g, are added in polytetrafluoroethylcontainer container, using heat collecting type temperature constant magnetic stirring
Device heated at constant temperature stirs 1h, 25 DEG C of heating temperature, and agitation revolution 200r/min makes mixture fully dissolve, and forms white gels
Solution；
2. constant temperature is stood
The polytetrafluoroethylcontainer container for filling mixed solution is placed on electric heater, 50 DEG C of electric heater heating temperature, heating time is
40h；
3. heating crystallization
The polytetrafluoroethylcontainer container for filling mixed solution is placed in reaction kettle, and it is closed, reaction kettle is then put into insulating box
Middle heating, 140 DEG C of heating temperature, constant temperature, static crystallization reaction 96h；
4. quenching
Heating crystallization after reaction, closes insulating box, reaction kettle is placed in quenching slot, quick in 10 DEG C of deionized water
It is cooled to 20 DEG C；
5. deionized water dilution centrifuges
Reaction kettle is opened after cooling, the mixing turbid in polytetrafluoroethylcontainer container is poured into beaker, adds in deionized water
600mL stirs 30min on magnetic stirring apparatus, and turbid is mixed into dilution；
Dilution mixing turbid is placed in centrifugal separating tube, is centrifuged, revolution 5000r/min is centrifuged, during separation
Between 15min, solid sediment, abandoning supernatant are retained after centrifugation；
6. cleaning is scattered, centrifuges
Solid sediment after separation is placed in beaker, deionized water 500mL is added in, is subsequently placed in ultrasonic wave separating apparatus,
Carry out ultrasonic cleaning and dispersion, ultrasonic frequency 40Hz, jitter time 30min；
Then dispersion soln is placed in the centrifugal separating tube of centrifuge, be centrifuged, centrifuge revolution 5000r/
Min, disengaging time 15min retain solid sediment, abandoning supernatant after centrifugation；
Cleaning is scattered, and centrifugation repeats 3 times；
7. it is dried in vacuo
Solid sediment is placed in quartz container, is subsequently placed in drying in vacuum drying chamber, drying temperature is 100 DEG C, vacuum
2Pa, drying time 12h are spent, powder product is obtained after dry；
8. vacuum baking
The roasting of multi-stage porous analcime carries out in vacuum sintering furnace, heat, vacuumize, argon gas protection, outer water cycle
Cooling is lower to be completed；
A, solid sediment is placed in quartz container, be subsequently placed on the workbench in vacuum sintering furnace；
B, vacuum sintering furnace is closed, opens vacuum pump, extracts furnace air, pressure in stove is made to reach 5Pa；
C, argon bottle, tunger tube are opened, argon gas is passed through into stove, makes in stove invariablenes pressure of liquid in 0.9MPa；
D, outer water circulating cooling pipe is opened, carries out outer water circulating cooling；
E, opening resistor heater, 550 DEG C of heating temperature, is roasted, heating roasting time 360min；
F, cool down, stop heating after roasting, the product in quartz container cools to 25 DEG C with the furnace；
G, multi-stage porous analcime is obtained after cooling down；
（4）, grinding, sieving
Powder product after roasting is ground, is then sieved with 200 mesh screens；It is ground up, sieved and is repeated, obtain final product multistage
Hole analcime.
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| CN112980586A (en) * | 2021-04-08 | 2021-06-18 | 武汉黄鹤楼香精香料有限公司 | Purification method of pearl blasting essential oil |
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| CN105983440A (en) * | 2015-04-02 | 2016-10-05 | 大连海鑫化工有限公司 | Composite nanometer thin layer molecular sieve and preparation method and application |
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|---|---|---|---|---|
| CN103626202A (en) * | 2012-08-21 | 2014-03-12 | 巩雁军 | Method for preparing catalyst used for methanol/dimethyl ether high selectivity propylene preparation |
| CN104211085A (en) * | 2013-06-05 | 2014-12-17 | 中国石油天然气股份有限公司 | Core-shell type ZSM-5 molecular sieve and preparation and application thereof |
| CN104722273A (en) * | 2013-12-18 | 2015-06-24 | 江南大学 | Method for preparing organic modified clay for removing organic pollutants from wastewater |
| CN105983440A (en) * | 2015-04-02 | 2016-10-05 | 大连海鑫化工有限公司 | Composite nanometer thin layer molecular sieve and preparation method and application |
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| CN112980586A (en) * | 2021-04-08 | 2021-06-18 | 武汉黄鹤楼香精香料有限公司 | Purification method of pearl blasting essential oil |
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