CN108101072B - Preparation method of analcite with micro-mesoporous structure - Google Patents
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Abstract
The invention discloses a preparation method of analcime with a micro-mesoporous structure, which takes white carbon black, sodium metaaluminate and sodium hydroxide as raw materials, an asymmetric gemini quaternary ammonium salt cationic surfactant as a guiding agent, deionized water as a solvent and a detergent, and prepares the hierarchical pore analcime in a reaction kettle through crystallization reaction, quenching, separation, washing, vacuum drying and high-temperature roasting, so as to improve the purity of the hierarchical pore analcime and expand the application range of the hierarchical pore analcime. The preparation method has the advantages of advanced process, precise and precise data, white powder of the product, and high purity of the product up to 99.8%, and is an advanced method for preparing the multi-stage pore zeolite.
Description
Technical Field
The invention belongs to the technical field of inorganic materials, and particularly relates to a preparation method of analcime with a micro-mesoporous structure.
Background
Analcite is a microporous molecular sieve with an ANA topology structure and microporous three-dimensional pore channels. It is a common byproduct of aluminosilicate zeolite synthesis systems, but pure phases can also be synthesized artificially by hydrothermal methods or in a manner free of organic templates. Research shows that the analcime has great development value in the aspects of ion exchange, wastewater treatment and catalytic application, but the analcime has small pore diameter, complicated pore channels and large diffusion resistance of macromolecular reactants in the pore channels, is not beneficial to material transmission in reaction, is easy to cause carbon deposition inactivation, so that the single microporous analcime is limited in practical application, and the preparation of the multi-level porous analcime is widely concerned.
The preparation of the hierarchical pore zeolite molecular sieve mainly comprises two major types of post-treatment method and template method. The post-treatment method is usually to remove the molecular sieve framework elements by alkali, acid treatment or high-temperature steam treatment, but the method is realized at the cost of the structural damage of the molecular sieve framework, so that the method is limited in practice. The template method is divided into a hard template method and a soft template method, the hierarchical pore molecular sieve is prepared by self-assembly of a template agent by silicon-aluminum species, however, the preparation of the template agents such as nano carbon particles, mesoporous carbon and the like in the hard template method relates to a carbonization process with high energy consumption, and the process is complex and is not beneficial to large-scale production. The soft template method is a method for efficiently preparing the hierarchical pore molecular sieve.
In recent years, in many soft templates, the use of gemini quaternary ammonium salt cationic surfactants has attracted much attention, and due to their special structure and good degradability, they exert an effective mesoporous guiding effect in the construction of hierarchical pore molecular sieves. The use of the asymmetric gemini quaternary ammonium salt cationic surfactant can serve as a bifunctional guiding agent, so that the technology is used for preparing the hierarchical porous analcime by utilizing the asymmetric gemini quaternary ammonium salt cationic surfactant according to the characteristics of the analcime. In the existing synthesis method, the reaction condition requirement is high, the utilization rate of raw materials is low, and no synthesis rule exists, so the technology is still in scientific research.
Disclosure of Invention
The invention aims to solve the problems and defects of the background art, and the method comprises the steps of taking white carbon black, sodium metaaluminate and sodium hydroxide as raw materials, taking an asymmetric gemini quaternary ammonium salt cationic surfactant as a guiding agent, taking deionized water as a solvent and a detergent, carrying out crystallization reaction in a reaction kettle, quenching, separating, washing, vacuum drying and high-temperature roasting to prepare the hierarchical pore analcime, so that the purity of the hierarchical pore analcime is improved, and the application range of the hierarchical pore analcime is expanded.
The invention is realized by adopting the following technical scheme:
a preparation method of analcime with a micro-mesoporous structure comprises the following steps:
(1) chemical material
The chemical materials used were: sodium metaaluminate, sodium hydroxide, deionized water, white carbon black and asymmetric gemini quaternary ammonium salt cationic surfactant, wherein the preparation dosage is as follows:
sodium metaaluminate: NaAlO20.630g
Sodium hydroxide: NaOH 0.480g
White carbon black: SiO 226.000g
Asymmetric gemini quaternary ammonium salt cationic surfactant: c33H72N2Br212.340g
Deionized water: h2O 12.25mL
C33H72N2Br2: asymmetric gemini quaternary ammonium salt cation tableThe surfactant has the following unique molecular structural formula:
(2) preparing sodium hydroxide solution
Weighing 0.48g of sodium hydroxide and 3m L g of deionized water, adding the sodium hydroxide and the deionized water into a beaker, stirring the mixture by using a stirrer for 30min, and stirring the mixture to obtain a 4 mol/L sodium hydroxide aqueous solution;
(3) preparation of hierarchical pore analcite
① preparing multi-stage pore analcime mixed solution
Weighing 9.25m L deionized water and 1.75m L sodium hydroxide solution, weighing 0.63g sodium metaaluminate, 12.34g asymmetric gemini quaternary ammonium salt cationic surfactant and 6g white carbon black, adding into a polytetrafluoroethylene container, heating and stirring for 1h at a constant temperature of 25 ℃ by using a heat collection type constant temperature magnetic stirrer, wherein the stirring revolution is 200r/min, so that the mixture is fully dissolved to form a white gel solution;
② standing at constant temperature
Placing the polytetrafluoroethylene container containing the mixed solution on an electric heater, wherein the electric heater is heated at 50 ℃ for 40 h;
③ heat crystallization
Placing the polytetrafluoroethylene container containing the mixed solution into a reaction kettle, sealing, then placing the reaction kettle into a thermostat, heating to 140 ℃, keeping the temperature constant, and carrying out static crystallization reaction for 96 hours;
④ quenching
After the heating crystallization reaction is finished, closing the constant temperature box, placing the reaction kettle in a quenching tank, and rapidly cooling the reaction kettle to 20 ℃ in deionized water at 10 ℃;
⑤ diluting with deionized water, and centrifuging
Opening the reaction kettle after cooling, pouring the mixed turbid liquid in the polytetrafluoroethylene container into a beaker, adding 600m L of deionized water, and stirring on a magnetic stirrer for 30min to obtain diluted mixed turbid liquid;
placing the diluted mixed turbid liquid in a centrifugal separation tube, performing centrifugal separation, wherein the centrifugal separation rotation number is 5000r/min, the separation time is 15min, retaining solid precipitate after centrifugal separation, and discarding supernatant;
⑥ washing, dispersing, and centrifuging
Placing the separated solid precipitate in a beaker, adding deionized water of 500m L, and then placing in an ultrasonic disperser for ultrasonic cleaning and dispersing, wherein the ultrasonic frequency is 40Hz, and the dispersing time is 30 min;
then placing the dispersion solution into a centrifugal separation tube of a centrifugal machine, carrying out centrifugal separation, wherein the centrifugal separation revolution number is 5000r/min, the separation time is 15min, retaining solid precipitate after centrifugal separation, and discarding supernatant;
cleaning, dispersing, and repeatedly performing centrifugal separation for 3 times;
⑦ vacuum drying
Putting the solid precipitate into a quartz container, then putting the quartz container into a vacuum drying oven for drying at the drying temperature of 100 ℃, the vacuum degree of 2Pa for 12h, and drying to obtain a powder product;
⑧ vacuum roasting
The roasting of the hierarchical pore analcite is carried out in a vacuum sintering furnace under the conditions of heating, vacuumizing, argon protection and external water circulation cooling;
A. putting the solid precipitate into a quartz container, and then putting the quartz container on a workbench in a vacuum sintering furnace;
B. closing the vacuum sintering furnace, starting a vacuum pump, and extracting air in the furnace to enable the pressure in the furnace to reach 5 Pa;
C. opening an argon bottle and an argon pipe, and introducing argon into the furnace to ensure that the pressure in the furnace is constant at 0.9 MPa;
D. opening an external water circulation cooling pipe to carry out external water circulation cooling;
E. starting a resistance heater, heating to 550 ℃, and roasting for 360 min;
F. cooling, stopping heating after roasting, and cooling a product in a quartz container to 25 ℃ along with a furnace;
G. cooling to obtain multi-grade pore zeolite;
(4) grinding and sieving
Grinding the roasted powder product, and then sieving by using a 200-mesh sieve; grinding and sieving are carried out repeatedly to obtain the final product of the multi-grade pore zeolite.
In the structure of the asymmetric gemini quaternary ammonium salt cationic surfactant used in the method, a connecting chain contains 3 carbon atoms, when the carbon atom number of the connecting chain of the gemini quaternary ammonium salt cationic surfactant is 6 or less, Hofmann reaction for eliminating rearrangement can occur under the condition of hydrothermal synthesis, and due to the structural characteristics, an ammonium salt containing a short hydrophobic chain and an ammonium salt containing a long hydrophobic chain can be formed after the connecting chain is broken, and the functions of a micropore template agent, a mesopore guiding agent and an occupation function are respectively exerted in the crystallization synthesis process of a molecular sieve.
The invention is directed against the difficult situation of preparation of zeolite of hierarchical pore side, regard white carbon black, sodium metaaluminate, sodium hydroxide, asymmetric gemini quaternary ammonium salt cationic surfactant as raw materials, regard deionized water as solvent, detergent, through preparing solution, reaction kettle crystallization reaction, constant temperature heating, quench cooling, wash dispersing, centrifugal separation, washing, vacuum drying, high-temperature vacuum roasting, grinding and sieving, make zeolite of hierarchical pore side of final product, this preparation method is advanced, the data is precise and actual, the product is white powder, the purity of the product reaches 99.8%, it is the advanced method to prepare zeolite of hierarchical pore side.
The invention has reasonable design and good market application and popularization value.
Drawings
FIG. 1 shows the X-ray diffraction intensity spectrum of a multiwell analcime.
Figure 2 shows a multiwell analcime morphology.
FIG. 3 shows the nitrogen adsorption and desorption isotherms of the hierarchical pore analcime.
Figure 4 shows a plot of the pore size distribution calculated for the multi-stage pore zeolite according to the N L DFT model.
Detailed Description
The following detailed description of specific embodiments of the invention refers to the accompanying drawings.
Hierarchical pore analciteThe preparation method uses chemical materials as follows: sodium metaaluminate, sodium hydroxide, deionized water, white carbon black and asymmetric gemini quaternary ammonium salt cationic surfactant, wherein the preparation dosage is as follows: in grams, milliliters and centimeters3As a unit of measure
Sodium metaaluminate: NaAlO20.630g±0.001g
Sodium hydroxide: NaOH0.480g ±0.001g
White carbon black: SiO 226.000g±0.001g
Asymmetric gemini quaternary ammonium salt cationic surfactant: c33H72N2Br212.340g±0.001g
Deionized water: h2O 12.25mL±0.01mL
Argon gas: ar 100000cm3±100cm3
C33H72N2Br2: the asymmetric gemini quaternary ammonium salt cationic surfactant has the following unique molecular structural formula:
the preparation method comprises the following steps
(1) Selecting chemical materials
The chemical material used for preparation is selected and subjected to quality purity control:
sodium metaaluminate: 99.9 percent of solid
Sodium hydroxide: 99.9 percent of solid
White carbon black: solid state 97%
Deionized water: 99.9 percent of liquid
Asymmetric gemini quaternary ammonium salt cationic surfactant: 98 percent of liquid
Argon gas: 99.9% of gaseous gas
(2) Preparing sodium hydroxide solution
Weighing 0.48g +/-0.001 g of sodium hydroxide and 3m L +/-0.01 m L of deionized water, adding the sodium hydroxide into a beaker, stirring the mixture by using a stirrer for 30min, and stirring the mixture to obtain a 4 mol/L sodium hydroxide aqueous solution;
(3) preparing the hierarchical pore analcite
Weighing deionized water 9.25m L +/-0.01 m L, sodium hydroxide solution 1.75m L +/-0.01 m L, weighing sodium metaaluminate 0.63g +/-0.001 g, asymmetric gemini quaternary ammonium salt cationic surfactant 12.34g +/-0.001 g and white carbon black 6g +/-0.001 g, adding into a polytetrafluoroethylene container, heating and stirring for 1h at the constant temperature of 25 +/-1 ℃ by adopting a heat-collecting constant-temperature magnetic stirrer, and fully dissolving the mixture at the stirring revolution of 200r/min to form a white gel solution;
Placing the polytetrafluoroethylene container containing the mixed solution on an electric heater, wherein the electric heater is heated at 50 +/-1 ℃ for 40 h;
Placing the polytetrafluoroethylene container containing the mixed solution into a reaction kettle, sealing, then placing the reaction kettle into a thermostat, heating to 140 +/-2 ℃, keeping the temperature, and carrying out static crystallization reaction for 96 hours;
After the heating crystallization reaction is finished, closing the constant temperature box, placing the reaction kettle in a quenching tank, and rapidly cooling the reaction kettle to 20 ℃ in deionized water at 10 ℃;
Opening the reaction kettle after cooling, pouring the mixed turbid liquid in the polytetrafluoroethylene container into a beaker, adding 600m L of deionized water, and stirring on a magnetic stirrer for 30min to obtain diluted mixed turbid liquid;
placing the diluted mixed turbid liquid in a centrifugal separation tube, performing centrifugal separation, wherein the centrifugal separation rotation number is 5000r/min, the separation time is 15min, retaining solid precipitate after centrifugal separation, and discarding supernatant;
Placing the separated solid precipitate in a beaker, adding deionized water of 500m L, and then placing in an ultrasonic disperser for ultrasonic cleaning and dispersing, wherein the ultrasonic frequency is 40Hz, and the dispersing time is 30 min;
then placing the dispersion solution into a centrifugal separation tube of a centrifugal machine, carrying out centrifugal separation, wherein the centrifugal separation revolution number is 5000r/min, the separation time is 15min, retaining solid precipitate after centrifugal separation, and discarding supernatant;
cleaning, dispersing, and repeatedly performing centrifugal separation for 3 times;
Putting the solid precipitate into a quartz container, then putting the quartz container into a vacuum drying oven for drying at the drying temperature of 100 ℃, the vacuum degree of 2Pa for 12h, and drying to obtain a powder product;
The roasting of the hierarchical pore analcite is carried out in a vacuum sintering furnace under the conditions of heating, vacuumizing, argon protection and external water circulation cooling;
A. putting the solid precipitate into a quartz container, and then putting the quartz container on a workbench in a vacuum sintering furnace;
B. closing the vacuum sintering furnace, starting a vacuum pump, and extracting air in the furnace to enable the pressure in the furnace to reach 5 Pa;
C. opening an argon bottle and an argon pipe, and introducing argon into the furnace to ensure that the pressure in the furnace is constant at 0.9 MPa;
D. opening an external water circulation cooling pipe to carry out external water circulation cooling;
E. starting a resistance heater, heating to 550 +/-2 ℃, and roasting for 360 min;
F. cooling, stopping heating after roasting, and cooling a product in a quartz container to 25 ℃ along with a furnace;
G. cooling to obtain multi-grade pore zeolite;
(4) grinding and sieving
Grinding the roasted powder product by using an agate mortar and a pestle, and then sieving by using a 200-mesh sieve;
grinding and sieving are carried out repeatedly to obtain the final product of the multi-grade pore zeolite;
(5) detection, analysis, characterization
Detecting, analyzing and characterizing the crystal structure, the appearance, the color and the chemical and physical properties of the prepared hierarchical pore analcime;
A. analysis of crystalline phase and crystallinity by X-ray diffractometer
Fig. 1 is an X-ray diffraction intensity spectrum of the hierarchical pore square zeolite, and as can be seen from the figure, the synthesized hierarchical pore square zeolite shows a characteristic diffraction peak, the peak shape is sharp, no other impurity peak exists, the diffraction intensity is high, and meanwhile, a small-angle range has an obvious diffraction peak, which proves that the synthesized hierarchical pore square zeolite contains rich ordered secondary pore channel structures.
B. Analysis of product crystal morphology by scanning electron microscope
FIG. 2 is a morphological diagram of a hierarchical pore analcime, and it can be seen that the surface roughness of the synthesized hierarchical pore analcime shows a large amount of mesopores and is rich in abundant accumulated secondary pore structures.
C. FIG. 3 is a graph of multistage analcime nitrogen adsorption and desorption curves, as shown by the formula N2The adsorption and desorption curves can be seen to be 0.4<P/P0<1.0, an obvious desorption hysteresis loop appears, which is due to the existence of mesopores, a capillary condensation phenomenon occurs, and the condition indicates that a large amount of mesopore structures exist in the synthesized hierarchical pore analcime.
D. FIG. 4 is a pore size distribution curve of hierarchical pore square zeolite, which shows that the synthesized hierarchical pore square zeolite molecular sieve has obvious micropore size distribution in the range of 0-1 nm, and has a mesopore size distribution in the range of 1-10 nm, which proves that intragranular mesopores exist, the pore size distribution is concentrated, and the high order degree is shown.
And (4) conclusion: the prepared hierarchical pore analcite is white powder, and the purity of the product reaches 99.8 percent;
(6) storage of the product
The prepared hierarchical porous analcite white powder is put into a brown transparent glass container and is stored in a sealed and light-proof way, and the storage temperature is 20 ℃ and the relative humidity is 10 percent, wherein the moisture protection, the sun protection and the corrosion resistance of acid, alkali and salt are required.
Finally, it should be noted that the above embodiments are only for illustrating the technical solutions of the present invention and not for limiting, and although the detailed description is made with reference to the embodiments of the present invention, it should be understood by those skilled in the art that modifications or equivalent substitutions may be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention, which shall be covered by the claims of the present invention.
Claims (1)
1. A method for preparing analcime with a micro-mesoporous structure is characterized by comprising the following steps: the method comprises the following steps:
(1) chemical material
The chemical materials used were: sodium metaaluminate, sodium hydroxide, deionized water, white carbon black and asymmetric gemini quaternary ammonium salt cationic surfactant, wherein the preparation dosage is as follows:
sodium metaaluminate: NaAlO20.630g
Sodium hydroxide: NaOH 0.480g
White carbon black: SiO 226.000g
Asymmetric gemini quaternary ammonium salt cationic surfactant: c33H72N2Br212.340g
Deionized water: h2O 12.25mL
C33H72N2Br2: the asymmetric gemini quaternary ammonium salt cationic surfactant has the following unique molecular structural formula:
(2) preparing sodium hydroxide solution
Weighing 0.48g of sodium hydroxide and 3m L g of deionized water, adding the sodium hydroxide and the deionized water into a beaker, stirring the mixture by using a stirrer for 30min, and stirring the mixture to obtain a 4 mol/L sodium hydroxide aqueous solution;
(3) preparing the hierarchical pore analcite
① preparing multi-stage pore analcime mixed solution
Weighing 9.25m L deionized water and 1.75m L sodium hydroxide solution, weighing 0.63g sodium metaaluminate, 12.34g asymmetric gemini quaternary ammonium salt cationic surfactant and 6g white carbon black, adding into a polytetrafluoroethylene container, heating and stirring for 1h at a constant temperature of 25 ℃ by using a heat collection type constant temperature magnetic stirrer, wherein the stirring revolution is 200r/min, so that the mixture is fully dissolved to form a white gel solution;
② standing at constant temperature
Placing the polytetrafluoroethylene container containing the mixed solution on an electric heater, wherein the electric heater is heated at 50 ℃ for 40 h;
③ heat crystallization
Placing the polytetrafluoroethylene container containing the mixed solution into a reaction kettle, sealing, then placing the reaction kettle into a thermostat, heating to 140 ℃, keeping the temperature constant, and carrying out static crystallization reaction for 96 hours;
④ quenching
After the heating crystallization reaction is finished, closing the constant temperature box, placing the reaction kettle in a quenching tank, and rapidly cooling the reaction kettle to 20 ℃ in deionized water at 10 ℃;
⑤ diluting with deionized water, and centrifuging
Opening the reaction kettle after cooling, pouring the mixed turbid liquid in the polytetrafluoroethylene container into a beaker, adding 600m L of deionized water, and stirring on a magnetic stirrer for 30min to obtain diluted mixed turbid liquid;
placing the diluted mixed turbid liquid in a centrifugal separation tube, performing centrifugal separation, wherein the centrifugal separation rotation number is 5000r/min, the separation time is 15min, retaining solid precipitate after centrifugal separation, and discarding supernatant;
⑥ washing, dispersing, and centrifuging
Placing the separated solid precipitate in a beaker, adding deionized water of 500m L, and then placing in an ultrasonic disperser for ultrasonic cleaning and dispersing, wherein the ultrasonic frequency is 40Hz, and the dispersing time is 30 min;
then placing the dispersion solution into a centrifugal separation tube of a centrifugal machine, carrying out centrifugal separation, wherein the centrifugal separation revolution number is 5000r/min, the separation time is 15min, retaining solid precipitate after centrifugal separation, and discarding supernatant;
cleaning, dispersing, and repeatedly performing centrifugal separation for 3 times;
⑦ vacuum drying
Putting the solid precipitate into a quartz container, then putting the quartz container into a vacuum drying oven for drying at the drying temperature of 100 ℃, the vacuum degree of 2Pa for 12h, and drying to obtain a powder product;
⑧ vacuum roasting
The roasting of the hierarchical pore analcite is carried out in a vacuum sintering furnace under the conditions of heating, vacuumizing, argon protection and external water circulation cooling;
A. putting the powder product into a quartz container, and then putting the quartz container on a workbench in a vacuum sintering furnace;
B. closing the vacuum sintering furnace, starting a vacuum pump, and extracting air in the furnace to enable the pressure in the furnace to reach 5 Pa;
C. opening an argon bottle and an argon pipe, and introducing argon into the furnace to ensure that the pressure in the furnace is constant at 0.9 MPa;
D. opening an external water circulation cooling pipe to carry out external water circulation cooling;
E. starting a resistance heater, heating to 550 ℃, and roasting for 360 min;
F. cooling, stopping heating after roasting, and cooling a product in a quartz container to 25 ℃ along with a furnace;
G. cooling to obtain multi-grade pore zeolite;
(4) grinding and sieving
Grinding the roasted powder product, and then sieving by using a 200-mesh sieve; grinding and sieving are carried out repeatedly to obtain the final product of the multi-grade pore zeolite.
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