CN112209399A - Method for preparing X-type zeolite from coal gangue - Google Patents
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Abstract
The invention discloses a method for preparing X-type zeolite from coal gangue. The method comprises the following steps: s1, activating and roasting gangue powder to obtain a roasted sample, mixing and grinding the roasted sample and solid alkali, and roasting and melting at high temperature to obtain a roasted product; s2, uniformly mixing the roasted product and water, and aging and crystallizing the obtained extracting solution to obtain a mixture; and S3, carrying out aftertreatment on the mixture to obtain the X-type zeolite. The method does not need to add a silicon source and an aluminum source, reduces the cost of raw materials, and the synthesized zeolite has uniform size, complete crystal form and high crystallinity.
Description
Technical Field
The invention belongs to the field of zeolite preparation, relates to a zeolite preparation method, and particularly relates to a method for preparing X-type zeolite from coal gangue.
Background
China is a big coal-producing country, more than 2000 coal gangue hills with larger scale exist, the total stacking amount of coal gangue reaches more than 50 hundred million tons, and the coal gangue is increased at the speed of 1.5-2.0 hundred million tons per year. A large amount of coal gangue occupies about 1.5 multiplied by 108m2The land of (2) enables the per capita cultivated land area to be seriously reduced, and is obviously threatened for China. Therefore, the exploration of the utilization value of the coal gangue becomes an important problem to be solved at present.
The coal gangue consists of mineral components such as quartz, albite, kaolinite, illite and the like, contains more than ten elements, and mainly contains chemical elements such as C, Si, Al, O, Fe, Ca, Mg and K. The artificially synthesized zeolite has less impurities, uniform pore passages, large specific surface area, good hydrothermal stability and stronger acid resistance, and can be used for adsorption, ion exchange and catalysis. Therefore, the artificially synthesized zeolite is widely applied to the fields of petrochemical industry, environmental protection, medicine and the like. The prior methods for synthesizing zeolite mainly comprise a direct conversion method, a traditional hydrothermal synthesis method, an alkali melt hydrothermal synthesis method, a microwave synthesis method, a thermal activation method, a gas phase crystallization method, a vapor phase method and the like. How to utilize and synthesize the zeolite with the coal gangue waste, solve the difficult problem of stacking the coal gangue, make the resource utilization of the coal gangue, and achieve the purpose of turning waste into wealth, becomes the technical problem to be solved urgently.
Disclosure of Invention
The invention provides a method for preparing X-type zeolite from coal gangue, which comprises the following steps:
s1, activating and roasting gangue powder to obtain a roasted sample, mixing and grinding the roasted sample and solid alkali, and roasting and melting at high temperature to obtain a roasted product;
s2, uniformly mixing the roasted product and water, and aging and crystallizing the obtained extracting solution to obtain a mixture;
and S3, carrying out aftertreatment on the mixture to obtain the X-type zeolite.
According to the embodiment of the invention, in the step S1, the coal gangue contains SiO in percentage by mass2And Al2O3，SiO2And Al2O3The sum of the masses of (A) and (B) accounts for 75-85%, preferably 78-82%, exemplarily 80%, 80.86%, 81% of the mass of the coal gangue.
Preferably, in the coal gangue, SiO2And Al2O3Is in the range of 4.5 to 6.5, such as 5.0 to 6.0, exemplary 5.2, 5.5, 5.8.
According to the embodiment of the invention, in step S1, the coal gangue further contains Fe2O3CaO, MgO and K2At least one of O.
Illustratively, the coal gangue comprises the following components in percentage by mass: SiO 22 61.68％，Al2O319.18％，Fe2O3 2.62％，CaO 0.46％，MgO 0.45％，K2O 3.09％，Na2O 1.14％，LOS10.02％。
According to an embodiment of the present invention, in step S1, the finer the particle size of the gangue powder, the better, for example, the particle size is less than 50 mesh, and further, less than 100 mesh.
According to the embodiment of the invention, in step S1, the temperature of the activation baking is 700-900 deg.C, such as 750-850 deg.C, and exemplary temperatures are 700 deg.C, 750 deg.C, 800 deg.C, 850 deg.C, 900 deg.C.
According to an embodiment of the present invention, in step S1, the activation firing time is 1-3h, such as 1.5-2.5h, and is exemplary 2 h.
According to an embodiment of the present invention, in step S1, the solid base may be at least one of solid NaOH and sodium carbonate; exemplary are NaOH pellets.
According to an embodiment of the invention, in step S1, the mass ratio of the roasted species to the solid base is 1 (1.1-1.6), such as 1 (1.1-1.3), illustratively 1:1.2, 1: 1.3.
According to an embodiment of the present invention, in step S1, the roasted sample and the solid base need to be well mixed and ground.
According to the embodiment of the invention, in step S1, the temperature of the high-temperature roasting is 700-900 ℃, such as 800-850 ℃, and an exemplary temperature is 850 ℃.
According to an embodiment of the present invention, in step S1, the high temperature baking time is 0.5 to 3 hours, such as 1 to 2.5 hours, and is exemplarily 1 hour.
According to an embodiment of the present invention, the roast needs to be ground into powder before being mixed with water in step S2. Among them, the smaller the particle size of the calcined powder, the better.
According to an embodiment of the invention, in step S2, the calcine to water alkali concentration ratio is 2.4-3.2, such as 2.8-3.2, illustratively 3.0. The alkali concentration is a concentration of an alkali in water, and is calculated as (molar mass of the sodium hydroxide raw material/volume of water added ═ alkali concentration).
According to an embodiment of the invention, the temperature of the aging in step S2 is 60-80 ℃, such as 65-75 ℃, exemplary 70 ℃.
According to an embodiment of the invention, in step S2, the aging time is 8-20h, such as 12-18h, for example 16 h.
According to an embodiment of the present invention, in step S2, the crystallization temperature is 90-120 deg.C, such as 100-110 deg.C, and is exemplary 100 deg.C.
According to an embodiment of the present invention, in step S2, the crystallization time is 3-18h, such as 5-15h, for example 9 h.
According to an embodiment of the present invention, the post-treatment comprises cooling, washing, and drying in step S3.
According to an exemplary embodiment of the invention, the method for preparing the type X zeolite from the coal gangue comprises the following steps:
s1, activating and roasting the coal gangue powder, mixing and grinding a roasted sample and NaOH particles, roasting and melting at high temperature, cooling and grinding to obtain a roasted product;
wherein, the coal gangue contains SiO in percentage by mass2And Al2O3，SiO2And Al2O3The mass sum of the coal gangue accounts for 75-85 percent of the mass of the coal gangue, and SiO accounts for2And Al2O3The molar ratio of (A) is 4.5-6.5;
the mass ratio of the roasted sample to NaOH is 1 (1.1-1.3);
s2, adding water into the roasted product obtained in the step S1, uniformly stirring, placing the extracting solution obtained by hydrothermal synthesis into a reaction kettle, and aging and crystallizing to obtain a mixture;
wherein the alkali concentration ratio of the roasted product to water is 2.8-3.2;
and S3, cooling, washing and drying the mixture obtained in the step S2 to obtain the X-type zeolite.
The invention also provides the X-type zeolite prepared by the method.
The invention has the beneficial effects that:
the invention provides a method for preparing X-type zeolite by using coal gangue, wherein the coal gangue in the Renbell area is preferably used as a raw material, so that reaction raw materials can be saved, a silicon source and an aluminum source are not required to be added in the synthesis process, resources are saved, X-type zeolite with uniform structure particle size, complete crystal form and clear edges and corners can be synthesized, and the crystallinity of the X-type zeolite is high.
Drawings
Fig. 1 is a method route diagram provided in example 1 of the present invention.
Figure 2 is an XRD pattern of the zeolite prepared under different calcination temperature conditions of example 1.
Figure 3 is an XRD pattern of the zeolite prepared under different soda ash ratio conditions of example 2.
FIG. 4 is an SEM image of zeolites prepared under different soda ash ratio conditions of example 2.
Figure 5 is an XRD pattern of the zeolite prepared under different base concentration conditions of example 3.
Figure 6 is an SEM image of zeolites prepared under different base concentration conditions for example 3.
Figure 7 is an XRD pattern of the zeolite prepared in example 4 at different aging times.
Figure 8 is an SEM image of the zeolite prepared in example 4 at different aging times.
Figure 9 is an XRD pattern of the zeolite prepared at different crystallization temperatures of example 5.
FIG. 10 is an SEM image of zeolites prepared at different crystallization temperatures of example 5.
Figure 11 is an XRD pattern of the zeolite prepared in example 6 at different crystallization times.
FIG. 12 is an SEM image of zeolites prepared at different crystallization times for example 6.
Detailed Description
The technical solution of the present invention will be further described in detail with reference to specific embodiments. It is to be understood that the following examples are only illustrative and explanatory of the present invention and should not be construed as limiting the scope of the present invention. All the technologies realized based on the above-mentioned contents of the present invention are covered in the protection scope of the present invention.
Unless otherwise indicated, the raw materials and reagents used in the following examples are all commercially available products or can be prepared by known methods.
Coal refuse used in the following examplesThe coal gangue in the Renbell area comprises the following components: by mass percent, SiO2 61.68％，Al2O3 19.18％，Fe2O3 2.62％，CaO 0.46％，MgO 0.45％，K2O 3.09％，Na21.14% of O, 10.02% of LOS and 1.36% of the rest; SiO 22And Al2O3Is about 5.5.
Example 1
As shown in the route of figure 1, coal gangue powder is taken into a crucible, activated for 2 hours in a muffle furnace at 800 ℃, an activated sample of 2g of coal gangue powder is taken and NaOH is 2.4g to adjust the alkali-ash ratio to be 1.2, the mixture is fully ground and mixed, the mixture is respectively placed into muffle furnaces at 700 ℃, 750 ℃, 800 ℃, 850 ℃ and 900 ℃ to be roasted for 1 hour, the mixture is cooled and ground into powder, water is added to adjust the alkali concentration ratio to be 2.8, the mixture is uniformly stirred on a constant-temperature magnetic stirrer, an extracting solution is placed into a reaction kettle and is aged for 12 hours at 70 ℃ and crystallized for 6 hours at 100 ℃ in a constant-temperature box, the solution is cooled, washed to be neutral, and dried to obtain the zeolite.
The XRD pattern of the synthetic zeolite is shown in figure 2. As can be seen from fig. 2: at the roasting temperature of 700-750 ℃, characteristic diffraction peaks of the A-type zeolite appear, while diffraction peaks of the X-type zeolite have weak intensity and more impurity peaks, which indicates that the zeolite synthesized at the temperature is a mixed phase of the A-type zeolite and the X-type zeolite. At the temperature of 800 ℃ and 850 ℃, the characteristic peak of the A-type zeolite disappears, the impurity peak is reduced, and the characteristic peak of the X-type zeolite is gradually strengthened, which shows that the mixed phase is gradually converted into a single phase along with the increase of the temperature. The number of peaks increased at 900 ℃ and the diffraction peak of the X-type zeolite decreased. The reason is probably that in the alkali melting process of the coal gangue and NaOH, effective silicon-aluminum components cannot be extracted at too low temperature, and as the temperature rises, carbonized substances and other impurity components in the coal gangue react with the NaOH, the dissolution rate of silicon-aluminum is improved, impurities are reduced, and the crystallization rate is improved, while when the temperature is too high, decomposed kaolinite in the coal gangue is converted into mullite without activity, and the silicon-aluminum ratio of an activation component is reduced, so that the crystallization rate is reduced. The zeolite has sharp characteristic peak at 850 ℃, less impurities and high crystallinity, so the optimum roasting temperature is 850 ℃.
Example 2
The method comprises the steps of putting coal gangue powder into a crucible, activating the powder in a muffle furnace at 800 ℃ for 2 hours, fully grinding and mixing an activated sample of 2g of the coal gangue powder and 2.4g of NaOH to adjust the alkali-ash ratio to be 1.2, 1.3, 1.4, 1.5 and 1.6, putting the mixture into the muffle furnace at 850 ℃ for roasting for 1 hour, cooling and grinding the mixture into powder, adding water to adjust the alkali concentration ratio to be 2.8, uniformly stirring the mixture on a constant-temperature magnetic stirrer, putting an extracting solution into a reaction kettle, ageing the extracting solution in a constant-temperature box at 70 ℃ for 12 hours, crystallizing the extracting solution at 100 ℃ for 6 hours, cooling and washing the extracting solution to be neutral, and drying the extracting solution to obtain the zeolite.
The XRD pattern of the synthetic zeolite is shown in figure 3. As can be seen from fig. 3: when the alkali-ash ratio is 1.2-1.3, the X-type characteristic diffraction peak is sharp and the intensity is enhanced, which shows that the synthesized zeolite has high crystallinity; at an alkali-ash ratio of 1.4-1.6, a weaker diffraction peak of the A-type zeolite appears, and the diffraction peak shape is gradually enhanced along with the increase of the alkali-ash ratio, which shows that the crystallinity of the A-type zeolite is gradually improved along with the increase of the alkali-ash ratio. Comparing the SEM images of the synthetic X-type zeolite at different alkali-ash ratios shown in FIG. 4, at an alkali-ash ratio of 1.2. The synthesized X-type zeolite has uniform particle size, clear edges and corners and relatively complete crystal form; when the alkali-ash ratio is 1.3, the synthesized zeolite has a sticky phenomenon, and when the alkali-ash ratio is 1.4-1.5, the zeolite has the sticky phenomenon and other impurities are generated quickly. This is probably because, as the alkali-ash ratio increases, the NaOH extracts, in addition to the silica-alumina component in the coal gangue, the excess NaOH reacts with other impurities in the coal gangue to form a melt, promoting the formation of impurities. The optimum soda-to-ash ratio is 1.2 as described in conjunction with fig. 3 and 4.
Example 3
Putting coal gangue powder into a crucible, activating for 2 hours in a muffle furnace at 800 ℃, taking an activated sample of 2g of coal gangue powder and 2.4g of NaOH to adjust the alkali-ash ratio to be 1.2, fully grinding and mixing, roasting for 1 hour in the muffle furnace at 850 ℃, cooling and grinding into powder, adding water to adjust the alkali concentration ratio to be 2.4, 2.8, 3.0, 3.2 and 3.4, uniformly stirring on a constant-temperature magnetic stirrer, putting an extracting solution into a reaction kettle, aging at 70 ℃ for 12 hours and crystallizing at 100 ℃ for 6 hours in a constant-temperature box, cooling, washing to be neutral, and drying to obtain the zeolite.
The XRD pattern of the synthetic zeolite is shown in figure 5. As can be seen from fig. 5: at 31.05 degrees of 2 theta, the peak intensity of the X-type characteristic diffraction peak shows a tendency of increasing and then decreasing along with the increase of the alkali concentration, at the alkali concentration ratio of 2.4, the characteristic peak intensity is weaker, the alkalinity is possibly too low, the crystal nucleation rate is slow, the formed zeolite has lower crystallinity, at the alkali concentration ratio of 3.0, the characteristic diffraction peak intensity is maximum, and along with the further increase of the alkali concentration, the characteristic peak intensity is gradually reduced, which possibly increases the alkalinity to accelerate the depolymerization rate of the gel system, so that the number of crystal nuclei in the gel system is increased, and the crystallinity is reduced. Comparing the SEM images of the different base concentration ratios synthetic X-type zeolite shown in fig. 6, it can be seen that at a base concentration ratio of 2.4, the synthesized zeolite particles are smaller and accompanied by a small amount of impurity formation; when the alkali concentration ratio is 2.8, the synthesized zeolite particles are small and the clustering phenomenon is severe. When the alkali concentration ratio is 3.0, the formed zeolite has a smooth surface, uniform particle size, clear edges and corners and high crystallinity; at a base concentration ratio of 3.2, the synthesized zeolite again showed clustering. Consistent with the XRD detection result, the crystallinity of the synthesized zeolite is higher when the alkali concentration ratio is 3.0.
Example 4
The method comprises the steps of putting coal gangue powder into a crucible, activating the powder in a muffle furnace at 800 ℃ for 2 hours, putting an activated sample of 2g of the coal gangue powder and 2.4g of NaOH to adjust the alkali-ash ratio to be 1.2, fully grinding and mixing, roasting in the muffle furnace at 850 ℃ for 1 hour, cooling and grinding into powder, adding water to adjust the alkali concentration ratio to be 3.0, uniformly stirring on a constant-temperature magnetic stirrer, putting an extracting solution into a reaction kettle, aging in a constant-temperature box at 70 ℃ for 8 hours, 12 hours, 14 hours, 16 hours, 18 hours and 20 hours respectively, crystallizing at 100 ℃ for 6 hours, cooling, washing to be neutral, and drying to obtain the zeolite.
The XRD pattern of the synthetic zeolite is shown in figure 7. As can be seen from fig. 7: when the time is 8-12h, the X-type diffraction peak is low, and the number of impurities is large, which indicates that the X-type zeolite formed in a short aging time is incomplete in crystal form and contains a large number of impurities; when the aging time is 14h-16h, the diffraction peak is gradually enhanced, wherein the diffraction peak has the highest intensity, few impurity peaks and high crystallinity at 16 h; at the aging time of 18-20h, the diffraction peak intensity is weakened again, which shows that the gel system is changed from uneven-even-uneven with the increase of the aging time, probably because the aging time is too short, so that the kaolin cannot be completely dissolved, and the aging time is too long, so that the crystal nucleus formed is transformed. Comparing the SEM images of X-type zeolite synthesized at different aging times shown in FIG. 8, it can be seen that the X-type zeolite formed at an aging time of 12h has an incomplete structure, severe stickiness and more impurities; when 14h, the impurities are reduced but small clusters still exist, and when the aging time is 16h, the formed zeolite has few impurities, no cluster phenomenon, uniform particle size and high crystallinity. At the aging time of 20h, large clusters appear in the zeolite, and the formed zeolite particles are smaller. The optimum aging time was therefore 16 h.
Example 5
Putting coal gangue powder into a crucible, activating in a muffle furnace at 800 ℃ for 2h, taking 2g of activated sample and 2.4g of NaOH to adjust the alkali-ash ratio to be 1.2, fully grinding and mixing, roasting in the muffle furnace at 850 ℃ for 1h, cooling and grinding into powder, adding water to adjust the alkali concentration ratio to be 3.0, uniformly stirring on a constant-temperature magnetic stirrer, putting an extracting solution into a reaction kettle, aging at 70 ℃ for 16h in a constant-temperature box, crystallizing at 95 ℃, 100 ℃, 110 ℃ and 120 ℃ for 6h respectively, cooling, washing to be neutral, and drying to obtain the zeolite.
The XRD pattern of the synthetic zeolite is shown in figure 9. As can be seen from fig. 9: when the crystallization temperature is 90 ℃, the formed X-type zeolite has very small characteristic peak and disordered peaks, which shows that the zeolite synthesized at the temperature has more impurities; the diffraction peak profile of the synthetic zeolite is sharp and narrow at 100 ℃, the intensity is high, the number of the impurity peaks is small, and the crystallinity is high; the diffraction peak intensity of the synthesized X-type zeolite is gradually reduced along with the increase of the crystallization temperature. Comparing with the SEM topography of the synthetic zeolite shown in FIG. 10, the zeolite synthesized at 90 ℃ has more impurities and incomplete crystal form, and the zeolite synthesized at 100 ℃ has less impurities, single crystal form, uniform size, smooth surface and high crystallinity; at the temperature of 110 ℃ and 120 ℃, although the synthesized X zeolite has complete crystal form and clear edges and corners, clustering phenomena with different degrees of sizes exist. This is probably because the increase of crystallization temperature accelerates the chemical reaction rate, increases the reaction rate of aluminum ions and alumino-silicate ions in the gel, promotes the rapid dissolution of the gel, accelerates the nucleation of crystal nuclei and the growth rate of crystals, forms zeolites with different structures, and when the crystallization temperature is too high, the crystal diameter is increased, and the phenomenon of sticking occurs or the crystal transformation occurs. Thus, the optimum crystallization temperature was determined to be 100 ℃ from XRD and SEM image analysis.
Example 6
The method comprises the steps of putting coal gangue powder into a crucible, activating the coal gangue powder in a muffle furnace at 800 ℃ for 2 hours, putting an activated sample of 2g of the coal gangue powder and 2.4g of NaOH to adjust the alkali-ash ratio to be 1.2, fully grinding and mixing, roasting in the muffle furnace at 850 ℃ for 1 hour, cooling and grinding into powder, adding water to adjust the alkali concentration ratio to be 3.0, uniformly stirring on a constant-temperature magnetic stirrer, putting an extracting solution into a reaction kettle, aging at 70 ℃ for 16 hours in a constant-temperature box, crystallizing at 100 ℃ for 3 hours, 6 hours, 9 hours, 12 hours and 18 hours respectively, cooling, washing to be neutral, and drying to obtain the zeolite.
The XRD pattern of the synthetic zeolite is shown in figure 11. As can be seen from fig. 11: the intensity of the X-type characteristic diffraction peak tends to increase and then decrease with the increase of the crystallization time. When the crystallization time is 3 hours, more impurity peaks are generated, and the diffraction peak is small, which indicates that more impurities exist; the diffraction peak intensity is gradually enhanced and the peak is narrow and sharp at 6-9h, which shows that the zeolite crystal form in the crystallization time period is gradually complete and the crystallinity is improved, and the reaction system mainly takes crystal growth as the main point; and when the time is 12-18h, the intensity of the characteristic diffraction peak is gradually reduced, which shows that the crystallinity of the zeolite is reduced in the crystallization time period. Comparing the SEM appearance images of X-type zeolite with different crystallization time shown in FIG. 12, when 6h, large clusters are generated in the synthesized zeolite, and the zeolite synthesized in 9h has uniform particle size and good appearance; the zeolite synthesized in 12-18h has small amount of impurities and non-uniform size clusters. This is probably because the crystallization time is prolonged, the condensation time of crystal nuclei is long, the crystal form of the formed crystal grains is complete, the crystallinity is high, and the crystallization time is too long, which causes the crystal grains to be transformed or aggregated to cause clustering. From the above analysis, the optimum crystallization time was 9 hours.
The embodiments of the present invention have been described above. However, the present invention is not limited to the above embodiment. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A method for preparing X-type zeolite from coal gangue is characterized by comprising the following steps:
s1, activating and roasting gangue powder to obtain a roasted sample, mixing and grinding the roasted sample and solid alkali, and roasting and melting at high temperature to obtain a roasted product;
s2, uniformly mixing the roasted product and water, and aging and crystallizing the obtained extracting solution to obtain a mixture;
and S3, carrying out aftertreatment on the mixture to obtain the X-type zeolite.
2. The method according to claim 1, wherein in step S1, the coal refuse contains SiO in percentage by mass2And Al2O3，SiO2And Al2O3The mass sum of (A) and (B) accounts for 75-85%, preferably 78-82%, preferably 80%, 80.86% and 81% of the mass of the coal gangue.
Preferably, in the coal gangue, SiO2And Al2O3Is from 4.5 to 6.5, for example from 5.0 to 6.0, preferably 5.2, 5.5, 5.8.
Preferably, the coal gangue also contains Fe2O3CaO, MgO and K2At least one of O.
Preferably, the coal gangue comprises the following components in percentage by mass: SiO 22 61.68％，Al2O319.18％，Fe2O3 2.62％，CaO 0.46％，MgO 0.45％，K2O 3.09％，Na2O 1.14％，LOS 10.02％。
3. The method according to claim 1 or 2, wherein in step S1, the gangue powder has a particle size of less than 50 mesh, such as less than 100 mesh.
Preferably, in step S1, the temperature of the activation baking is 700-900 deg.C, such as 750-850 deg.C.
Preferably, in step S1, the activation baking time is 1-3h, such as 1.5-2.5 h.
4. The method according to any one of claims 1 to 3, wherein in step S1, the solid base is at least one of solid NaOH and sodium carbonate.
Preferably, in step S1, the mass ratio of the roasted sample to the solid base is 1 (1.1-1.6), for example 1 (1.1-1.3).
Preferably, in step S1, the roasted sample and the solid alkali need to be mixed and ground thoroughly.
Preferably, in step S1, the temperature of the high-temperature calcination is 700-900 ℃, such as 800-850 ℃.
Preferably, in step S1, the high temperature roasting time is 0.5-3h, such as 1-2.5 h.
5. The method as claimed in any one of claims 1 to 4, wherein in step S2, the calcine is ground into powder before being mixed with water.
Preferably, in step S2, the ratio of the calcine to the alkali concentration of water is 2.4 to 3.2, for example 2.8 to 3.2.
6. The process according to any one of claims 1 to 5, wherein in step S2, the temperature of aging is 60 to 80 ℃, such as 65 to 75 ℃.
Preferably, in step S2, the aging time is 8-20h, such as 12-18 h.
7. The method as claimed in any one of claims 1 to 6, wherein the temperature of the crystallization in step S2 is 90-120 ℃, such as 100-110 ℃.
Preferably, in step S2, the crystallization time is 3-18h, for example 5-15 h.
8. The method according to any one of claims 1 to 7, wherein the post-treatment comprises cooling, washing and drying in step S3.
9. The method of claim 1, wherein the coal gangue preparation method for type X zeolite comprises the steps of:
s1, activating and roasting the coal gangue powder, mixing and grinding a roasted sample and NaOH particles, roasting and melting at high temperature, cooling and grinding to obtain a roasted product;
wherein, the coal gangue contains SiO in percentage by mass2And Al2O3，SiO2And Al2O3The mass sum of the coal gangue accounts for 75-85 percent of the mass of the coal gangue, and SiO accounts for2And Al2O3The molar ratio of (A) is 4.5-6.5;
the mass ratio of the roasted sample to NaOH is 1 (1.1-1.3);
s2, adding water into the roasted product obtained in the step S1, uniformly stirring, placing the extracting solution obtained by hydrothermal synthesis into a reaction kettle, and aging and crystallizing to obtain a mixture;
wherein the alkali concentration ratio of the roasted product to water is 2.8-3.2;
and S3, cooling, washing and drying the mixture obtained in the step S2 to obtain the X-type zeolite.
10. Zeolite X prepared by the process of any one of claims 1 to 9.
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Cited By (4)
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| CN112958144A (en) * | 2021-02-07 | 2021-06-15 | 内蒙古师范大学 | Preparation method and application of X-type zeolite molecular sieve catalyst |
| CN113428874A (en) * | 2021-05-31 | 2021-09-24 | 东南大学 | Preparation method and application method of gangue-based sodium ion type molecular sieve based on alkali fusion method |
| CN114751425A (en) * | 2022-04-02 | 2022-07-15 | 四川大学 | Preparation method and application of zeolite soil passivator with high iron content |
| CN114988426A (en) * | 2022-06-06 | 2022-09-02 | 西安科技大学 | Coal gangue-based molecular sieve and alkali fusion-hydrothermal preparation method thereof |
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| CN113428874A (en) * | 2021-05-31 | 2021-09-24 | 东南大学 | Preparation method and application method of gangue-based sodium ion type molecular sieve based on alkali fusion method |
| CN114751425A (en) * | 2022-04-02 | 2022-07-15 | 四川大学 | Preparation method and application of zeolite soil passivator with high iron content |
| CN114988426A (en) * | 2022-06-06 | 2022-09-02 | 西安科技大学 | Coal gangue-based molecular sieve and alkali fusion-hydrothermal preparation method thereof |
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