CN109095476B - Method for preparing hydroxysodalite by using fly ash sub-molten salt alkaline hydrothermal method - Google Patents
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Abstract
The invention provides a method for preparing hydroxyl sodalite zeolite by using fly ash, belonging to the field of production and preparation of inorganic functional materials. The method takes fly ash as a raw material, adopts a sub-molten salt system alkali hydrothermal method to synthesize and prepare the zeolite hydroxysodalite, completely converts a large amount of insoluble inert substances in the fly ash into the hydroxysodalite under the condition of ultrahigh-concentration sodium hydroxide hydrothermal, fully utilizes the silicon-aluminum substances in the fly ash, reduces silicate impurities, and can synthesize and prepare the high-purity hydroxysodalite, the method needs larger alkali concentration, does not need to add or add a small amount of other medicines, and the purity of the prepared hydroxysodalite zeolite reaches more than 90%.
Description
Technical Field
The invention relates to a method for preparing hydroxysodalite by using fly ash sub-molten salt alkaline hydrothermal method, which adopts a hydrothermal method to synthesize hydroxysodalite in a sub-molten salt system, and belongs to the field of production and preparation of inorganic functional materials.
Background
The fly ash is fine powdery industrial solid waste which is generated in a coal burning process of a coal burning power plant and is obtained by trapping. The fly ash discharge and the pushing quantity of China are huge, and data shows that the fly ash stacking quantity of China currently exceeds 60 hundred million tons, and the annual output of the fly ash stacking quantity of China exceeds 1 hundred million tons. The zeolite is aluminosilicate mineral with communicated pore channels and has ion exchange, catalysis, adsorption, photochromism, hydrogen storage performance and the like. The synthesis of zeolite by using the fly ash is one of the channels for the high added value utilization of the fly ash in recent years, and mainly forms the processes and methods such as the traditional hydrothermal method, the alkali fusion hydrothermal method, the microwave-assisted hydrothermal method, the seed crystal synthesis method and the like.
Patent CN201410677200.0 discloses a preparation method of zeolite, which utilizes water glass and a blending liquid to prepare a precursor by blending crystal seeds, the precursor is aged, and two-stage crystallization is performed to synthesize P-type zeolite and sodalite zeolite. The method uses chemical agents as raw materials, the synthesized product is pure but not single-phase hydroxyl sodalite, and the process is very complex. Patent CN201110055234.2 discloses a method for preparing single-phase hydroxysodalite from fly ash. The method has the advantages that the single-phase hydroxyl sodalite is prepared, but the method comprises two steps of roasting activation and hydrothermal crystallization, and the process complexity is increased. Patent CN201310608808.3 discloses a method for synthesizing sodalite zeolite by using fly ash. The method has the advantages that the traditional hydrothermal synthesis method is adopted, the process is simple, the reaction conditions are mild, but the synthesized product contains more impurities such as mullite, quartz, xonotlite and the like, and the purity of the sodalite product is poor. Patent CN201310697898.8 discloses a method for synthesizing Na-X and hydroxysodalite by using fly ash filter cake through dry process. The method has the advantages that the alkali fusion roasting process is adopted, different types of zeolite can be obtained by adjusting subsequent process conditions, but the complexity is higher by alkali fusion roasting, water dissolving and various subsequent adjusting processes. Therefore, the traditional hydrothermal method for synthesizing zeolite has the limitation that the mullite phase in the fly ash cannot be fully utilized, and the utilization rate of the fly ash is low.
Disclosure of Invention
In order to solve the problems, the invention provides a method for preparing hydroxysodalite from fly ash, which has simple process and extremely high efficiency. The method for preparing the hydroxysodalite zeolite by the novel hydrothermal method of the fly ash is provided by the research, aims to overcome the defects of the existing synthesis method in process, energy consumption and product, adopts a sub-molten salt system to synthesize the hydroxysodalite product with the purity of up to 90 percent on the basis of one-step hydrothermal method, does not need aging, has simple process and short reaction period, and efficiently utilizes the silicon-aluminum component in the fly ash. The method solves the problem that the mullite phase in the fly ash cannot be fully utilized in the conventional hydrothermal method for synthesizing the zeolite, and greatly improves the purity of the hydroxyl sodalite zeolite synthesized by the fly ash. And provides a new method for utilizing the fly ash. Has great significance for consuming industrial solid waste fly ash, utilizing secondary resources and protecting environment.
The invention provides a method for preparing zeolite, which takes fly ash as a raw material and adopts a sub-molten salt system alkali hydrothermal method to synthesize and prepare zeolite hydroxy sodalite.
Preferably, the mass ratio of the prepared solution to the fly ash is more than 10.
Preferably, the hydrothermal reaction step is as follows: the reaction is carried out in a high-temperature high-pressure reaction kettle, the reaction temperature is not lower than 220 ℃, and the reaction time is 60-120 min.
Preferably, the separation step is as follows: and separating the residue and the liquid, wherein the mother liquid can be circularly used as the ingredient in the preparation method after being added with NaOH.
Preferably, the slag and liquid in the reaction kettle can be separated by using the high pressure in the reaction kettle without cooling the reaction system, such as designing related process equipment.
Preferably, the filter residue is washed for multiple times by water or deionized water to obtain a filter cake, and the washing liquid can be continuously added with NaOH and circularly used for the ingredients in the preparation method, and can also be evaporated, crystallized and recycled with NaOH.
Preferably, the drying step is as follows: and drying the obtained filter cake at 90-120 ℃ for 6-24 h to obtain the synthetic product, namely the hydroxysodalite.
The invention also provides a zeolite material and the hydroxyl sodalite prepared by the method.
In the art, a number of documents indicate that hydrothermal conditions tend to produce hydroxysodalite product under alkaline hydrothermal conditions, and that higher basicities are more likely to form. The Li Hui spring finds that the residual solid phase of alkali-soluble aluminum extraction in the first-step aluminum extraction process is hydroxysodalite in the alkali-soluble aluminum extraction process of the sub-molten salt method. These studies provide the basis for the preparation of hydroxysodalite by a new hydrothermal process.
The method for preparing the hydroxysodalite by using the fly ash as the main raw material through the novel hydrothermal method not only can solve the problem of high cost of the raw material for synthesizing the sodalite, but also provides a new channel for high-added-value utilization of the solid waste fly ash. The sodalite serving as a photochromic material and a potential high-quality hydrogen storage material has extremely high development value, and the preparation of the hydroxyl sodalite product with low price and excellent performance has important significance for the development of novel inorganic materials.
The method for preparing the fly ash hydroxysodalite by the sub-molten salt alkaline hydrothermal method has the advantages of easily obtained raw materials, low energy consumption, recyclable hydrothermal mother liquor and simple process, and compared with the existing hydrothermal synthesis method, the synthesized hydroxysodalite product has greatly improved purity, is an excellent hydroxysodalite synthesis process and has extremely high development value.
The beneficial effects of the invention include the following:
(1) according to the invention, a sub-molten salt system hydrothermal synthesis method is adopted, so that a large amount of insoluble inert substances in the fly ash can be completely converted into the hydroxysodalite, silicon and aluminum substances in the fly ash are fully utilized, and silicate impurities are reduced; the high-purity hydroxysodalite can be synthesized and prepared without adding or adding a small amount of additional aluminum source.
(2) The sub-molten salt alkaline hydrothermal method provided by the invention has the advantages of no need of aging in the synthesis process, simple process, short synthesis period and high synthesis efficiency.
(3) The method for synthesizing the sub-molten salt by the alkali-water heating method has the advantages that the synthetic mother liquor can be used for recycling of the process, secondary formed slag is avoided, secondary resources of the fly ash are fully utilized, and the method is environment-friendly.
(4) The invention further expands the synthesis method and process of zeolite, and deepens and innovates the process method for synthesizing the hydroxysodalite material by using the fly ash. The utilization of the fly ash is combined with the synthesis of inorganic materials, so that the channel for the utilization of solid wastes and the synthesis of inorganic materials is widened, and the foundation is laid for the industrialization of the synthesis of fly ash zeolite.
(5) The method breaks through the limitation that the mullite phase in the fly ash cannot be fully utilized by the traditional hydrothermal method, and the hypofused salt system is utilized to synthesize the high-purity hydroxysodalite, wherein the sodalite content reaches more than 90%.
Detailed Description
The present invention is described in further detail below with reference to specific examples and with reference to the data. It will be understood that these examples are intended to illustrate the invention and are not intended to limit the scope of the invention in any way.
The fly ash feedstock in the examples of the invention was from a power plant in the inner Mongolia region and the composition is shown in Table 1 (without loss on ignition): through measurement, the loss on ignition of the used fly ash is about 2 percent, and the combustible content is less.
Table 1 elemental composition and content (%)
The following examples are further illustrative of the present invention and are not intended to limit the scope of the present invention. The comparative examples 1 and 2 are added in the invention examples for comparison to show that the hydroxy sodalite product with better quality can be obtained within a reasonable range of test conditions in the invention.
Example 1:
preparing 30g of 40% NaOH solution, weighing 3g of raw material coal ash, sequentially adding the coal ash and the NaOH solution into a high-pressure reaction kettle with a polytetrafluoroethylene lining, and stirring for about 30 seconds by using a glass rod to fully mix solid and liquid without deposition. And (3) placing the reaction kettle which is filled with the materials into a constant-temperature drying box for constant-temperature reaction for 90min, wherein the reaction temperature is 220 ℃, flushing and cooling the reaction kettle after the reaction is finished, collecting reaction mother liquor by using a dry suction bottle, wherein the reaction mother liquor can be used for circulating ingredients, then repeatedly washing a solid-phase product to be neutral by using deionized water, and placing a filter cake into the constant-temperature drying box for drying for 8h at the temperature of 105 ℃ to obtain a hydroxysodalite single-phase product with the purity of about 91%.
Example 2:
preparing 30g of 40% NaOH solution, weighing 1.5g of raw material coal ash, sequentially adding the coal ash and the NaOH solution into a high-pressure reaction kettle with a polytetrafluoroethylene lining, and stirring by a glass rod for about 30 seconds to fully mix solid and liquid without deposition. And (3) placing the reaction kettle which is filled with the materials into a constant-temperature drying box for constant-temperature reaction for 90min, wherein the reaction temperature is 220 ℃, flushing and cooling the reaction kettle after the reaction is finished, collecting reaction mother liquor by using a dry suction bottle, wherein the reaction mother liquor can be used for circulating ingredients, then repeatedly washing a solid-phase product to be neutral by using deionized water, and placing a filter cake into the constant-temperature drying box for drying for 8h at the temperature of 105 ℃ to obtain a hydroxysodalite single-phase product with the purity of 92%.
Example 3:
preparing 30g of 50% NaOH solution, weighing 6g of raw material coal ash, sequentially adding the coal ash and the NaOH solution into a high-pressure reaction kettle with a polytetrafluoroethylene lining, and stirring for about 30 seconds by using a glass rod to fully mix solid and liquid without deposition. And (3) placing the loaded reaction kettle into a constant-temperature drying box for constant-temperature reaction for 120min, wherein the reaction temperature is 220 ℃, flushing and cooling the reaction kettle after the reaction is finished, collecting reaction mother liquor by using a dry suction flask, wherein the reaction mother liquor can be used for circulating ingredients, then repeatedly washing a solid-phase product to be neutral by using deionized water, and placing a filter cake into the constant-temperature drying box for drying for 10h at the temperature of 105 ℃ to obtain a hydroxysodalite single-phase product with the purity of 91.5%.
Example 4:
preparing 30g of 50% NaOH solution, weighing 3g of raw material coal ash, sequentially adding the coal ash and the NaOH solution into a high-pressure reaction kettle with a polytetrafluoroethylene lining, and stirring for about 30 seconds by using a glass rod to fully mix solid and liquid without deposition. And (3) placing the reaction kettle which is filled with the materials into a constant-temperature drying box for constant-temperature reaction for 90min, wherein the reaction temperature is 230 ℃, flushing and cooling the reaction kettle after the reaction is finished, collecting reaction mother liquor by using a dry suction bottle, wherein the reaction mother liquor can be used for circulating ingredients, then repeatedly washing a solid-phase product to be neutral by using deionized water, and placing a filter cake into the constant-temperature drying box for drying for 12h at the temperature of 105 ℃ to obtain a hydroxysodalite single-phase product with the purity of 93%.
Example 5:
preparing 30g of 60% NaOH solution, weighing 6g of raw material coal ash, sequentially adding the coal ash and the NaOH solution into a high-pressure reaction kettle with a polytetrafluoroethylene lining, and stirring for about 30 seconds by using a glass rod to fully mix solid and liquid without deposition. And (3) placing the loaded reaction kettle into a constant-temperature drying box for constant-temperature reaction for 90min, wherein the reaction temperature is 230 ℃, flushing and cooling the reaction kettle after the reaction is finished, collecting reaction mother liquor by using a dry suction flask, wherein the reaction mother liquor can be used for circulating ingredients, then repeatedly washing a solid-phase product to be neutral by using deionized water, and placing a filter cake into the constant-temperature drying box for drying for 12h at the temperature of 105 ℃ to obtain a hydroxysodalite single-phase product with the purity of 92.7%.
Example 6:
30g of 30% NaOH solution is prepared, 3g of raw material coal ash is weighed, the coal ash and the NaOH solution are sequentially added into a high-pressure reaction kettle with a polytetrafluoroethylene lining, and the mixture is stirred by a glass rod for about 30 seconds, so that solid and liquid are fully mixed without deposition. And (3) placing the reaction kettle which is filled with the materials into a constant-temperature drying box for constant-temperature reaction for 30min, wherein the reaction temperature is 220 ℃, flushing and cooling the reaction kettle after the reaction is finished, collecting reaction mother liquor by using a dry suction bottle, wherein the reaction mother liquor can be used for circulating ingredients, then repeatedly washing a solid-phase product to be neutral by using deionized water, and placing a filter cake into the constant-temperature drying box for drying for 8h at the temperature of 105 ℃ to obtain a hydroxyl sodalite single-phase product with the purity of 90%.
Comparative example 1:
30g of 30% NaOH solution is prepared, 3g of raw material coal ash is weighed, the coal ash and the NaOH solution are sequentially added into a high-pressure reaction kettle with a polytetrafluoroethylene lining, and the mixture is stirred by a glass rod for about 30 seconds, so that solid and liquid are fully mixed without deposition. And (3) placing the reaction kettle which is filled with the materials into a constant-temperature drying box for constant-temperature reaction for 30min, wherein the reaction temperature is 210 ℃, flushing and cooling the reaction kettle after the reaction is finished, collecting reaction mother liquor by using a dry suction bottle, wherein the reaction mother liquor can be used for circulating ingredients, then repeatedly washing a solid-phase product to be neutral by using deionized water, and placing a filter cake into the constant-temperature drying box for drying for 8h at the temperature of 105 ℃ to obtain a hydroxysodalite product with the purity of 76%.
Comparative example 2:
preparing 30g of 20% NaOH solution, weighing 6g of raw material fly ash, sequentially adding the fly ash and the NaOH solution into a high-pressure reaction kettle with a polytetrafluoroethylene lining, and stirring for about 30 seconds by using a glass rod to fully mix solid and liquid without deposition. And (3) placing the reaction kettle which is filled with the materials into a constant-temperature drying box for constant-temperature reaction for 90min, wherein the reaction temperature is 230 ℃, flushing and cooling the reaction kettle after the reaction is finished, collecting reaction mother liquor by using a dry suction bottle, wherein the reaction mother liquor can be used for circulating ingredients, then repeatedly washing a solid-phase product to be neutral by using deionized water, and placing a filter cake into the constant-temperature drying box for drying for 12h at the temperature of 105 ℃ to obtain a hydroxysodalite single-phase product with the purity of 71%.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
Furthermore, it should be understood that although the present description refers to embodiments, not every embodiment may contain only a single embodiment, and such description is for clarity only, and those skilled in the art should integrate the description, and the embodiments may be combined as appropriate to form other embodiments understood by those skilled in the art.
Claims (8)
1. A method for preparing hydroxysodalite by using a fly ash sub-molten salt alkali hydrothermal method is characterized by comprising the following steps: the method comprises the steps of taking fly ash as a raw material and sodium hydroxide solution as a solvent, and synthesizing and preparing zeolite hydroxysodalite by a sub-molten salt system alkaline hydrothermal method, wherein a large amount of insoluble and inert substances in the fly ash are completely converted into hydroxysodalite, silicon-aluminum substances in the fly ash are fully utilized, silicate impurities are reduced, and the high-purity hydroxysodalite can be synthesized and prepared; the method comprises the following process steps: proportioning, carrying out hydrothermal reaction to obtain residue liquid, separating to obtain filter residue and mother liquor, carrying out suction filtration, washing and drying; the NaOH solution is 30-60% of NaOH solution in percentage by mass; the reaction temperature of the hydrothermal reaction is not lower than 220 ℃.
2. The method for preparing hydroxysodalite by using the fly ash sub-molten salt alkaline hydrothermal method according to claim 1, wherein the method comprises the following steps: the burdening steps are as follows: preparing 30-60 mass percent NaOH solution, weighing a certain mass of fly ash and the prepared solution, adding the fly ash and the prepared solution into a reaction kettle, and mixing, wherein the mass ratio of the prepared solution to the fly ash is more than 5.
3. The method for preparing hydroxysodalite by using the fly ash sub-molten salt alkaline hydrothermal method according to claim 2, wherein the method comprises the following steps: the mass ratio of the prepared solution to the fly ash is more than 10.
4. The method for preparing hydroxysodalite by using the fly ash sub-molten salt alkaline hydrothermal method according to claim 1, wherein the method comprises the following steps: the hydrothermal reaction comprises the following steps: the reaction is carried out in a high-temperature high-pressure reaction kettle, the reaction temperature is not lower than 220 ℃, and the reaction time is 60-120 min.
5. The method for preparing hydroxysodalite by using the fly ash sub-molten salt alkaline hydrothermal method according to claim 1, wherein the method comprises the following steps: the separation steps are as follows: and separating the residue and the liquid, and circularly using the mother liquid after being added with NaOH as the ingredient in the preparation method.
6. The method for preparing hydroxysodalite by using the fly ash sub-molten salt alkaline hydrothermal method according to claim 1, wherein the method comprises the following steps: and washing the filter residue for multiple times by using water to obtain a filter cake, and continuously adding NaOH into the washing liquid for circularly using the washing liquid as a material in the preparation method or recovering the NaOH by evaporation and crystallization.
7. The method for preparing hydroxysodalite by using the fly ash sub-molten salt alkaline hydrothermal method according to claim 1, wherein the method comprises the following steps: and washing the filter residue for multiple times by using deionized water to obtain a filter cake, and continuously adding NaOH into the washing liquid for circularly using the washing liquid as a material in the preparation method or recovering the NaOH by evaporation and crystallization.
8. The method for preparing hydroxysodalite by using the fly ash sub-molten salt alkaline hydrothermal method according to claim 7, wherein the method comprises the following steps: the drying step is as follows: and drying the obtained filter cake at 90-120 ℃ for 6-24 h to obtain the synthetic product, namely the hydroxysodalite.
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