CN112875718A - Method for preparing molecular sieve with high silica-alumina ratio based on biomass ash activated fly ash - Google Patents
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Abstract
The invention relates to a method for preparing a molecular sieve with high silica-alumina ratio based on biomass ash activated fly ash. The method recycles silicon oxide and aluminum oxide in the coal-fired power plant fly ash, silicon oxide in biomass ash and the like, solves the problem of low silicon-aluminum ratio of the molecular sieve synthesized by the traditional method, improves the quality and the yield of the molecular sieve, can adjust the silicon and aluminum of the molecular sieve produced by the method, and provides a new thought for the synergistic treatment of various industrial solid wastes with high quality and low cost.
Description
Technical Field
The invention belongs to the technical field of comprehensive resource utilization of byproduct coal ash and biomass ash generated by biomass combustion in the coal-fired power generation industry, and particularly relates to a method for preparing a molecular sieve with a high silica-alumina ratio based on activated coal ash of biomass ash.
Background
Zeolite is a substance existing in nature and having the functions of molecular sieving, adsorption, ion exchange and catalysis, and artificially synthesized zeolite, also called molecular sieve, is a type of aluminosilicate with a framework structure formed from TO4Crystalline materials having a three-dimensional framework structure of tetrahedra sharing apical oxygen atoms for connection, wherein the T atom is usually a Si, Al or P atom, but may be other atoms substituted for Si, Al or P. The framework space structure of the molecular sieve is filled with open regular pore canals and cavities, and has a huge internal surface area, so the molecular sieve is named because of the capability of sieving molecules. Zeolite molecular sieve has been used as the main catalytic material, adsorptive separation, for nearly half a centuryThe material and the ion exchange material play more and more important roles in the industries of petroleum processing, petrochemical industry, fine chemical industry and daily chemical industry.
The fly ash is a mixture consisting of oxides and silicate minerals obtained by burning inorganic mineral substances in coal, is a byproduct of a coal-fired power plant, and has a phase mainly comprising a vitreous body accounting for 50-80%. Because the yield of the fly ash is large and the yield is increased every year, a large amount of fly ash is accumulated to be treated urgently. The fly ash contains a large amount of SiO2And Al2O3And a small amount of Fe2O3CaO, MgO, unburned carbon and the like, and are commonly used in industries of industrial aluminum extraction, soil improvement, blended concrete, adsorbent improvement and the like. The mass ratio of the main chemical components in the fly ash can be expressed by the following empirical formula:
Si1.0Al0.45Ca0.51Na0.047Fe0.039Mg0.020K0.013Ti0.011
the research of synthesizing the zeolite molecular sieve by using the fly ash has been over 30 years, and many scientists adopt different process methods to research the zeolite molecular sieve, so that the development of the research of preparing the zeolite molecular sieve by using the fly ash is promoted.
The biomass ash generally refers to lignocellulose such as straws and trees except grains and fruits generated in agriculture and forestry, agricultural and forestry wastes, livestock and poultry manure and wastes in animal husbandry and the like which are remained after combustion, and has the characteristics of difficult regeneration, low pollution and wide distribution. The biomass ash from different sources has different components, and the main component is SiO2、CaO、K2And O and the like, which are subjected to targeted treatment by analyzing the components of the biomass ash, so that the resource utilization can be performed to the maximum extent.
Disclosure of Invention
In order to comprehensively solve the problem of resource treatment of the fly ash and the biomass ash, the invention provides a method for preparing a molecular sieve with a high silica-alumina ratio based on activated fly ash of biomass ash, wherein a proper amount of biomass ash is added into the fly ash to improve the problem of low silica-alumina ratio of the molecular sieve synthesized by the traditional fly ash, improve the quality and yield of the molecular sieve and provide a new way for the synergistic treatment and utilization of various industrial solid wastes.
In order to achieve the purpose, the invention adopts the following technical scheme:
a method for preparing a molecular sieve with a high silica-alumina ratio based on biomass ash activated fly ash comprises the steps of crushing and mixing raw material fly ash and biomass ash, and performing acid leaching, solid alkali fusion or alkali liquor activation and hydrothermal reaction to obtain a molecular sieve product.
Preferably, the method for preparing the molecular sieve with high silica-alumina ratio based on the biomass ash activated fly ash comprises the following steps:
(1) crushing and mixing raw materials: proportioning the fly ash and the biomass ash according to a proportion, crushing the mixture and uniformly mixing;
(2) acid leaching: mixing the mixed product with hydrochloric acid, continuously stirring uniformly, reacting at 80-100 ℃, separating, washing and drying to obtain acid leaching fly ash;
(3) solid alkali melting: placing the acid-leaching fly ash and alkali in a crucible to be melted at the temperature of 500-1000 ℃, and dissolving, filtering and washing the obtained product to obtain an extracting solution;
(4) hydrothermal reaction: and concentrating the extracting solution, placing the extracting solution into a hydrothermal reaction kettle, reacting at the temperature of 70-150 ℃, and separating, washing and drying to obtain a molecular sieve crystal product.
Preferably, the method for preparing the molecular sieve with high silica-alumina ratio based on the biomass ash activated fly ash comprises the following steps:
(1) crushing and mixing raw materials: proportioning the fly ash and the biomass ash according to a proportion, crushing the mixture and uniformly mixing;
(2) acid leaching: mixing the mixed product with hydrochloric acid, continuously stirring uniformly, reacting at 80-100 ℃, separating, washing and drying to obtain acid leaching fly ash;
(3) alkali liquor activation: adding acid-leaching fly ash into alkali liquor, mixing, stirring and aging;
(4) hydrothermal reaction: and placing the aged mixed solution into a hydrothermal reaction kettle, reacting at the temperature of 70-150 ℃, and separating, washing and drying to obtain a molecular sieve crystal product.
Preferably, the biomass ash is one or any combination of more than two of wheat straw ash, rice hull ash and rice straw ash.
Preferably, the alkali is NaOH or Na2CO3、Ca(OH)2Or KOH.
Preferably, the raw materials are crushed, mixed and sieved, and the particle size of the mixed product is controlled to be below 200 meshes.
Preferably, the mass concentration of the hydrochloric acid in the step (2) is 10-25%, and the liquid-solid ratio of the hydrochloric acid to the mixed product is 15-20.
Preferably, the alkali ash ratio of the alkali to the acid leaching fly ash in the step (3) is 1-2.
Preferably, the liquid-solid ratio of the alkali liquor to the acid leaching fly ash is 4-8.
Preferably, the hydrothermal reaction time in the step (4) is 6-48 h.
The invention has the beneficial effects that:
1. the biomass ash is solid waste residue generated in biomass combustion, contains more Si elements, is used for improving the Si content in the molecular sieve, optimizing the structure of the molecular sieve, reducing the production cost and realizing the resource utilization of the biomass ash;
2. in the process, silicon source and aluminum source chemicals are not additionally added, so that the cost is reduced;
3. the method has simple production process, the produced molecular sieve product has higher silica-alumina ratio, and the molecular sieve products with different silica-alumina ratios are obtained by adjusting the addition amount of the biomass ash, so the method is an economic and efficient resource utilization mode.
Drawings
FIG. 1 is a process flow diagram of the present invention;
FIG. 2 is a SEM spectrum of fly ash;
FIG. 3 is a SEM spectrogram of a molecular sieve with Si/Al of 4 prepared from rice hull ash activated fly ash by an alkali fusion method;
FIG. 4 is an XRD spectrum of molecular sieves prepared by different alkali concentrations in the alkali activation method.
Detailed Description
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the present invention is further described with reference to the drawings and the embodiments, but the protection scope of the present invention is not limited thereto. In the following description, numerous specific details are set forth in order to provide a more thorough understanding of the present invention. It will be apparent, however, to one skilled in the art, that the present invention may be practiced without one or more of these specific details. It is to be understood that the practice of the invention is not limited to the following examples, and that any variations and/or modifications may be made thereto without departing from the scope of the invention.
Referring to fig. 1, the method for preparing the molecular sieve with high silica-alumina ratio based on the biomass ash activated fly ash comprises the following process flows: the molecular sieve product is obtained by carrying out acid leaching, solid alkali fusion or alkali liquor activation and hydrothermal reaction on the pulverized and mixed raw material fly ash and biomass ash (raw material pulverization and mixing).
Example 1
Preparation of rice hull ash activated fly ash based molecular sieve by alkali fusion method
The coal ash raw material sample is from a power plant at Zhejiang, the rice hull ash in the biomass ash is taken as a regulating raw material, and the chemical compositions of the coal ash and the biomass ash sample are shown in Table 1.
TABLE 1
| Sample (I) | SiO2 | Al2O3 | CaO | Fe2O3 | TiO2 | Na2O | Others | Si/Al |
| Fly ash | 44.7 | 26.2 | 10.4 | 8.97 | 2.41 | 0.76 | 6.56 | 1.44 |
| Rice hull ash | 95.8 | 0.1 | 1.1 | 0.1 | - | 2.3 | 2.5 | ∞ |
The raw materials were treated by the process shown in fig. 1, taking 50g of fly ash and 200g of rice hull ash, pulverizing them into powder by a pulverizer, and mixing them uniformly. After sieving, 50g of the mixture is weighed and mixed with 1000mL of hydrochloric acid with the mass concentration of 10% (liquid-solid ratio is 20), the temperature is raised to 85 ℃ for reaction for 2h, and the acid leaching fly ash is obtained after separation, washing and drying. 20.00g of acid-leaching fly ash and 21.79g of NaOH (the alkali-ash ratio is 1.2) are put in a crucible to be uniformly mixed, the mixture is melted at the temperature of 850 ℃, the obtained product is dissolved, filtered and washed to obtain an extracting solution, the silicon-aluminum ratio in the extracting solution is increased to 11.5 by ICP (inductively coupled plasma), and the content of other impurity ions is obviously reduced.
Concentrating the extracting solution to 60mL, placing the extracting solution in an 80L hydrothermal reaction kettle, reacting for 12h at the temperature of 90 ℃, separating, washing and drying at the temperature of 80 ℃ to obtain a molecular sieve crystallization sample, and determining that the silicon-aluminum ratio in the obtained molecular sieve is 10 by adopting an X-ray fluorescence spectrum analyzer (American Saimerle Feishale, XRF-ADVANT' X4200 type), the difference with the silicon-aluminum ratio in the extracting solution is not large, and the silicon-aluminum ratio is obviously improved compared with that in the traditional method.
Example 2
Preparation of rice hull ash activated fly ash based molecular sieve by alkali fusion method
The composition of fly ash and rice hull ash used in this example was the same as example 1, and the raw materials were treated by the process shown in fig. 1, and 200g of fly ash and 200g of rice hull ash were taken, pulverized into powder by a pulverizer, and mixed uniformly. And (3) after sieving, mixing 20g of the mixture with 400mL of hydrochloric acid with the mass concentration of 15% (liquid-solid ratio is 20), heating to 100 ℃, reacting for 2h, separating, washing and drying to obtain the acid leaching fly ash. 10.00g of acid-leaching fly ash and 10.89g of NaOH (the alkali-ash ratio is 1.2) are put in a crucible to be uniformly mixed, the mixture is melted at the temperature of 550 ℃, the obtained product is dissolved, filtered and washed to obtain an extracting solution, and the silicon-aluminum ratio in the extracting solution is 4 measured by adopting ICP. Concentrating the extracting solution to 60mL under the heating condition, placing the extracting solution in an 80L hydrothermal reaction kettle, reacting for 12h at the temperature of 90 ℃, separating and washing, drying at the temperature of 80 ℃ to obtain a molecular sieve crystal sample, and measuring by adopting XRF (X-ray fluorescence) to obtain the molecular sieve with the silicon-aluminum ratio of 3.5 which is not different from the silicon-aluminum ratio of the extracting solution.
A scanning electron microscope (SEM-SU-8010 model, Hitachi, Japan) is adopted to observe the appearance and the granularity of a sample, the sample needs to be uniformly dispersed on conductive adhesive and subjected to gold spraying treatment before being tested, the SEM spectrogram of fly ash is shown in figure 2, the SEM spectrogram of a molecular sieve with the Si/Al content of 4 for preparing the rice hull ash activated fly ash by an alkali fusion method is shown in figure 3, and the prepared zeolite product can be seen to be in a square shape, a prism shape and an irregular shape.
Example 3
Preparation of rice hull ash activated fly ash based molecular sieve by alkali liquor activation method
The composition of fly ash and rice hull ash used in this example was the same as example 1, and the raw materials were treated by the process shown in fig. 1, and 200g of fly ash and 200g of rice hull ash were taken, pulverized into powder by a pulverizer, and mixed uniformly. And (3) after sieving, mixing 20g of the mixture with 400mL of hydrochloric acid with the mass concentration of 15% (liquid-solid ratio is 20), heating to 100 ℃, reacting for 2h, separating, washing and drying to obtain the acid leaching fly ash. Accurately weighing 5g of acid-leaching fly ash, respectively adding the acid-leaching fly ash into a prepared sodium hydroxide solution according to a liquid-solid ratio of 6, mixing, stirring and aging for 24h, placing the mixture into a hydrothermal reaction kettle, sealing, carrying out hydrothermal reaction for 12h at 120 ℃, cooling, carrying out centrifugal separation, washing for multiple times until the pH value is 9-10, drying in a drying oven at 105 ℃, and grinding to obtain a sample.
The silicon-aluminum ratio of the molecular sieve obtained by adopting the X-ray fluorescence spectrum analyzer is about 7, and is improved to a certain extent compared with the silicon-aluminum ratio of the traditional method.
Example 4
Influence of alkali liquor concentration on characteristics of fly ash-based molecular sieve activated by rice hull ash prepared by alkali liquor activation method
The composition of fly ash and rice hull ash used in this example was the same as example 1, and the raw materials were treated by the process shown in fig. 1, taking 100g of fly ash and 200g of rice hull ash, pulverizing them into powder by a pulverizer, and mixing them uniformly. And mixing 50g of the mixture with 1000mL of hydrochloric acid with the mass concentration of 10% (liquid-solid ratio is 20), heating to 100 ℃, reacting for 2h, separating, washing and drying to obtain the acid leaching fly ash. Accurately weighing 5g of acid leaching fly ash, and respectively adding 2 mol. L according to the liquid-solid ratio of 6-1、2.5mol·L-1、3mol·L-1、4mol·L-1Mixing the sodium hydroxide solution, stirring and aging for 24h, sealing the mixture in a hydrothermal reaction kettle, carrying out hydrothermal reaction for 48h at the temperature of 95 ℃, cooling, carrying out centrifugal separation, washing for multiple times until the pH value is 9-10, and carrying out hydrothermal reaction on the mixtureDrying at 105 ℃ in a drying oven, and grinding to obtain a sample.
The crystal phase analysis was carried out using an X-ray diffractometer (Japan science, XRD-Rigaku Smart Lab (3KW) type) under the following detection conditions: cu target, Ka diffraction source, tube voltage 40kV, tube current 40mA, scanning speed 8 degree min-1And the angle range is 5-60 degrees (data are processed by using Jade 6.5 software), an XRD spectrogram of the molecular sieve prepared by different alkali liquor concentrations in the alkali liquor activation method is shown in figure 4, and the obtained results of the influence of the alkali liquor concentration on the phase characteristics of the molecular sieve are shown in Table 2.
TABLE 2
| Alkali liquor concentration (mol. L)-1) | Hydrothermal temperature (. degree.C.) | Relative crystallinity (%) | Composition of crystalline phase |
| 2 | 95 | -- | M+Q |
| 2.5 | 95 | 3.7 | M+Q+P |
| 3 | 95 | 74.9 | M+Q+P |
| 4 | 95 | 20.1 | M+Q+P+C+X |
Note: m-mullite, Q-quartz, C-chabazite, P-P type zeolite, X-X type zeolite
It can be seen from fig. 4 and table 2 that the alkali concentration has a great influence on the zeolite crystal form synthesized. At 2.0 mol. L-1The NaOH solution of (1) was only quartz and mullite in the product. The concentration of NaOH reaches 2.5 mol.L-1When the method is compared with a Powder Diffraction File (PDF) card in a standard database, a characteristic peak of NaP type zeolite (PDF 44-0052) appears, and the molecular formula is Na3.6Al3.6Si12.4O32·14H2O, the relative crystallinity of zeolite is very low, only 3.7%. When the concentration reaches 3.0 mol.L-1When the product is used, the peak of the P-type zeolite is strongest, the characteristic peaks are respectively 12.4 degrees, 17.6 degrees, 21.6 degrees and 33.3 degrees, the strongest peak is 28.1 degrees, and the relative crystallinity is improved to 74.9 percent. However, when the alkali concentration reaches 4 mol. L-1In this case, other phases such as X-type zeolite and chabazite start to be formed, and the relative crystallinity of P-type zeolite decreases to 20.1%.
The method recycles silicon oxide and aluminum oxide in the coal-fired power plant fly ash, silicon oxide in biomass ash and the like, solves the problem of low silicon-aluminum ratio of the molecular sieve synthesized by the traditional method, improves the quality and the yield of the molecular sieve, can adjust the silicon and aluminum of the molecular sieve produced by the method, and provides a new thought for the synergistic treatment of various industrial solid wastes with high quality and low cost.
The present invention is described in detail with reference to the examples, but the description is only a specific embodiment of the present invention, and the present invention is not to be construed as being limited to the claims. It should be noted that, for those skilled in the art, variations and modifications made within the scope of the present invention shall fall within the scope of the claims of the present invention without departing from the spirit of the present invention.
Claims (10)
1. A method for preparing a molecular sieve with a high silica-alumina ratio based on biomass ash activated fly ash is characterized by comprising the following steps: the raw materials of fly ash and biomass ash are crushed and mixed, and then are subjected to acid leaching, solid alkali fusion or alkali liquor activation and hydrothermal reaction to obtain a molecular sieve product.
2. The method for preparing the molecular sieve with high silica-alumina ratio based on the biomass ash activated fly ash as claimed in claim 1, which is characterized by comprising the following steps:
(1) crushing and mixing raw materials: proportioning the fly ash and the biomass ash according to a proportion, crushing the mixture and uniformly mixing;
(2) acid leaching: mixing the mixed product with hydrochloric acid, continuously stirring uniformly, reacting at 80-100 ℃, separating, washing and drying to obtain acid leaching fly ash;
(3) solid alkali melting: grinding and mixing acid-leaching fly ash and alkali, placing the mixture in a crucible, melting the mixture at the temperature of 500-1000 ℃, and dissolving, filtering and washing the obtained product to obtain an extracting solution;
(4) hydrothermal reaction: and concentrating the extracting solution, placing the extracting solution into a hydrothermal reaction kettle, reacting at the temperature of 70-150 ℃, and separating, washing and drying to obtain a molecular sieve crystal product.
3. The method for preparing the molecular sieve with high silica-alumina ratio based on the biomass ash activated fly ash as claimed in claim 1, which is characterized by comprising the following steps:
(1) crushing and mixing raw materials: proportioning the fly ash and the biomass ash according to a proportion, crushing the mixture and uniformly mixing;
(2) acid leaching: mixing the mixed product with hydrochloric acid, continuously stirring uniformly, reacting at 80-100 ℃, separating, washing and drying to obtain acid leaching fly ash;
(3) alkali liquor activation: adding acid-leaching fly ash into alkali liquor, mixing, stirring and aging;
(4) hydrothermal reaction: and placing the aged mixed solution into a hydrothermal reaction kettle, reacting at the temperature of 70-150 ℃, and separating, washing and drying to obtain a molecular sieve crystal product.
4. The method for preparing the molecular sieve with high silica-alumina ratio based on the biomass ash activated fly ash as claimed in claim 1, wherein the method comprises the following steps: the biomass ash is one or more of wheat straw ash, rice hull ash and rice straw ash in any combination.
5. The method for preparing the molecular sieve with high silica-alumina ratio based on the biomass ash activated fly ash as claimed in claim 1, wherein the method comprises the following steps: the alkali is NaOH or Na2CO3、Ca(OH)2Or KOH.
6. The method for preparing the molecular sieve with high silica-alumina ratio based on the biomass ash activated fly ash as claimed in claim 2 or 3, wherein the method comprises the following steps: the raw materials are crushed and mixed, and then the granularity of the mixed product is controlled below 200 meshes after the raw materials are sieved.
7. The method for preparing the molecular sieve with high silica-alumina ratio based on the biomass ash activated fly ash as claimed in claim 2 or 3, wherein the method comprises the following steps: in the step (2), the mass concentration of the hydrochloric acid is 10-25%, and the liquid-solid ratio of the hydrochloric acid to the mixed product is 15-20.
8. The method for preparing the molecular sieve with high silica-alumina ratio based on the biomass ash activated fly ash as claimed in claim 2, wherein the method comprises the following steps: and (4) the alkali ash ratio of the alkali to the acid leaching fly ash in the step (3) is 1-2.
9. The method for preparing the molecular sieve with high silica-alumina ratio based on the biomass ash activated fly ash as claimed in claim 3, wherein the method comprises the following steps: the liquid-solid ratio of the alkali liquor to the acid leaching fly ash is 4-8.
10. The method for preparing the molecular sieve with high silica-alumina ratio based on the biomass ash activated fly ash as claimed in claim 2 or 3, wherein the method comprises the following steps: the hydrothermal reaction time in the step (4) is 6-48 h.
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