CN113428874A - Preparation method and application method of gangue-based sodium ion type molecular sieve based on alkali fusion method - Google Patents
Preparation method and application method of gangue-based sodium ion type molecular sieve based on alkali fusion method Download PDFInfo
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Abstract
The invention relates to a preparation method and an application method of a gangue-based sodium ion type molecular sieve based on an alkali fusion method, wherein the gangue without heavy metal pollution and sodium hydroxide in Ordos areas are mainly utilized, the gangue is subjected to alkali fusion method steps such as pretreatment, alkali fusion, aging, crystallization, water washing and drying and the like on the premise of not adding a silicon-aluminum source to prepare the gangue-based sodium ion type molecular sieve, the molecular sieve has an octahedral crystal structure, a large specific surface area and a large pore volume, and has high adsorption capacity and adsorption effect on heavy metals, the adsorption test on Cd (II) and Cu (II) is verified, the adsorption rates of the Cd (II) and the Cu (II) can reach more than 90%, an important basis is provided for preparing the molecular sieve by utilizing the gangue, and an important approach is provided for comprehensive utilization of the gangue.
Description
Technical Field
The invention relates to a preparation method and an application method of a gangue-based sodium ion type molecular sieve based on an alkali fusion method, and belongs to the technical field of gangue resource utilization technology and water treatment materials.
Background
The coal gangue is solid waste generated in the coal mining and washing processes, is a black gray rock which has lower carbon content and is harder than coal and is associated with a coal bed in the coal forming process, and the mineral components of the coal gangue mainly comprise kaolin, quartz, montmorillonite, feldspar, illite, limestone and the like; the main chemical component of the alloy is Al2O3、SiO2And in addition a small amount of Fe2O3CaO and trace rare elements. The traditional utilization mode of the coal gangue mainly comprises heat value recovery, building materials and backfill engineering, wherein two ways with the largest scale are coal gangue energy regeneration and building materials; therefore, the high value-added utilization is an important supplement for the comprehensive utilization of the coal gangue and becomes a development direction of the comprehensive utilization of the coal gangue.
In all development directions, the sodium ion type molecular sieve is a material with an eight-face type crystal structure, and has one of the best adsorbents which are widely applied to removing heavy metal ions in the aspect of heavy metal adsorption of water treatment as an adsorption material. In addition, it is also possible to use CH4、CO2The gas is adsorbed, and meanwhile, the catalyst is used as a main component of a cracking catalyst in the petroleum refining industry, and the like, so that the catalyst has wide application prospect; the alkali fusion method is common in the preparation method for obtaining the sodium ion type molecular sieve, but the existing molecular sieve prepared by the alkali fusion method has high preparation cost and cannot obtain satisfactory adsorption effect, so that the development of a preparation method for preparing the sodium ion type molecular sieve is urgently needed to meet the actual requirement.
Disclosure of Invention
The invention provides a preparation method and an application method of a gangue-based sodium ion type molecular sieve based on an alkali fusion method.
The technical scheme adopted by the invention for solving the technical problems is as follows:
a preparation method of a coal gangue based sodium ion type molecular sieve based on an alkali fusion method comprises the following steps:
firstly, washing the coal gangue subjected to pretreatment and screening, removing surface dust and soil, screening, and then crushing to form coal gangue powder;
secondly, adding NaOH into the coal gangue powder for uniform mixing;
thirdly, the formed mixture is placed in a muffle furnace and heated to obtain a blue-green alkali fusion product;
fourthly, aging the obtained blue-green alkali fusion product to form a gel product;
fifthly, putting the gel product into a reaction kettle with a polytetrafluoroethylene lining, and crystallizing to obtain a crystallized product;
sixthly, filtering the crystallized product, washing the crystallized product by using deionized water, and drying the washed product to prepare the coal gangue-based sodium ion type molecular sieve;
as a further optimization of the invention, in the first step, the mixture ratio of the mass parts of the raw materials in the screened coal gangue is Na2O:Al2O3:SiO2:H2O＝3.5:1:2.9:150；
Sieving the coal gangue with a 100-mesh sieve before crushing;
as a further preference of the invention, in the second step, the mass fraction ratio of the NaOH and the gangue powder is 1: 1;
as a further preference of the present invention, in the third step, the mixture is put into a muffle furnace, heated at 800 ℃ for 2 hours;
as a further preferable aspect of the present invention, in the fourth step, the time for aging the alkali fusion product is 6 hours;
as a further preferable aspect of the present invention, in the fifth step, the temperature in the reaction vessel is set to 100 ℃, and the reaction time is continued for 10 hours;
an application method of a gangue-based sodium ion type molecular sieve prepared by a gangue-based sodium ion type molecular sieve preparation method based on an alkali fusion method comprises the steps of adding 2g/L of the obtained gangue-based sodium ion type molecular sieve at the adsorption temperature of room temperature, adsorbing two heavy metal ions of Cd (II) and Cu (II) with the initial PH of 5, wherein the adsorption rate reaches 90% when the concentrations of the two heavy metal ions are 100mg/L, and obtaining the adsorption capacity of the two heavy metal ions respectively reaching 100.11mg g/g through an adsorption isothermal model-1And 95.29mg g-1。
Through the technical scheme, compared with the prior art, the invention has the following beneficial effects:
1. the sodium ion type molecular sieve prepared by the preparation method provided by the invention has an octahedral crystal structure and also has a large specific surface area and a large pore volume, so that the molecular sieve has high stability and a good adsorption effect;
2. according to the method, the coal gangue powder obtained through pretreatment can meet the requirement of preparing the molecular sieve without adding a silica-alumina source in the preparation process, and the production cost is reduced.
Drawings
The invention is further illustrated with reference to the following figures and examples.
FIG. 1 is an XRD pattern of a gangue-based sodium ion type molecular sieve prepared by the invention;
FIGS. 2 a-2 b are SEM images of the gangue-based Na-ion molecular sieve prepared by the method, wherein FIG. 2a is a product magnification of 5 times, and FIG. 2b is a product magnification of 10 times;
FIG. 3 is an FTIR diagram of a coal gangue-based Na-ion molecular sieve prepared by the present invention;
FIG. 4a is a drawing of Cd (II) absorption of the gangue-based sodium-ion molecular sieve prepared by the invention, and FIG. 4b is a drawing of Cu (II) absorption of the gangue-based sodium-ion molecular sieve;
FIG. 5a is a fitting curve of Cd (II) isothermal adsorption of the gangue-based Na-ion molecular sieve prepared by the method, and FIG. 5b is a fitting curve of Cu (II) isothermal adsorption of the gangue-based Na-ion molecular sieve.
Detailed Description
The existing preparation method of the sodium ion type molecular sieve mainly comprises a hydrothermal synthesis method, an alkali fusion method, a microwave synthesis method, a seed crystal synthesis method and the like, wherein the alkali fusion method is to mix a raw material and alkali and then calcine and heat the mixture, and to activate substances such as quartz, kaolinite and the like with stable structures in the raw material at high temperature, so that the defects of low purity and low yield of the molecular sieve product caused by difficult dissolution of crystal components in the traditional hydrothermal method are overcome, and meanwhile, the high-temperature roasting can burn off carbon in coal gangue, activate inert components in the raw material and improve the purity of the zeolite product; therefore, the method is widely applied, but in the prior art, most of the sodium ion type molecular sieves obtained by an alkali fusion method cannot achieve the optimal adsorption effect, and the preparation cost is high.
Based on the problems stated above, the application aims to provide a preparation method of a coal gangue-based sodium-ion type molecular sieve based on an alkali fusion method, so that the prepared sodium-ion type molecular sieve has a large specific surface area and a good adsorption effect; the method specifically comprises the following steps:
firstly, washing coal gangue, removing impurities such as surface dust, soil and the like, sieving, and then crushing to form coal gangue powder; it is to be noted that the coal gangue used in the present application is coal gangue located in the Ore region, and the raw material of the coal gangue is SiO in the ore component2With Al2O3The molar ratio of the compound is close to 2.9, the compound conforms to the range of the silicon-aluminum ratio of the prepared X molecular sieve, and simultaneously, the requirement of preparing the molecular sieve can be met without adding a silicon-aluminum source in the preparation process, so that the production cost is reduced; after a plurality of experiments, the proportion of the specific raw materials in parts by mass is Na in order to obtain the best adsorption effect2O:Al2O3:SiO2:H2O＝3.5:1:2.9:150；
Before the coal gangue is crushed for use, the impurities such as surface dust and soil are removed, and the coal gangue is treated byThe purpose of the 100-mesh sieve is to ensure SiO in the coal gangue2And Al2O3The total ratio is more than 90%.
And secondly, adding NaOH into the coal gangue powder for uniform mixing, wherein the mass fraction ratio of the NaOH to the coal gangue powder is 1: 1.
And thirdly, putting the formed mixture into a muffle furnace, and heating at 800 ℃ for 2 hours (air atmosphere) to obtain a blue-green alkali fusion product.
And fourthly, standing the obtained blue-green alkali fusion product, and aging the product for 6 hours to ensure that the alkali fusion product gradually forms a silicon-aluminum gel product in order to accelerate disordered ions in the product to be converted into an ordered state as soon as possible and ensure the crystallization process.
And fifthly, placing the aged gel product into a reaction kettle with a polytetrafluoroethylene lining for crystallization, ensuring the effectiveness of the crystallization process and the stability and purity of the generated crystal substance according to the mutual influence relationship between crystallization temperature and time, strengthening and enhancing the characteristic peak of the crystal, setting the temperature of the reaction kettle to be 100 ℃ in the crystallization process, and keeping the reaction time for 10 hours, thereby effectively promoting the formation and growth of the crystal.
And sixthly, after the crystallization process is finished, filtering the crystallized product, washing the crystallized product by using deionized water, and drying the washed product to prepare the coal gangue-based sodium ion type molecular sieve.
In order to verify that the molecular sieve prepared by the method can achieve the expected adsorption effect, the application carries out experimental verification, and the prepared molecular sieve is firstly subjected to X-ray powder diffraction (XRD) measurement, so that the molecular sieve has diffraction characteristic peaks of Faujasite (FAU) which are obvious as shown in figure 1 in the attachments of 2 theta of 6.14 degrees, 10.04 degrees, 15.48 degrees, 23.38 degrees, 26.74 degrees, 31.04 degrees and the like.
As can be seen from the SEM scanning images given in fig. 2 a-2 b, the product is magnified 5 times in fig. 2a and 10 times in fig. 2b, and the molecular sieve is found to be an octahedral structure with uniform particles and complete structure, and the size of the octahedral structure is about 2 μm.
From the FTIR chart (infrared spectrum) given in FIG. 3, it was found that the peak values were found at 567, 673, 754, 1024. 1644 and 3462cm-1A characteristic band of a double six-membered ring, TO, respectively appears in the vicinity of the iso4Tetrahedral external and internal connection symmetric stretching vibration band, TO4The internal connection and the external connection of the tetrahedron are antisymmetric telescopic vibration bands, valence bond vibration absorption peaks of physically adsorbed water, distortion vibration absorption peaks of physically adsorbed water and the like, and are characteristic bands and framework structures of typical sodium ion type molecular sieves.
As can be seen from the BET specific surface area test method, the molecular sieve has an octahedral crystal structure, and the specific surface area of the molecular sieve is 406.7m2Per g, pore volume 0.242m3/g。
Then, preparing Cd (II) and Cu (II) simulated wastewater solutions with different concentrations by adopting hydrated cadmium nitrate and hydrated copper sulfate aiming at the obtained molecular sieve, and then performing simulated adsorption tests by using the molecular sieves with different adding amounts and at different temperatures;
firstly, setting experiment conditions, wherein the adsorption temperature is room temperature, the adding amount of the obtained coal gangue based sodium ion type molecular sieve is 2g/L, the initial PH of the wastewater is 5, and the obtained coal gangue based sodium ion type molecular sieve adsorbs two heavy metal ions, namely Cd (II), FIG. 4a is an adsorption diagram of Cd (II), FIG. 4b is an adsorption diagram of Cu (II), and as can be seen from FIGS. 4 a-4 b, the best adsorption rate effect can reach 90% when the concentration of the two heavy metal ions is 100 mg/L; finally, as can be seen from FIGS. 5a to 5b, the maximum adsorption capacities of the molecular sieve prepared by the method for Cd (II) and Cu (II) respectively reach 100.11mg g by the adsorption kinetic analysis of the Langmuir adsorption isothermal model-1And 95.29mg g-1。
In conclusion, multiple researches show that the sodium ion type molecular sieve prepared by the alkali fusion method has large specific surface area and good adsorption effect, and is particularly obvious for heavy metal ions in sewage and wastewater.
It will be understood by those skilled in the art that, unless otherwise defined, all terms (including technical and scientific terms) used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs. It will be further understood that terms, such as those defined in commonly used dictionaries, should be interpreted as having a meaning that is consistent with their meaning in the context of the prior art and will not be interpreted in an idealized or overly formal sense unless expressly so defined herein.
The meaning of "and/or" as used herein is intended to include both the individual components or both.
The term "connected" as used herein may mean either a direct connection between components or an indirect connection between components via other components.
In light of the foregoing description of the preferred embodiment of the present invention, many modifications and variations will be apparent to those skilled in the art without departing from the spirit and scope of the invention. The technical scope of the present invention is not limited to the content of the specification, and must be determined according to the scope of the claims.
Claims (7)
1. A coal gangue based sodium ion type molecular sieve preparation method based on an alkali fusion method is characterized in that: the method comprises the following steps:
firstly, washing the coal gangue subjected to pretreatment and screening, removing surface dust and soil, screening, and then crushing to form coal gangue powder;
secondly, adding NaOH into the coal gangue powder for uniform mixing;
thirdly, the formed mixture is placed in a muffle furnace and heated to obtain a blue-green alkali fusion product;
fourthly, aging the obtained blue-green alkali fusion product to form a gel product;
fifthly, putting the gel product into a reaction kettle with a polytetrafluoroethylene lining, and crystallizing to obtain a crystallized product;
and sixthly, filtering the crystallized product, washing the crystallized product by using deionized water, and drying the washed product to prepare the coal gangue-based sodium ion type molecular sieve.
2. The alkali fusion process-based sodium ion type coal gangue fraction as set forth in claim 1The preparation method of the subsieve is characterized in that: in the first step, the mass part ratio of the raw materials in the screened coal gangue is Na2O:Al2O3:SiO2:H2O＝3.5:1:2.9:150；
Sieving with 100 mesh sieve before pulverizing coal gangue.
3. The method for preparing the coal gangue-based sodium ion type molecular sieve based on the alkali fusion method according to claim 1, which is characterized in that: in the second step, the mass fraction ratio of NaOH and gangue powder is 1: 1.
4. The method for preparing the coal gangue-based sodium ion type molecular sieve based on the alkali fusion method according to claim 1, which is characterized in that: in the third step, the mixture was placed in a muffle furnace at a heating temperature of 800 ℃ for a duration of 2 hours.
5. The method for preparing the coal gangue-based sodium ion type molecular sieve based on the alkali fusion method according to claim 1, which is characterized in that: in the fourth step, the time for aging the alkali fusion product is 6 hours.
6. The method for preparing the coal gangue-based sodium ion type molecular sieve based on the alkali fusion method according to claim 1, which is characterized in that: in the fifth step, the temperature in the reaction vessel was set to 100 ℃ and the reaction time was continued for 10 hours.
7. An application method of a gangue-based sodium ion type molecular sieve prepared by a preparation method of the gangue-based sodium ion type molecular sieve based on an alkali fusion method is characterized by comprising the following steps: under the condition that the adsorption temperature is room temperature, the adding amount of the coal gangue-based sodium ion type molecular sieve obtained in the claims 1 to 6 is 2g/L, the initial PH of the wastewater is 5, two heavy metal ions of Cd (II) and Cu (II) are adsorbed, the adsorption rate reaches 90% when the concentration of the two heavy metal ions is 100mg/L, and the adsorption capacities of the two heavy metal ions respectively reach 100.11 mg-g obtained by an adsorption isothermal model-1And 95.29mg g-1。
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Cited By (3)
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| 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 |
| CN115583688A (en) * | 2022-01-19 | 2023-01-10 | 河南理工大学 | Spiral fluidization continuous adsorption device and method based on coal gangue-based molecular sieve |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115583688A (en) * | 2022-01-19 | 2023-01-10 | 河南理工大学 | Spiral fluidization continuous adsorption device and method based on coal gangue-based molecular sieve |
| CN115583688B (en) * | 2022-01-19 | 2024-08-16 | 河南理工大学 | Spiral fluidization continuous adsorption device and method based on gangue-based molecular sieve |
| 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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