CN114988426A - Coal gangue-based molecular sieve and alkali fusion-hydrothermal preparation method thereof - Google Patents
Coal gangue-based molecular sieve and alkali fusion-hydrothermal preparation method thereof Download PDFInfo
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Abstract
The invention provides a coal gangue-based molecular sieve and an alkali fusion-hydrothermal preparation method thereof, wherein the preparation method comprises the steps of mixing and grinding coal gangue powder and sodium hydroxide, and then roasting to prepare alkali fusion coal gangue; mixing the alkali fused coal gangue, sodium metaaluminate and water, uniformly stirring, and carrying out hydrothermal reaction to obtain a molecular sieve crude product, and sequentially filtering, washing and drying the molecular sieve crude product to obtain the coal gangue-based molecular sieve. The alkaline fusion-hydrothermal preparation method of the coal gangue-based molecular sieve takes coal gangue powder, sodium hydroxide and sodium metaaluminate as raw materials, and combines an alkaline fusion method and a hydrothermal method, so that the coal gangue-based molecular sieve with excellent structural characteristics can be prepared. The preparation method simplifies the preparation process of the molecular sieve, and further improves the synthesis efficiency of the molecular sieve.
Description
Technical Field
The invention belongs to the technical field of solid waste resource utilization, relates to coal gangue resource utilization, and particularly relates to a coal gangue-based molecular sieve and an alkali fusion-hydrothermal preparation method thereof.
Background
With the rapid development of global economy and times, industrial solid wastes from industries such as mineral development and energy production are rapidly increased, and the industrial solid wastes are large in yield, difficult to store and difficult to degrade. Coal is used as the second major energy source in the world, and a large amount of coal-based solid wastes mainly comprising coal gangue are generated in the process of mining and utilizing the coal. The cumulative amount of coal gangue is increased primarily due to coal mining and utilization activities, which have become the major hazardous by-product of the coal mining industry today. The average yield of coal gangue is about 10-15% of the raw coal yield, and the current China coal gangue storage is about 50 hundred million tons.
The coal gangue is a main industrial solid waste separated from lump coal in the coal dressing process, and the accumulation of the coal gangue in a large amount not only occupies large-area land resources, but also induces a series of environmental problems of land degradation, underground water pollution and the like, so that the efficient treatment of the coal gangue becomes a worldwide difficult problem. The main resource utilization ways of the coal gangue comprise power generation, underground goaf filling, civil engineering and the like. And can be used as a catalyst carrier, a cement production raw material, and recovery of valuable metals.
The coal gangue mainly comprises carbonaceous shale, marl, sandy shale, pyrite mineral, argillaceous shale and a small amount of coal, wherein the main chemical component of the coal gangue is silicon dioxide (SiO) 2 ) And aluminum oxide (Al) 2 O 3 ) Very similar in elemental composition to zeolites. Because the coal gangue is low in sintering temperature, the silicon element and the aluminum element in the coal gangue mainly exist in a high-activity amorphous state, and the coal gangue is an ideal raw material for synthesizing the artificial zeolite molecular sieve from the aspect of chemical composition.
Molecular sieve, also known as zeolite, is a porous sodium aluminosilicate whose framework in crystal is made of SiO 4 Tetrahedron and AlO 4 The tetrahedron is formed by connecting oxygen atoms of fixed coke, the aperture of the tetrahedron is less than 2nm, and the micropore structure is a regular pore canal or cage-shaped structure. Therefore, the molecular sieve has large specific surface area and pore structure properties, strong adsorption capacity and high cation exchange capacity, and in addition, has excellent hydrothermal stability. Is currently classified intoThe sub-sieve is widely applied to the environmental and industrial fields, including new-leading-edge fields of adsorbents, catalysts, ion exchangers, antibacterial materials and the like.
The existing preparation method of the molecular sieve needs to adopt a template agent, and the template agent can play a role in adjusting and guiding the microporous structure of the molecular sieve. However, in the actual preparation process, the problems of complex process, low synthesis efficiency and the like exist. In addition, a hydrothermal method is mostly adopted for synthesizing the molecular sieve, a large amount of deionized water is needed as a solvent for the hydrothermal synthesis method, and alkaline wastewater generated during preparation causes serious environmental pollution.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a coal gangue-based molecular sieve and an alkali fusion-hydrothermal preparation method thereof, and solve the technical problems of complex process and low synthesis efficiency of the molecular sieve preparation method in the prior art.
In order to solve the technical problems, the invention adopts the following technical scheme:
an alkali fusion-hydrothermal preparation method of a coal gangue-based molecular sieve comprises the following steps: mixing and grinding the coal gangue powder and sodium hydroxide, and then roasting to prepare alkali fusion coal gangue; mixing alkali-fused coal gangue, sodium metaaluminate and water, uniformly stirring, and performing hydrothermal reaction to obtain a molecular sieve crude product, and sequentially filtering, washing and drying the molecular sieve crude product to obtain a coal gangue-based molecular sieve;
the coal gangue-based molecular sieve is composed of alkali fused coal gangue and sodium metaaluminate.
The invention also has the following technical characteristics:
specifically, the preparation method does not adopt a template agent.
Specifically, the mass ratio of the alkali fused coal gangue to the sodium metaaluminate is (3-5): 1.
Specifically, the average pore diameter of the coal gangue-based molecular sieve is
In particular, the coal gangueThe BET specific surface area of the stone-based molecular sieve is 150-200 m 2 (ii)/g; the pore volume of the coal gangue-based molecular sieve is 0.05-0.15 cm 3 /g。
Specifically, the bulk density of the coal gangue-based molecular sieve is 0.5-0.9 g/mL.
Specifically, the mass of the water is 5-7 times of the sum of the mass of the pretreated coal gangue and the mass of the sodium metaaluminate.
Specifically, the roasting temperature is 700-800 ℃, and the roasting time is 3-5 hours.
Specifically, the temperature of the hydrothermal reaction is 100-110 ℃, and the time of the hydrothermal reaction is 8-14 h; the stirring temperature is 55-60 ℃, and the stirring time is 1-3 h.
The invention also provides a coal gangue-based molecular sieve which is prepared by adopting the alkali fusion-hydrothermal preparation method of the coal gangue-based molecular sieve.
Compared with the prior art, the invention has the following technical effects:
according to the alkali fusion-hydrothermal preparation method of the coal gangue-based molecular sieve, coal gangue powder, sodium hydroxide and sodium metaaluminate are used as raw materials, and an alkali fusion method and a hydrothermal method are combined, so that the coal gangue-based molecular sieve can be prepared.
According to the alkali fusion-hydrothermal preparation method of the coal gangue-based molecular sieve, a template agent is not required, so that compared with the traditional hydrothermal method, the method greatly reduces the water consumption in the zeolite synthesis process, thereby reducing the alkaline wastewater generated in the preparation process and realizing green and environment-friendly effects.
(III) the coal gangue-based molecular sieve of the present invention has an average pore diameter of
The BET specific surface area is 150 to 200m 2 Per g, pore volume of 0.05-0.15 cm 3 The bulk density is 0.5-0.9 g/mL, the structure is excellent, and the method has a wide popularization prospect in practical application.
(IV) the coal gangue-based molecular sieve takes coal gangue as a main raw material, so that the synthesis cost of the molecular sieve is reduced, and the efficient resource utilization of the coal gangue is realized.
Drawings
Fig. 1 is a schematic diagram of an alkali fusion-hydrothermal preparation method of a coal gangue-based molecular sieve.
Fig. 2(a) is an XRD pattern of the coal gangue-based molecular sieves in examples 1 to 3.
Fig. 2(B) is an XRD pattern of the coal gangue-based molecular sieves in example 1 and examples 4 to 3.
Fig. 2(C) is an XRD pattern of the coal gangue-based molecular sieves in examples 7 to 10.
Fig. 2(D) is an XRD pattern of the coal gangue-based molecular sieves in example 1, example 11 and example 12.
FIG. 3 is an electron micrograph of the coal gangue-based molecular sieve of example 1.
Fig. 4 is a spectrum diagram of the coal gangue-based molecular sieve in example 1.
The present invention will be explained in further detail with reference to examples.
Detailed Description
In the invention:
the "BET" in the BET specific surface area is specifically Brunauer-Emmett-Teller.
It is to be noted that all the raw materials in the present invention, unless otherwise specified, may be those known in the art.
The present invention is not limited to the following embodiments, and equivalent changes made on the basis of the technical solutions of the present invention fall within the scope of the present invention.
Example 1:
this embodiment provides an alkali fusion-hydrothermal preparation method of a coal gangue-based molecular sieve, which specifically includes the following steps:
step one, preparing alkali fused coal gangue;
mixing and grinding the coal gangue powder and the solid sodium hydroxide particles according to the mass ratio of 1:0.6, and roasting at 750 ℃ for 4 hours to obtain the alkali fused coal gangue.
In this embodiment, the coal gangue powder has a particle size of 200 mesh. The coal gangue powder comprises an oxide component, wherein the oxide component comprises the following oxides in percentage by mass: SiO 2 2 64.58 percent of CaO, 1.01 percent of CaO, and Al 2 O 3 22.01% of Na 2 0.06% of O, 1.47% of MgO and K 2 O3.29%, Fe 2 O 3 5.58% of TiO 2 1.15%, MnO 0.10%, LiO 0.75%.
Step two, preparing a molecular sieve crude product;
and (2) mixing the alkali fused coal gangue prepared in the step one and sodium metaaluminate to prepare a solid mixture, mixing the solid mixture and water in a mass ratio of 1:6, and stirring for 2 hours at 60 ℃ to prepare a premixed reactant.
Step three, preparing a coal gangue-based molecular sieve;
and (3) carrying out hydrothermal reaction on the premixed reactant prepared in the second step at 100 ℃ for 8 hours to prepare a molecular sieve crude product, and sequentially filtering, washing and drying the molecular sieve crude product until the pH value is 7-8 to prepare the coal gangue-based molecular sieve.
The coal gangue-based molecular sieve prepared in the embodiment is composed of alkali fused coal gangue and sodium metaaluminate, and the mass ratio of the alkali fused coal gangue to the sodium metaaluminate is 5: 1.
In this example, the characterization data of the coal gangue-based molecular sieve is as follows:
the XRD spectrum of the gangue-based molecular sieve is shown in fig. 2(a), and as can be seen from fig. 2(a), the XRD spectrum of the gangue-based molecular sieve is highly consistent with that of the commercial 13-X molecular sieve. The microscopic morphology of the coal gangue-based molecular sieve is shown in FIG. 3, and the energy spectrum of the coal gangue-based molecular sieve is shown in FIG. 4.
In this example, the structural characteristic parameters of the coal gangue-based molecular sieves are shown in table 1.
Example 2:
this example provides an alkali fusion-hydrothermal preparation method of a coal gangue-based molecular sieve, which has the following steps: in the third step, the hydrothermal reaction time is 10 h.
The components and the component contents of the gangue-based molecular sieve prepared in this example are completely the same as those of example 1.
In this example, an XRD spectrum of the coal gangue-based molecular sieve is shown in fig. 2 (a).
Example 3:
this example provides an alkali fusion-hydrothermal method for preparing a gangue-based molecular sieve, which is substantially the same as example 1 except that: in the third step, the hydrothermal reaction time is 14 h.
The components and the component contents of the gangue-based molecular sieve prepared in this example are completely the same as those of example 1.
In this example, an XRD spectrum of the coal gangue-based molecular sieve is shown in fig. 2 (a).
Example 4:
this example provides an alkali fusion-hydrothermal method for preparing a coal gangue-based molecular sieve, which has the same steps as in example 1.
The coal gangue-based molecular sieve prepared in the embodiment is composed of alkali fused coal gangue and sodium metaaluminate, and the mass ratio of the alkali fused coal gangue to the sodium metaaluminate is 6: 1.
In this example, an XRD spectrum of the gangue-based molecular sieve is shown in fig. 2 (B).
In this example, the structural characteristic parameters of the coal gangue-based molecular sieves are shown in table 1.
Example 5:
this example provides an alkali fusion-hydrothermal method for preparing a coal gangue-based molecular sieve, which has the same steps as in example 1.
The coal gangue-based molecular sieve prepared in the embodiment is composed of alkali fused coal gangue and sodium metaaluminate, and the mass ratio of the alkali fused coal gangue to the sodium metaaluminate is 4: 1.
In this example, the XRD spectrum of the coal gangue-based molecular sieve is shown in fig. 2 (B).
Example 6:
this example provides an alkali fusion-hydrothermal method for preparing a gangue-based molecular sieve, which includes the same steps as in example 1.
The coal gangue-based molecular sieve prepared in the embodiment is composed of alkali fused coal gangue and sodium metaaluminate, and the mass ratio of the alkali fused coal gangue to the sodium metaaluminate is 3: 1.
In this example, the XRD spectrum of the coal gangue-based molecular sieve is shown in fig. 2 (B).
Example 7:
this example provides an alkali fusion-hydrothermal preparation method of a coal gangue-based molecular sieve, which has the following steps: in the first step, coal gangue powder and solid sodium hydroxide particles are mixed according to the mass ratio of 1: 0.8.
The coal gangue-based molecular sieve prepared in the embodiment is composed of alkali fused coal gangue and sodium metaaluminate, and the mass ratio of the alkali fused coal gangue to the sodium metaaluminate is 6: 1.
In this example, an XRD spectrum of the coal gangue-based molecular sieve is shown in fig. 2 (C).
Example 8:
this example provides an alkali fusion-hydrothermal preparation method of a coal gangue-based molecular sieve, which has the following steps: in the first step, coal gangue powder and solid sodium hydroxide particles are mixed according to the mass ratio of 1: 0.8.
The coal gangue-based molecular sieve prepared in the embodiment is composed of alkali fused coal gangue and sodium metaaluminate, and the mass ratio of the alkali fused coal gangue to the sodium metaaluminate is 5: 1.
In this example, an XRD spectrum of the coal gangue-based molecular sieve is shown in fig. 2 (C).
Example 9:
this example provides an alkali fusion-hydrothermal preparation method of a coal gangue-based molecular sieve, which has the following steps: in the first step, coal gangue powder and solid sodium hydroxide particles are mixed according to the mass ratio of 1: 0.8.
The coal gangue-based molecular sieve prepared in the embodiment is composed of alkali fused coal gangue and sodium metaaluminate, and the mass ratio of the alkali fused coal gangue to the sodium metaaluminate is 4: 1.
In this example, an XRD spectrum of the coal gangue-based molecular sieve is shown in fig. 2 (C).
Example 10:
this example provides an alkali fusion-hydrothermal preparation method of a coal gangue-based molecular sieve, which has the following steps: in the first step, coal gangue powder and solid sodium hydroxide particles are mixed according to the mass ratio of 1: 0.8.
The gangue-based molecular sieve prepared in this example is composed of alkali fused gangue and sodium metaaluminate, and the mass ratio of the alkali fused gangue to the sodium metaaluminate is 3: 1.
In this example, an XRD spectrum of the coal gangue-based molecular sieve is shown in fig. 2 (C).
Comparative example 1:
the comparative example provides a preparation method of a coal gangue-based molecular sieve, and the preparation method is mainly different from the preparation method of the example 1 in that: the preparation method adopts a template agent.
The method specifically comprises the following steps:
in this comparative example, step one was exactly the same as step one of example 1.
Step two, preparing a premixed reactant containing a template agent;
mixing the alkali fused coal gangue prepared in the step one and sodium metaaluminate according to the mass ratio of 5:1 to prepare a solid mixture, mixing the solid mixture and water according to the mass ratio of 1:6, adding a template agent, and stirring at 60 ℃ for 2 hours to prepare a premixed reactant containing the template agent. In the comparative example, the template agent is cetyl trimethyl ammonium bromide, and the addition amount of the template agent is one seventh of the mass of the coal gangue powder.
In this comparative example, step three was substantially the same as step three of example 1, except that the premixed reactant containing the template prepared in step two was subjected to hydrothermal reaction.
The coal gangue-based molecular sieve prepared by the comparative example consists of alkali fused coal gangue, sodium metaaluminate and a template agent, wherein the mass ratio of the alkali fused coal gangue to the sodium metaaluminate to the template agent is 35:7: 5.
In this comparative example, the XRD spectrum of the coal gangue-based molecular sieve is shown in fig. 2 (D).
In this comparative example, the structural characteristic parameters of the gangue-based molecular sieves are shown in table 1.
Comparative example 2:
the comparative example provides a preparation method of a coal gangue-based molecular sieve, which is basically the same as the comparative example 1, and the difference is that in the second step, the addition amount of the template agent is three-sevenths of the mass of the coal gangue powder.
The coal gangue-based molecular sieve prepared by the comparative example consists of alkali fused coal gangue, sodium metaaluminate and a template agent, wherein the mass ratio of the alkali fused coal gangue to the sodium metaaluminate to the template agent is 35:7: 15.
In this comparative example, the XRD spectrum of the coal gangue-based molecular sieve is shown in fig. 2 (D).
Table 1 structural characteristic parameters of coal gangue-based molecular sieves in example 1 and comparative example 1
The following conclusions can be drawn from example 1, example 4 and comparative example 1:
(A) the bulk densities of example 1 and comparative example 1 were 0.574g/mL and 0.731g/mL, respectively, with higher bulk densities indicating less volume of molecular sieve required for the same adsorption requirements. From the above analysis, it can be seen that the volume required for example 1 is larger than that of comparative example 1 for the same adsorption requirement.
(B) The BET specific surface areas of example 1 and comparative example 1 were 199.445m 2 G and 29.6789m 2 The pore volume is 0.103 cm/g 3 G and 0.042cm 3 The larger the specific surface area and pore volume, the stronger the adsorption capacity. From the above analysis, it can be seen that the BET specific surface area and the pore volume of example 1 are much larger than those of comparative example 1, which shows that the molecular sieve prepared in example 1 has a better adsorption capacity than that of comparative example 1.
(C) The average pore diameters of example 1 and comparative example 1 were respectively
And
the smaller the average pore size, the smaller the molecular sieve is able to adsorb molecules. From the above analysis, it is understood that example 1 can adsorb a smaller molecule than comparative example 1.
Claims (10)
1. An alkali fusion-hydrothermal preparation method of a coal gangue-based molecular sieve is characterized by comprising the following steps: mixing and grinding the coal gangue powder and sodium hydroxide, and roasting to prepare alkali fusion coal gangue; mixing alkali-fused coal gangue, sodium metaaluminate and water, uniformly stirring, and performing hydrothermal reaction to obtain a molecular sieve crude product, and sequentially filtering, washing and drying the molecular sieve crude product to obtain a coal gangue-based molecular sieve;
the coal gangue-based molecular sieve is composed of alkali fused coal gangue and sodium metaaluminate.
2. The alkaline melt-hydrothermal process for preparing a coal gangue-based molecular sieve of claim 1, wherein no templating agent is used.
3. The alkali fusion-hydrothermal preparation method of the coal gangue-based molecular sieve as defined in claim 1, wherein the mass ratio of the alkali fused coal gangue to the sodium metaaluminate is (3-5): 1.
4. The alkali fusion-hydrothermal process for preparing a coal gangue-based molecular sieve of claim 1, wherein the coal gangue-based molecular sieve has an average pore size of
5. The method of claim 1The alkali fusion-hydrothermal preparation method of the coal gangue-based molecular sieve is characterized in that the BET specific surface area of the coal gangue-based molecular sieve is 150-200 m 2 (ii)/g; the pore volume of the coal gangue-based molecular sieve is 0.05-0.15 cm 3 /g。
6. The alkali fusion-hydrothermal preparation method of the coal gangue-based molecular sieve of claim 1, wherein the bulk density of the coal gangue-based molecular sieve is 0.5-0.9 g/mL.
7. The alkali fusion-hydrothermal preparation method of the coal gangue-based molecular sieve of claim 1, wherein the mass of the water is 5 to 7 times of the sum of the mass of the pretreated coal gangue and the mass of the sodium metaaluminate.
8. The alkali fusion-hydrothermal preparation method of the coal gangue-based molecular sieve of claim 1, wherein the roasting temperature is 700-800 ℃ and the roasting time is 3-5 h.
9. The alkali fusion-hydrothermal preparation method of the coal gangue-based molecular sieve of claim 1, wherein the temperature of the hydrothermal reaction is 100-110 ℃, and the time of the hydrothermal reaction is 8-14 h; the stirring temperature is 55-60 ℃, and the stirring time is 1-3 h.
10. A coal gangue-based molecular sieve produced by the alkali fusion-hydrothermal production method of a coal gangue-based molecular sieve as defined in any one of claims 1 to 9.
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| CN112209399A (en) * | 2020-09-11 | 2021-01-12 | 内蒙古师范大学 | Method for preparing X-type zeolite from coal gangue |
| AU2020104217A4 (en) * | 2020-12-22 | 2021-03-11 | Hubei University For Nationalities | The alkali activation of active element selenium in coal gangue and a preparation method of its selenium fertilizer |
| 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 |
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|---|---|---|---|---|
| CN1254681A (en) * | 1999-11-09 | 2000-05-31 | 复旦大学 | Processf or preparing X-zeolite from coal gangue |
| CN1346794A (en) * | 2001-09-24 | 2002-05-01 | 复旦大学 | High-temp alkali fusing-hydrothermal crystallizing process for preparing A-type zeolite from coal gangue |
| CN101214973A (en) * | 2008-01-08 | 2008-07-09 | 中国日用化学工业研究院 | Method for preparing high whiteness A-type zeolite from coal gangue |
| CN104556119A (en) * | 2015-01-28 | 2015-04-29 | 西安科技大学 | Method for preparing 13X molecular sieve by adopting coal slime |
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| AU2020104217A4 (en) * | 2020-12-22 | 2021-03-11 | Hubei University For Nationalities | The alkali activation of active element selenium in coal gangue and a preparation method of its selenium fertilizer |
| 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 |
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