CN110877911B - Synthesis method of magnetic Na-P type zeolite - Google Patents
Synthesis method of magnetic Na-P type zeolite Download PDFInfo
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- CN110877911B CN110877911B CN201911171277.XA CN201911171277A CN110877911B CN 110877911 B CN110877911 B CN 110877911B CN 201911171277 A CN201911171277 A CN 201911171277A CN 110877911 B CN110877911 B CN 110877911B
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- C01B39/00—Compounds having molecular sieve and base-exchange properties, e.g. crystalline zeolites; Their preparation; After-treatment, e.g. ion-exchange or dealumination
- C01B39/02—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof; Direct preparation thereof; Preparation thereof starting from a reaction mixture containing a crystalline zeolite of another type, or from preformed reactants; After-treatment thereof
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- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
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- H—ELECTRICITY
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- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
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- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
Abstract
The invention discloses a synthesis method of magnetic Na-P type zeolite, which comprises the steps of putting zinc slag, fly ash, sodium hydroxide and deionized water into a high-pressure kettle, carrying out hydrothermal reaction, washing and drying to obtain the Na-P type zeolite, wherein the mass ratio of the zinc slag, the fly ash, the sodium hydroxide and the deionized water is 0.25-1.5: 1: 0.73: 15. the invention takes industrial solid waste zinc slag and fly ash as raw materials, adopts hydrothermal reaction, and directly synthesizes magnetic Na-P type zeolite by a one-step method. The synthetic process is simple, the cost is low, the principle of circular economy development is met, and the method is a new way for high-added-value utilization of industrial solid waste zinc slag and fly ash.
Description
Technical Field
The invention belongs to the field of resource utilization of solid wastes and synthesis of zeolite, and relates to a method for synthesizing zeolite, in particular to a method for directly synthesizing magnetic Na-P type zeolite by using solid wastes, namely zinc slag and fly ash as raw materials through a one-step method.
Background
The zinc slag is an industrial solid waste discharged in the process of smelting metal zinc. In the zinc smelting process flow, according to the report of the national statistical bureau and the data center of the Chinese report hall[1]568.1 million tons of zinc are produced by zinc smelting enterprises in 2018, 0.96 ton of zinc dross is discharged when 1 ton of metal zinc is produced, and according to the estimation, the discharge amount of the zinc dross in China is about 545 million tons only in 2018, and the historical stock of the zinc dross exceeds hundred million tons[2]. The stacking of a large amount of zinc slag not only pollutes the environment, but also contains metal zinc, iron, manganese, lead, cadmium, nickel, copper and the like, and if the zinc slag is not used, valuable metals are wasted.
The fly ash is the main solid waste discharged by coal-fired power plants, and the discharge amount of the fly ash is increased year by year along with the continuous development of the electric power industry in China. The annual discharge amount of fly ash in China exceeds five hundred million tons[3,4]. When a large amount of fly ash is piled up, the fly ash is blown by wind and rain, thereby not only generating dust and polluting atmosphere, but also causing silting of a drainage system and underground water quality pollution。
Fly ash has been widely used in the art as a primary raw material for zeolite production.
Xu Ying[5]Etc. magnetic Fe3O4The nano particles are loaded on the surface of the fly ash, then alkali and an aluminum source are added to synthesize the magnetic fly ash zeolite by hydrothermal method, and NaOH and NaAlO are investigated2The addition amount has influence on the synthesis of magnetic fly ash zeolite, which is a mixture of A-type zeolite, sodalite, analcite, etc. and magnetic Fe3O4A composite of nanoparticles.
Wang Kai [6]Using fly ash as main raw material, acidifying fly ash by hydrochloric acid to load magnetic Fe3O4Then the magnetic fly ash is obtained. The magnetic fly ash solid and 2mol/L NaOH solution are stirred vigorously for 1h, the mixture is placed in a metal reaction kettle, then the mixture is aged for 1h at 50 ℃, then the temperature is raised to 110 ℃, and then the mixture is crystallized for 24h, and finally the magnetic fly ash zeolite is obtained after washing and drying.
Wen Xiaoqing[7]Taking fly ash as a raw material, and carrying out acidification treatment on the fly ash by adopting hydrochloric acid under the water bath heating condition of 80 ℃; then mixing and grinding the pretreated fly ash and solid NaOH according to the ratio of 1:1.2, carrying out melt calcination at 550 ℃ for 1h, and cooling to room temperature; with magnetic Fe3O4@TiO2Taking nano particles, fly ash and a sample which is fused and calcined at 550 ℃ by solid NaOH as raw materials, adding sodium stearate and distilled water, and synthesizing the loaded Fe through high-pressure reaction3O4@TiO2The magnetic Na-P type zeolite composite material of (1).
Sun Qi[8]Taking kaolin as a raw material, preparing 4A zeolite by adopting a hydrothermal method, and then loading magnetic Fe3O4Magnetic 4A zeolite was prepared.
Sun Qi et al[9]The patent reports that P-type zeolite is prepared by taking fly ash calcined at 500-800 ℃ as a raw material and adopting a hydrothermal method, and then Fe3O4The magnetic P-type zeolite is obtained by loading the P-type zeolite.
Periapical peak and the like[10]Mixing fly ash and solid NaOH according to the mass ratio of alkali ash of 1Mixing at a ratio of 2: 1, and weighing a certain amount of SiO2Adding the powder into the mixture to enable the Si/Al molar ratio to be 1.0, grinding, uniformly mixing, placing into a crucible, adding a small amount of deionized water, and placing into a high-temperature furnace to roast for 2 hours at 600 ℃ to obtain the fly ash clinker. Mixing Fe3O4Fine particles dissolved in a small amount of deionized water to produce Fe3O4And (3) dispersing the mixture. Weighing a certain amount of fly ash clinker and Fe3O4Mixing the dispersion liquid, mixing the dispersion liquid with 6 times of deionized water, stirring at room temperature for 24h to achieve the purpose of aging, taking supernatant liquid, placing in a high-temperature high-pressure reaction kettle, and crystallizing at 100 ℃ for 4 h. The A-type zeolite can be prepared.
Yamaura et al[11,12]Taking fly ash as a raw material, preparing hydroxysodalite through hydrothermal reaction, and then mixing the hydroxysodalite with magnetic Fe3O4And mixing and stirring the mixture in the aqueous solution according to the mass ratio of 3:1 to obtain the magnetic hydroxyl sodalite.
In addition, the magnetic zeolite can be prepared by ion exchange, electrostatic adsorption, or the like. Horikawa et al[13]Selecting Ni+The ions react with Na in Na-A, Na-Y zeolite+The ions are ion exchanged to form Ni-A, Ni-Y two kinds of magnetic zeolite.
Anunziata, etc[14]Passing Na-ZSM-11 through NH4 +Exchange preparation of ammonium ion exchanged NH4-ZSM-11 zeolite, followed by FeSO4·7H2O and Fe (NO)3)3·9H2Soaking solution of O salt in NH4-ZSM-11 zeolite, N2Roasting at 500 ℃ for 10h in an air atmosphere, and continuously roasting a sample at 500 ℃ for 12h in an air atmosphere to obtain the loaded Fe3O4The magnetic H-ZSM-11 zeolite composite material.
Tao et al[15]Dispersing fly ash in 95% ethanol, screening floating beads with diameter of 200-300 μm, chemically plating nickel on the surface of the floating beads, electrostatically adsorbing ZSM-5 zeolite seed crystal with average particle size of 180nm on the surface of the nickel-plated floating beads (Ni/floating beads), mixing with surfactant (tetraethylammonium bromide), NaOH, aluminum foil, tetraethyl orthosilicate and deionized water in a certain proportion, carrying out hydrothermal reaction at 180 ℃ for 12-24h, and baking at 550 DEG CAnd (5) burning for 5h to prepare the ZSM-5/Ni/fly ash floating bead magnetic composite material.
In summary, applicants have systematically consulted a large amount of domestic and foreign literature, and the existing literature reports mainly through Fe3O4The magnetic zeolite is formed by compounding a magnetic substance with A-type, P-type and ZSM-5 zeolite through a plurality of steps of loading, ion exchange, electrostatic adsorption and the like. However, no relevant literature report is found that solid wastes, namely the zinc dross and the fly ash, are used as raw materials, magnetic components in the zinc dross and the fly ash are fully utilized, and no magnetic substance is added, so that the magnetic zeolite is directly synthesized by a one-step method.
The following are references given by the inventors:
[1]http://www.chinabgao.com/chanliang/284778.html。
[2] hawaiping, Han dynasty, Gaoyanqiang, etc. comprehensive utilization of zinc smelting slag [ J ] inorganic salt industry, 2017,49(7): 57-60.
[3] Physical property and resource utilization of Zhuwanxin fly ash [ J ] colored equipment, 2016,4: 44-47.
[4] Jin dawn, guoping, zana et al research on fly ash synthetic zeolites advanced [ J ] environmental chemistry, 2015, 34 (11): 2025-2038.
[5]Preparation of magnetic fly ash zeolite and its application in Cu2+Study of adsorption [ J]Nonmetallic mine, 2014,37(6): 62-65.
[6] Wangkai, Li Xiuhua, Berger et al, preparation of magnetic fly ash based zeolite and its adsorption study on methylene blue [ J ]. Chifeng college bulletin (Nature edition), 2016,32(21): 12-14.
[7]Load Fe under the condition of mild weather3O4@TiO2Preparation of Zeolite composite and oil absorption study thereof [ D]Master academic thesis, tianjin university, 2016.
[8] Sunzhi, Kaolin and fly ash, Zeolite synthesis and magnetic particle loading research [ D ]. doctor academic thesis, geological university of China, 2015.
[9] Grand, royal, liu and bin, etc. a preparation method of a magnetic P-type zeolite molecular sieve, chinese patent publication no: CN 109336186a, 2019.
[10] Zhou Lifeng, anyao, Guyue, etc. the research on the synthesis and adsorption performance of the fly ash-based magnetic A-type zeolite, metallurgical energy, 2018, 37(6): 54-58.
[11]Yamaura M，Fungaro D A.Synthesis and characterization of magnetic adsorbent preparedby magnetite nanoparticles and zeolite from coal fly ash,Journal of Material Science,2013，48:5093-5101。
[12]Fungaro D A，Yamaura M，Craesmeyer G R.Removal from aqueous solution by zeolitefrom fly ash-iron oxide magnetic nanocomposite，International Review of Chemical Engineering，2012，4(3):353-358。
[13]Horikawa Y，Ohnishi N，Hiraga K.Structures and magnetic susceptibility of Ni-ion-introduced zeolite A and X[J].Materials Science and Engineering A，1996，217/218:139-141。
[14]Anunziata O A，Costa M G,Beltramone A R.Fe-ZSM-11magnetic properties:Its relation with the catalytic activity for NOx SCR with isobutane and O2[J].Applied Catalysis A General，2006，307(2):263-269。
[15]Tao H，Yao J，Zhang L，et al.Preparation of magnetic ZSM-5/Ni/fly-ash hollow microspheres using fly-ash cenospheres as the template[J].Materials Letters，2009，63(2):203-205。
Disclosure of Invention
In order to accord with the principle of circular economy development and further utilize industrial solid waste with high added value, the invention aims to provide a method for synthesizing magnetic Na-P type zeolite.
In order to realize the task, the invention adopts the following technical solution:
a synthesis method of magnetic Na-P type zeolite is characterized by comprising the steps of putting zinc dross, fly ash, sodium hydroxide and deionized water into a high-pressure kettle, carrying out hydrothermal reaction, washing and drying to obtain the Na-P type zeolite, wherein the mass ratio of the zinc dross to the fly ash to the sodium hydroxide to the deionized water is 0.25-1.5: 1: 0.73: 15.
the method specifically comprises the following steps:
(1) weighing zinc slag and fly ash according to the formula ratio, and uniformly mixing to obtain a mixture;
(2) weighing solid sodium hydroxide according to the formula ratio, and placing the solid sodium hydroxide into a beaker;
(3) weighing deionized water according to the formula amount, pouring the deionized water into the beaker in the step (2), and stirring to completely dissolve sodium hydroxide to form 45mL of 1-2 mol/L sodium hydroxide solution;
(4) and (3) placing the sodium hydroxide solution obtained in the step (3) and the mixture obtained in the step (1) into a high-pressure reaction kettle, sealing the kettle, reacting for 12-48 hours at 90-120 ℃, and naturally cooling, filtering, washing and drying after the reaction is finished to obtain the magnetic Na-P type zeolite.
The synthesis method of the magnetic Na-P type zeolite has the innovation points that: the pure magnetic Na-P type zeolite is directly synthesized by a one-step method by taking solid wastes of zinc dross and fly ash as raw materials and adopting a hydrothermal reaction. The method not only realizes the high added value utilization of the zinc slag and the fly ash, but also simplifies the synthesis process of the magnetic zeolite and reduces the synthesis cost of the magnetic zeolite.
Drawings
FIG. 1 is the XRD pattern of example 1;
FIG. 2 is a hysteresis loop in example 1;
FIG. 3 is a photograph showing a magnetic separation experiment of the magnetic Na-P type zeolite in example 1;
FIG. 4 is XRD patterns of comparative Experimental example 1 and comparative Experimental example 2;
the present invention will be described in further detail with reference to the following drawings and examples.
Detailed Description
It should be noted that the following examples are only for better illustrating the present invention and the present invention is not limited to these examples.
In the following embodiment, the raw materials of the prepared magnetic Na-P type zeolite comprise zinc dross, fly ash, sodium hydroxide and deionized water, wherein the mass ratio of the zinc dross to the fly ash to the sodium hydroxide to the deionized water is 0.25-1.5: 1: 0.73: 15.
(1) zinc slag: from a commercial zinc plant.
The main oxide composition (mass percent) of the zinc slag is as follows: fe2O3(39.68％)，SiO2(16.79％)，Al2O3(8.49％)，CaO(9.10％)，K2O(4.00％)，MgO(2.32％)，Na2O(1.00％)，SO3(0.42％)，LOI(18.20％)。
(2) Fly ash from inner Mongolia thermal power plants.
The main oxide composition (mass percent) of the fly ash is as follows: al (Al)2O3(42.24％)，SiO2(37.15％)，CaO(2.97％)，Fe2O3(3.01％)，TiO2(2.02％)，Na2O(0.41％)，MgO(0.31％)，K2O(0.45％)，P2O5(0.23％)，SO3(0.89％)，LOI(10.32％)。
(3) Sodium hydroxide (anhydrous), purchased from Shanghai Michelin Biochemical technology Ltd, analytical grade reagent, molecular weight: 39.996.
(4) deionized water, self-made in laboratories.
The following are specific examples given by the inventors and comparative experimental examples.
Example 1:
accurately weighing zinc dross, fly ash, sodium hydroxide and deionized water, wherein the mass ratio of the zinc dross to the fly ash to the sodium hydroxide is 0.25: 1: 0.73: 15; fully and uniformly stirring the zinc slag and the fly ash to obtain a mixture; dissolving sodium hydroxide in deionized water to obtain 1.2mol/L sodium hydroxide solution, cooling the solution to room temperature, then pouring the mixture into the sodium hydroxide solution, and stirring for 2min to obtain uniform slurry; putting the slurry into a high-pressure reaction kettle, sealing the kettle, and placing the kettle in an oven for hydrothermal reaction at 90 ℃ for 12 hours; taking out, washing and drying to obtain the magnetic Na-P type zeolite.
FIG. 1 is an XRD spectrum of a synthesized magnetic Na-P type zeolite. As can be seen from FIG. 1, except for the magnetic Fe3O4And no other miscellaneous peak except the diffraction peak of the Na-P type zeolite exists, indicating thatPure magnetic Na-P type zeolite is synthesized by using zinc slag and fly ash solid waste as raw materials.
FIG. 2 is a hysteresis loop of the synthesized magnetic Na-P type zeolite. As can be seen from FIG. 2, the specific saturation magnetization of the magnetic Na-P type zeolite is 3.85emu/G, the coercive force is 70.02G, and the remanence is 0.05 emu/G.
FIG. 3 is a photograph showing a magnetic separation experiment of the synthesized magnetic Na-P type zeolite. As can be seen from FIG. 3, when the magnetic Na-P type zeolite sample dispersed in water was placed in a magnetic field, the magnetic Na-P type zeolite was adsorbed on the magnet side, indicating that the resultant magnetic Na-P type zeolite had strong magnetism.
Example 2:
accurately weighing zinc dross, fly ash, sodium hydroxide and deionized water, wherein the mass ratio of the zinc dross to the fly ash to the sodium hydroxide is 0.67: 1: 0.73: 15; fully and uniformly stirring the zinc slag and the fly ash, dissolving solid sodium hydroxide in deionized water to obtain a 1.2mol/L sodium hydroxide solution, cooling the solution to room temperature, then pouring the mixture into the sodium hydroxide solution, and stirring for 2min to obtain uniform slurry; putting the slurry into a high-pressure reaction kettle, sealing the kettle, and carrying out hydrothermal reaction at 105 ℃ for 24 hours; then taking out, washing and drying to obtain the magnetic Na-P type zeolite.
Example 3:
accurately weighing zinc dross, fly ash, sodium hydroxide and deionized water, wherein the mass ratio of the zinc dross to the fly ash to the sodium hydroxide is 1.5: 1: 0.73: 15; fully and uniformly stirring the zinc slag and the fly ash, dissolving solid sodium hydroxide in deionized water to obtain a 1.2mol/L sodium hydroxide solution, cooling the solution to room temperature, then pouring the mixture into the sodium hydroxide solution, and stirring for 2min to obtain uniform slurry; putting the slurry into a high-pressure reaction kettle, sealing the kettle, and carrying out hydrothermal reaction at 120 ℃ for 24 hours; then taking out, washing and drying to obtain the magnetic Na-P type zeolite.
Comparative experimental examples are given below:
comparative experimental example 1:
accurately weighing zinc dross, fly ash, sodium hydroxide and deionized water, wherein the mass ratio of the zinc dross to the fly ash to the sodium hydroxide is 1: 0: 0.73: 15, dissolving solid sodium hydroxide in deionized water to obtain a 1.2mol/L sodium hydroxide solution, cooling the solution to room temperature, then pouring zinc slag into the sodium hydroxide solution, and stirring for 2min to obtain uniform slurry; filling the slurry into a high-pressure reaction kettle, sealing the kettle, and carrying out hydrothermal reaction at 105 ℃ for 24 hours; then, the sample was taken out, washed and dried to obtain comparative sample 1, as shown in FIG. 4. As can be seen from FIG. 4, no magnetic Na-P type zeolite is formed under the reaction conditions.
Comparative experiment example 2:
accurately weighing zinc dross, fly ash, sodium hydroxide and deionized water, wherein the mass ratio of the zinc dross to the fly ash to the sodium hydroxide is 0: 1: 0.73: 15, dissolving solid sodium hydroxide in deionized water to obtain a 1.2mol/L sodium hydroxide solution, cooling the solution to room temperature, then pouring the fly ash into the sodium hydroxide solution, and stirring for 2min to obtain uniform slurry; filling the slurry into a high-pressure reaction kettle, sealing the kettle, and carrying out hydrothermal reaction at 105 ℃ for 24 hours; then, the sample was taken out, washed and dried to obtain comparative sample 2, and no magnetic Na-P type zeolite was produced under the reaction conditions.
Comparative experiment example 3:
accurately weighing zinc dross, fly ash, sodium hydroxide and deionized water, wherein the mass ratio of the zinc dross to the fly ash to the sodium hydroxide is 1.5: 1: 0.73: 15; fully and uniformly stirring the zinc slag and the fly ash, dissolving solid sodium hydroxide in deionized water to obtain a 1.2mol/L sodium hydroxide solution, cooling the solution to room temperature, then pouring the mixture into the sodium hydroxide solution, and stirring for 2min to obtain uniform slurry; filling the slurry into a high-pressure reaction kettle, sealing the kettle, and carrying out hydrothermal reaction at 80 ℃ for 24 hours; then, the sample was taken out, washed and dried to obtain comparative sample 3, in which no magnetic Na-P type zeolite was formed under the reaction conditions.
Claims (3)
1. A synthesis method of magnetic Na-P type zeolite is characterized by comprising the steps of putting zinc dross, fly ash, sodium hydroxide and deionized water into a high-pressure kettle, carrying out hydrothermal reaction, washing and drying to obtain the Na-P type zeolite, wherein the mass ratio of the zinc dross to the fly ash to the sodium hydroxide to the deionized water is 0.25-1.5: 1: 0.73: 15;
the hydrothermal reaction is carried out for 12 to 48 hours at the temperature of between 90 and 120 ℃;
the zinc slag comprises the following main oxides in percentage by mass: fe2O3：39.68％，SiO2：16.79％，Al2O3：8.49％，CaO：9.10％，K2O：4.00％，MgO：2.32％，Na2O：1.00％，SO3：0.42％，LOI：18.20％；
The main oxides of the fly ash comprise the following components in percentage by mass: al (Al)2O3：42.24％，SiO2：37.15％，CaO：2.97％，Fe2O3：3.01％，TiO2：2.02％，Na2O：0.41％，MgO：0.31％，K2O：0.45％，P2O5：0.23％，SO3：0.89％，LOI：10.32％。
2. The method according to claim 1, characterized in that it is carried out in particular by the following steps:
(1) weighing zinc slag and fly ash according to the formula ratio, and uniformly mixing to obtain a mixture;
(2) weighing solid sodium hydroxide according to the formula ratio, and placing the solid sodium hydroxide into a beaker;
(3) weighing deionized water according to the formula amount, pouring the deionized water into the beaker in the step (2), and stirring to completely dissolve sodium hydroxide to form 45mL of 1-2 mol/L sodium hydroxide solution;
(4) and (3) placing the sodium hydroxide solution obtained in the step (3) and the mixture obtained in the step (1) into a high-pressure reaction kettle, sealing the kettle, reacting for 12-48 hours at 90-120 ℃, and naturally cooling, filtering, washing and drying after the reaction is finished to obtain the magnetic Na-P type zeolite.
3. A magnetic Na-P zeolite obtainable by the process of claim 1 or 2.
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