CN114014332A - Method for preparing 4A molecular sieve by using aluminum ash and micro silicon powder - Google Patents
Method for preparing 4A molecular sieve by using aluminum ash and micro silicon powder Download PDFInfo
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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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Abstract
A method for preparing a 4A molecular sieve by using aluminum ash and micro silicon powder comprises the steps of washing the aluminum ash at 30-50 ℃, drying a filter cake, adding 1-3 times of alkali by mass, mixing, placing in a crucible, placing in a muffle furnace, roasting at 600-800 ℃ to obtain sodium aluminate clinker, and preparing into a sodium aluminate solution; uniformly mixing micro silicon powder and 1-2 times of alkali by mass, placing the mixture in a muffle furnace, roasting at 550-750 ℃ to obtain sodium silicate clinker, and preparing a sodium silicate solution; mixing the sodium aluminate solution and the sodium silicate solution, adjusting the silica-alumina ratio to be 1.0-3.0, crystallizing for a preset time at the temperature of 80-120 ℃, and filtering and drying to obtain white powder, namely the 4A molecular sieve. According to the invention, the solid wastes of aluminum ash and silica fume are used as raw materials, no by-product is generated in the reaction process, the final product of the 4A molecular sieve plays an important role in water treatment, metallurgy, petrifaction and medicine industries, and the resource utilization of the solid wastes can be realized.
Description
Technical Field
The invention relates to a technology for preparing a 4A molecular sieve by utilizing aluminum ash and micro silicon powder, belonging to the technology of comprehensive utilization of wastes.
Background
The aluminum ash is solid waste generated in the process of casting aluminum, and mainly contains substances such as aluminum and oxide valuable components thereof, aluminum nitride (AlN), other metal oxides, inorganic salts and the like. The micro silicon powder is spherical dust formed by combining silicon gas generated in a silicon electric furnace and oxygen in the air in the smelting process of ferrosilicon alloy and metal silicon, and is also solid waste. The dust mainly contains valuable component silicon dioxide. According to statistics, 180-290 kg of aluminum ash is generated in the process of processing and applying 1t of aluminum; 1t of silicon micropowder can be produced when 3t of industrial silicon is produced, and 1t of silicon micropowder can be produced when 5t of ferrosilicon is produced. At present, the treatment mode of the aluminum ash and the micro silicon powder is mainly accumulation or landfill, and the method not only can cause the waste of valuable substances, but also can cause serious harm to the environment. Toxic substances in the aluminum ash can be leached and permeate into the ground surface, and gas is discharged into the air after the aluminum ash is affected with damp; the micro silicon powder particles have small particle size and are easy to float, and can cause harm to human bodies and the environment. Therefore, how to utilize the huge amount of industrial wastes as resources is a problem that enterprises need to solve urgently.
The 4A molecular sieve is aluminosilicate with porous structure and molecular formula of Na12Al12Si12O48·27H2Because of the special crystallization mode, the O has unique adsorption, catalysis and ion exchange capacities, and is widely applied to the aspects of drying of gas and liquid, washing aids, sewage treatment and the like.
At present, two preparation methods of the 4A molecular sieve are mainly used, one is chemical synthesis, and the main raw materials are sodium hydroxide, water glass, aluminum hydroxide and the like; the other is a semi-chemical method, and the main raw materials are kaolin, bentonite, coal gangue, fly ash, white mud and the like. CN111908484A discloses a method for preparing a 4A molecular sieve from white mud, which requires deoiling, calcining, washing, and acid washing in the pretreatment process of white mud, and an aluminum source in the subsequent process, and has complex process and high cost.
Disclosure of Invention
The invention aims to provide a method for preparing a 4A molecular sieve by using aluminum ash and micro silicon powder.
The invention relates to a method for preparing a 4A molecular sieve by using aluminum ash and micro silicon powder, which comprises the following steps:
weighing 400-600 g of casting aluminum ash, ball-milling and sieving;
step (2), keeping the temperature of the aluminum ash and water at 30-50 ℃ for 1-3 h according to the solid-to-liquid ratio of 1:5, washing a filter cake with water to be neutral, drying and grinding to obtain desalted aluminum ash;
mixing the desalted aluminum ash and sodium hydroxide according to the mass ratio of 1: 1-1: 3, putting the mixture into a crucible, placing the crucible into a muffle furnace, and roasting the mixture at 600-800 ℃ for 1-3 h at the heating rate of 5 ℃/min to obtain sodium aluminate clinker;
reacting the sodium aluminate clinker with water at a solid-to-liquid ratio of 1:4 at 80 ℃ for 30min to obtain a sodium aluminate solution;
mixing the micro silicon powder and sodium hydroxide according to the mass ratio of 1: 1-1: 2, putting the mixture into a crucible, placing the crucible into a muffle furnace, and roasting the mixture at 550-750 ℃ for 3-5 h at the heating rate of 5 ℃/min to obtain sodium silicate clinker;
reacting the sodium silicate clinker with water at a solid-to-liquid ratio of 1:5 at 60 ℃ for 30min to obtain a sodium silicate solution;
and (7) mixing the sodium aluminate solution and the sodium silicate solution, adjusting the silica-alumina ratio, performing hydrothermal treatment at 80-120 ℃ for 8-14 h, filtering, drying, and grinding to obtain white powder.
Compared with other technical methods, the invention has the beneficial technical effects that:
(1) the raw materials used in the invention are the aluminum ash and the micro silicon powder, and the aluminum ash and the micro silicon powder are treated, so that the pollution to the environment caused by stacking the aluminum ash and the micro silicon powder is avoided, and the valuable components in the aluminum ash and the micro silicon powder are fully utilized; the 4A molecular sieve is prepared from the aluminum ash and the silica fume, an aluminum source or a silicon source is not required to be added, the resource utilization of industrial wastes is realized, and the method is economical and environment-friendly. (2) The process of the present invention does not require the addition of any directing agent. (3) The production process of the invention has no harmful substances, simple process and low cost. (4) The product produced by the method has good whiteness and high calcium ion exchange capacity.
Drawings
FIG. 1 is a process flow diagram of the present invention, FIG. 2 is an XRD pattern of the 4A molecular sieve prepared in example 1 of the present invention, FIG. 3 is an SEM pattern of the 4A molecular sieve prepared in example 1 of the present invention, FIG. 4 is an XRD pattern of the 4A molecular sieve prepared in example 2 of the present invention, FIG. 5 is an SEM pattern of the 4A molecular sieve prepared in example 2 of the present invention, FIG. 6 is an XRD pattern of the 4A molecular sieve prepared in example 3 of the present invention, and FIG. 7 is an SEM pattern of the 4A molecular sieve prepared in example 3 of the present invention.
Detailed Description
As shown in figure 1, the invention is a method for preparing a 4A molecular sieve by using aluminum ash and micro silicon powder, which comprises the following steps:
weighing 400-600 g of casting aluminum ash, ball-milling and sieving;
step (2), keeping the temperature of the aluminum ash and water at 30-50 ℃ for 1-3 h according to the solid-to-liquid ratio of 1:5, washing a filter cake with water to be neutral, drying and grinding to obtain desalted aluminum ash;
mixing the desalted aluminum ash and sodium hydroxide according to the mass ratio of 1: 1-1: 3, putting the mixture into a crucible, placing the crucible into a muffle furnace, and roasting the mixture at 600-800 ℃ for 1-3 h at the heating rate of 5 ℃/min to obtain sodium aluminate clinker;
reacting the sodium aluminate clinker with water at a solid-to-liquid ratio of 1:4 at 80 ℃ for 30min to obtain a sodium aluminate solution;
mixing the micro silicon powder and sodium hydroxide according to the mass ratio of 1: 1-1: 2, putting the mixture into a crucible, placing the crucible into a muffle furnace, and roasting the mixture at 550-750 ℃ for 3-5 h at the heating rate of 5 ℃/min to obtain sodium silicate clinker;
reacting the sodium silicate clinker with water at a solid-to-liquid ratio of 1:5 at 60 ℃ for 30min to obtain a sodium silicate solution;
and (7) mixing the sodium aluminate solution and the sodium silicate solution, adjusting the silica-alumina ratio, performing hydrothermal treatment at 80-120 ℃ for 8-14 h, filtering, drying, and grinding to obtain white powder.
According to the method, the ball milling time in the step (1) is 1h, and the mesh number is 200 meshes.
According to the method, the water washing temperature in the step (2) is 30-50 ℃, and the water washing time is 1-3 hours.
According to the method, the roasting temperature of the aluminum ash in the step (3) is 600-800 ℃, and the roasting time is 1-3 hours.
According to the method, the reaction temperature in the step (4) is 80 ℃, and the reaction time is 30 min.
According to the method, the roasting temperature of the micro silicon powder in the step (5) is 550-750 ℃, and the roasting time is 3-5 hours.
In the method, the reaction temperature in the step (6) is 60 ℃, and the reaction time is 30 min.
According to the method, the silicon-aluminum ratio in the step (7) is 1.0-3.0, the crystallization temperature is 80-120 ℃, and the crystallization time is 8-12 hours.
The aluminum ash adopted in the embodiment of the invention is from Lanzhou branch of aluminum industry in China, and the main components of the aluminum ash are Al-33.943%, O-29.476%, Mg-14.209%, Na-9.542%, Cl-3.449%, K-2.865%, F-2.579% and other impurities.
The micro silicon powder adopted in the embodiment of the invention is mainly composed of Si-85.556%, C-4.947%, K-8.752%, P-1.108%, Ca-1.089%, S-0.963%, Fe-0.552% and other impurities.
In the embodiment of the invention, the raw materials are aluminum ash and micro silicon powder, any substance with the main components of aluminum and silicon can be used as an aluminum source and a silicon source, and the method of the invention is not limited to the substances.
Example 1: weighing 400g of aluminum ash, ball-milling for 1h, sieving with a 200-mesh sieve, taking 30g of sieved aluminum ash in a three-neck flask, adding 5 times of water by mass, washing for 3h at 30 ℃, filtering, and drying for 12h at 105 ℃ to obtain desalted aluminum ash;
mixing and grinding the obtained desalted aluminum ash and NaOH uniformly according to the mass ratio of 1:1, then placing the mixture into a crucible, and roasting the mixture for 3 hours at 600 ℃ to obtain sodium aluminate clinker;
reacting the sodium aluminate clinker with deionized water according to the liquid-solid ratio of 1:4 at 80 ℃ for 30min to obtain a sodium aluminate solution;
mixing and grinding the micro silicon powder and NaOH uniformly according to the mass ratio of 1:1, then placing the mixture into a crucible, and roasting the mixture for 5 hours at 550 ℃ to obtain sodium silicate clinker;
reacting the sodium silicate clinker with deionized water according to a liquid-solid ratio of 1:5 at 60 ℃ for 30min to obtain a sodium silicate solution;
mixing sodium aluminate solution and sodium silicate solution to make n (SiO)2)/n(Al2O3) =1.0, continuously stirring, crystallizing at 80 deg.C for 12h, filtering, oven drying, grinding to obtain white powderAnd (3) powder.
FIG. 2 shows the XRD pattern of the 4A molecular sieve prepared in example 1 of the present invention. FIG. 3 shows an SEM image of a 4A molecular sieve prepared in example 1 of the present invention.
Example 2: weighing 400g of aluminum ash, ball-milling for 1h, sieving with a 200-mesh sieve, taking 30g of sieved aluminum ash in a three-neck flask, adding 5 times of water by mass, washing for 2h at 40 ℃, filtering, and drying for 12h at 105 ℃ to obtain desalted aluminum ash;
mixing and grinding the obtained desalted aluminum ash and NaOH uniformly according to the mass ratio of 1:2, putting the mixture into a crucible, and roasting the mixture for 2 hours at 700 ℃ to obtain sodium aluminate clinker;
reacting the sodium aluminate clinker with deionized water according to the liquid-solid ratio of 1:4 at 80 ℃ for 30min to obtain a sodium aluminate solution;
mixing and grinding micro silicon powder and NaOH uniformly according to the mass ratio of 1:1.2, then placing the mixture into a crucible, and roasting the mixture for 4 hours at 650 ℃ to obtain sodium silicate clinker;
reacting the sodium silicate clinker with deionized water according to a liquid-solid ratio of 1:5 at 60 ℃ for 30min to obtain a sodium silicate solution;
mixing sodium aluminate solution and sodium silicate solution to make n (SiO)2)/n(Al2O3) And (4) =2.0, crystallizing at 100 ℃ for 10 hours, filtering, drying, and grinding to obtain white powder.
FIG. 4 shows an XRD pattern of the 4A molecular sieve prepared in example 2 of the present invention, and FIG. 5 shows an SEM pattern of the 4A molecular sieve prepared in example 2 of the present invention.
Example 3: weighing 400g of aluminum ash, ball-milling for 1h, sieving with a 200-mesh sieve, taking 30g of sieved aluminum ash in a three-neck flask, adding 5 times of water by mass, washing for 1h at 50 ℃, filtering, and drying for 12h at 105 ℃ to obtain desalted aluminum ash;
mixing and grinding the obtained desalted aluminum ash and NaOH uniformly according to the mass ratio of 1:3, putting the mixture into a crucible, and roasting the mixture for 1h at 800 ℃ to obtain sodium aluminate clinker;
reacting the sodium aluminate clinker with deionized water according to the liquid-solid ratio of 1:4 at 80 ℃ for 30min to obtain a sodium aluminate solution;
mixing and grinding the micro silicon powder and NaOH uniformly according to the mass ratio of 1:1.4, then placing the mixture into a crucible, and roasting the mixture for 3 hours at 750 ℃ to obtain sodium silicate clinker;
reacting the sodium silicate clinker with deionized water according to a liquid-solid ratio of 1:5 at 60 ℃ for 30min to obtain a sodium silicate solution;
mixing sodium aluminate solution and sodium silicate solution to make n (SiO)2)/n(Al2O3) And (4) =3.0, crystallizing at 120 ℃ for 8 hours, filtering, drying, and grinding to obtain white powder.
FIG. 6 shows an XRD pattern of the 4A molecular sieve prepared in example 3 of the present invention, and FIG. 7 shows an SEM pattern of the 4A molecular sieve prepared in example 3 of the present invention.
Claims (8)
1. A method for preparing a 4A molecular sieve by using aluminum ash and micro silicon powder is characterized by comprising the following steps:
weighing 400-600 g of casting aluminum ash, ball-milling and sieving;
step (2), keeping the temperature of the aluminum ash and water at 30-50 ℃ for 1-3 h according to the solid-to-liquid ratio of 1:5, washing a filter cake with water to be neutral, drying and grinding to obtain desalted aluminum ash;
mixing the desalted aluminum ash and sodium hydroxide according to the mass ratio of 1: 1-1: 3, putting the mixture into a crucible, placing the crucible into a muffle furnace, and roasting the mixture at 600-800 ℃ for 1-3 h at the heating rate of 5 ℃/min to obtain sodium aluminate clinker;
reacting the sodium aluminate clinker with water at a solid-to-liquid ratio of 1:4 at 80 ℃ for 30min to obtain a sodium aluminate solution;
mixing the micro silicon powder and sodium hydroxide according to the mass ratio of 1: 1-1: 2, putting the mixture into a crucible, placing the crucible into a muffle furnace, and roasting the mixture at 550-750 ℃ for 3-5 h at the heating rate of 5 ℃/min to obtain sodium silicate clinker;
reacting the sodium silicate clinker with water at a solid-to-liquid ratio of 1:5 at 60 ℃ for 30min to obtain a sodium silicate solution;
and (7) mixing the sodium aluminate solution and the sodium silicate solution, adjusting the silica-alumina ratio, performing hydrothermal treatment at 80-120 ℃ for 8-14 h, filtering, drying, and grinding to obtain white powder.
2. The method for preparing the 4A molecular sieve by using the aluminum ash and the micro silicon powder as claimed in claim 1, wherein the method comprises the following steps: the ball milling time in the step (1) is 1h, and the mesh number is 200 meshes.
3. The method for preparing the 4A molecular sieve by using the aluminum ash and the micro silicon powder as claimed in claim 1, wherein the method comprises the following steps: and (3) washing at 30-50 ℃ for 1-3 h.
4. The method for preparing the 4A molecular sieve by using the aluminum ash and the micro silicon powder as claimed in claim 1, wherein the method comprises the following steps: and (4) roasting the aluminum ash obtained in the step (3) at the temperature of 600-800 ℃ for 1-3 h.
5. The method for preparing the 4A molecular sieve by using the aluminum ash and the micro silicon powder as claimed in claim 1, wherein the method comprises the following steps: the reaction temperature in the step (4) is 80 ℃, and the reaction time is 30 min.
6. The method for preparing the 4A molecular sieve by using the aluminum ash and the micro silicon powder as claimed in claim 1, wherein the method comprises the following steps: and (5) roasting the micro silicon powder at 550-750 ℃ for 3-5 h.
7. The method for preparing the 4A molecular sieve by using the aluminum ash and the micro silicon powder as claimed in claim 1, wherein the method comprises the following steps: the reaction temperature in the step (6) is 60 ℃, and the reaction time is 30 min.
8. The method for preparing the 4A molecular sieve by using the aluminum ash and the micro silicon powder as claimed in claim 1, wherein the method comprises the following steps: the silicon-aluminum ratio in the step (7) is 1.0-3.0, the crystallization temperature is 80-120 ℃, and the crystallization time is 8-12 h.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114890436A (en) * | 2022-05-09 | 2022-08-12 | 南京信息工程大学 | Method for preparing NaA type zeolite material from casting dust and application |
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