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Method for preparing 4A zeolite from gangue serving as raw material through two-step hydrothermal synthesis

A technology of hydrothermal synthesis and coal gangue, which is applied in the direction of A-type crystalline aluminosilicate zeolite, crystalline aluminosilicate zeolite, etc., can solve the problems of weak operability, high cost, weak operability, etc.

Pending Publication Date: 2018-09-04
SHAANXI NORMAL UNIV
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  • Summary
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Problems solved by technology

[0004] At present, the main method of using coal gangue as raw material to synthesize 4A zeolite is the alkali fusion hydrothermal synthesis method, such as the Chinese patent with the publication number CN1346794A "Method for preparing A-type zeolite by high-temperature alkali fusion-hydrothermal crystallization using coal gangue as raw material" , the coal gangue is alkali-fused at high temperature in an alkali flux, and then water is added to the alkali-fused gangue to crystallize and synthesize zeolite, wherein an aluminum source needs to be supplemented to adjust the silicon-aluminum ratio; for example, the Chinese patent "a kind of coal The method for preparing A-type zeolite from gangue "reacts calcined coal gangue and alkali flux at high temperature, and the alkali melt is dissolved in water to remove iron and then added aluminum salt to crystallize to synthesize zeolite. Although this method is simple and easy, silicon Aluminum source, but still need to supplement aluminum salt, the ratio is difficult to control, and the operability is weak; such as the Chinese patent "a method for preparing high whiteness A-type zeolite from coal gangue" with the publication number CN101214973A, after the coal gangue is alkali-fused Water-soluble, add aluminum salt aging hydrothermal crystallization to synthesize zeolite, add complexing agent to whiten during the crystallization process, although this method synthesizes high-purity and high-whiteness A-type zeolite, but adding aluminum salt and complexing agent causes High cost and weak operability

Method used

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  • Method for preparing 4A zeolite from gangue serving as raw material through two-step hydrothermal synthesis
  • Method for preparing 4A zeolite from gangue serving as raw material through two-step hydrothermal synthesis
  • Method for preparing 4A zeolite from gangue serving as raw material through two-step hydrothermal synthesis

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Experimental program
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Effect test

Embodiment 1

[0037] (1) After the coal gangue raw material is dried, crushed and ground, sieved to 300 mesh to obtain the coal gangue powder;

[0038] (2) Put the coal gangue powder in a muffle furnace for calcination at 750°C for 2 hours. After cooling, the mass ratio of sodium carbonate and gangue is 1.3. Mix the sodium carbonate and gangue powder evenly and place them in the muffle furnace at 830°C. Calcined at ℃ for 1 h to obtain a molten mixture;

[0039] (3) After cooling, add deionized water to the molten mixture at a liquid-solid ratio of 30mL / g, stir in a magnetic stirrer at 40°C for 1 hour, filter to obtain filter residue, and dry it in an oven;

[0040] (4) Mix the dried filter residue with sodium hydroxide solution, the concentration of sodium hydroxide solution is 3mol / L, the liquid-solid ratio is 20mL / g, stir at 60°C for 1h in a magnetic stirrer, filter to obtain the filtrate, Stir the filtrate at 60°C for 2 hours to age to obtain the precursor;

[0041] (5) Place the aging...

Embodiment 2

[0043] (1) After the coal gangue raw material is dried, crushed and ground, sieved to 300 mesh to obtain the coal gangue powder;

[0044] (2) Put the coal gangue powder in a muffle furnace for calcination at 700°C for 2 hours. After cooling, the mass ratio of sodium carbonate and gangue is 1.4. Mix the sodium carbonate and gangue powder evenly and place them in the muffle furnace at 830°C. Calcined at ℃ for 1 h to obtain a molten mixture;

[0045] (3) After cooling, add deionized water to the molten mixture at a liquid-solid ratio of 20mL / g, stir in a magnetic stirrer at 40°C for 1 hour, filter to obtain a filter residue, and dry it in an oven;

[0046] (4) Mix the dried filter residue with sodium hydroxide solution, the concentration of sodium hydroxide solution is 2.8mol / L, the liquid-solid ratio is 20mL / g, stir at 40°C for 1h in a magnetic stirrer, and filter to obtain the filtrate , the filtrate was aged at 70°C for 2h to obtain the precursor;

[0047] (5) Place the aging ...

Embodiment 3

[0049] (1) After the coal gangue raw material is dried, crushed and ground, sieved to 300 mesh to obtain the coal gangue powder;

[0050] (2) Put the coal gangue powder in a muffle furnace for calcination at 800°C for 2 hours. After cooling, the mass ratio of sodium carbonate and gangue is 1.5. Mix the sodium carbonate and coal gangue powder evenly and place them in the muffle furnace at 830°C. Calcined at ℃ for 2h to obtain a molten mixture;

[0051] (3) After cooling, add deionized water to the molten mixture at a liquid-solid ratio of 50mL / g, stir in a magnetic stirrer at 40°C for 1 hour, filter to obtain filter residue, and dry it in an oven;

[0052] (4) Mix the dried filter residue with sodium hydroxide solution, the concentration of sodium hydroxide solution is 2.5mol / L, the liquid-solid ratio is 20mL / g, stir at 50°C for 1h in a magnetic stirrer, and filter to obtain the filtrate , the filtrate was aged at 65°C for 2h to obtain the precursor;

[0053] (5) Place the ag...

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Abstract

The invention discloses a method for preparing 4A zeolite from gangue serving as a raw material through two-step hydrothermal synthesis. The method comprises the following steps: firstly, crushing andgrinding gangue, performing thermal activation pretreatment, mixing the gangue subjected to thermal activation and sodium carbonate uniformly, and melting at high temperature to obtain a molten mixture; secondly, mixing the molten mixture and water under the water solution condition to dissolve out sodium silicate, filtering to obtain filter residues and drying the filter residues; thirdly, completely stirring the dried filter residues and a sodium hydroxide solution under the alkali dissolution condition, filtering to obtain a silicon aluminum solution, and ageing the silicon aluminum solution to obtain a precursor; finally, performing hydrothermal crystallization treatment on the precursor, and filtering, water-washing and drying to obtain the 4A zeolite. According to the synthesis method, the gangue serves as the raw material, the gangue is subjected to high-end resource-based development and utilization, and the gangue does not need to be subjected to acid leaching pretreatment, so that secondary pollution on the environment is reduced; and an aluminum source does not need to be added in the synthesis process, so the method is simple, high in operability and low in cost.

Description

technical field [0001] The invention relates to a method for preparing 4A zeolite, in particular to a method for hydrothermally synthesizing 4A zeolite in two steps using coal gangue as a raw material. Background technique [0002] 4A zeolite is a kind of artificial zeolite synthesized by humans. It does not pollute the environment, has strong ion exchange capacity and adsorption performance, and has great application potential in general daily use, petrochemical, smelting and other industries and high-tech fields. [0003] At present, there are three main raw materials for synthesizing 4A zeolite: chemical raw materials, natural minerals and industrial waste. Chemical raw materials are raw materials for total chemical synthesis and auxiliary raw materials for semi-synthetic methods. They mainly include sodium hydroxide, water glass, sulfuric acid, alumina, etc., and their cost is high and their operation is complicated. Natural minerals are based on SiO 2 and Al 2 o 3 M...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/16C01B39/14
CPCC01B39/14C01B39/16C01P2002/72C01P2004/03
Inventor 卢新卫王倩石栋奇
Owner SHAANXI NORMAL UNIV
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