Method for synthesizing 4A molecular sieve by double crystallization

A chemical synthesis and molecular sieve technology, applied in the direction of molecular sieve compounds, chemical instruments and methods, molecular sieve characteristic silicates, etc., can solve the problems of long synthesis time, long activation time, and complicated steps, so as to reduce synthesis cost and reduce the degree of agglomeration , the effect of improving yield and synthesis efficiency

Inactive Publication Date: 2019-02-01
KUNMING UNIV OF SCI & TECH
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  • Abstract
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  • Claims
  • Application Information

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Problems solved by technology

[0003] The synthesis of 4A molecular sieve traditionally adopts the hydrothermal synthesis method, but the synthesis time is long, the steps are complicated, and the yield is not high, which limits its development.
The molecular sieve synthesized by the alkali fusion method does not contain the crystal phase of mullite and quartz, and improves the yield of zeolite. By adjusting the ratio of silicon to aluminum, a product with high practical value and purity can be obtained, but its disadvantages are longer activation t...

Method used

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  • Method for synthesizing 4A molecular sieve by double crystallization
  • Method for synthesizing 4A molecular sieve by double crystallization
  • Method for synthesizing 4A molecular sieve by double crystallization

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Embodiment 1

[0020] A method for synthesizing 4A molecular sieves by twin crystallization, the specific steps are as follows:

[0021] (1) First pretreat the coal gangue. The pretreatment method is as follows: heat preservation at 1000°C for 9 hours, pickle the calcined product with 1mol / L hydrochloric acid, and then dry it naturally. Then, according to the mass volume ratio g:mL of 1:6 Ratio, mix the pretreated coal gangue with NaOH solution with a concentration of 0.1mol / L, stir at a constant speed of 250r / min for 600min, vacuum filter and separate to obtain the supernatant;

[0022] (2) Mix Al powder and NaOH solution with a concentration of 0.1mol / L according to the molar ratio of Al and NaOH of 1:5, and stir until the aluminum powder is completely dissolved to obtain a mixed solution;

[0023] (3) Mix the supernatant obtained in step (1) with the mixed solution obtained in step (2) at a volume ratio of 1:1, and place the mixture in an oil bath at 70°C for 5 hours, remove the white flo...

Embodiment 2

[0027] A method for synthesizing 4A molecular sieves by twin crystallization, the specific steps are as follows:

[0028] (1) First pretreat the coal gangue. The pretreatment method is: heat preservation at 900°C for 12 hours, pickle the calcined product with 1mol / L hydrochloric acid and then dry it naturally, and then according to the mass volume ratio g:mL of 1:12 Ratio, mix the pretreated coal gangue with NaOH solution with a concentration of 1mol / L, stir at a constant speed of 350r / min for 40min, vacuum filter and separate to obtain the supernatant;

[0029] (2) Mix Al powder and NaOH solution with a concentration of 1mol / L according to the molar ratio of Al and NaOH of 1:10, and stir until the aluminum powder is completely dissolved to obtain a mixed solution;

[0030] (3) Mix the supernatant obtained in step (1) with the mixed solution obtained in step (2) at a volume ratio of 1:2, and place the mixture in an oil bath at 100°C for 3 hours, remove the white flocs The sup...

Embodiment 3

[0033] A method for synthesizing 4A molecular sieves by twin crystallization, the specific steps are as follows:

[0034] (1) First pretreat the coal gangue. The pretreatment method is: heat preservation at 950°C for 10 hours, pickle the calcined product with 1mol / L hydrochloric acid and then dry it naturally, and then according to the mass volume ratio g:mL of 1:10 Ratio, mix the pretreated gangue with NaOH solution with a concentration of 2mol / L, stir at a constant speed of 300r / min for 400min, vacuum filter and separate to obtain the supernatant;

[0035] (2) Mix Al powder and NaOH solution with a concentration of 2mol / L according to the molar ratio of Al and NaOH of 1:6, and stir until the aluminum powder is completely dissolved to obtain a mixed solution;

[0036] (3) Mix the supernatant obtained in step (1) with the mixed solution obtained in step (2) at a ratio of 1:3 by volume, and place the mixed solution in an oil bath at 140°C for 2 hours, remove the white flocs Th...

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Abstract

The invention discloses a method for synthesizing a 4A molecular sieve by double crystallization. The method comprises the following steps: pre-treating a raw material, sufficiently mixing the raw material with a NaOH solution, and performing stirring at constant speed; performing filtering and separating under a vacuum state to obtain supernate; mixing and stirring Al powder and the NaOH solutionuntil the Al powder is completely dissolved to obtain a mixed solution; mixing the mixed solution with the supernate, performing standing at constant temperature, and performing filtering to obtain aclear solution; and aging the clear solution under a room temperature condition, performing microwave assisted hydrothermal double crystallization to obtain the 4A molecular sieve. According to the method, the yield and synthesizing efficiency can be greatly improved, cost can be reduced, and industrial synthesizing application of the 4A molecular sieve can be benefited.

Description

technical field [0001] The invention belongs to the technical field of high-value utilization of industrial waste, and in particular relates to a method for synthesizing 4A molecular sieves by twin crystallization. Background technique [0002] Coal gangue is the waste ore extracted in the process of coal mining, and a large amount of it has not been used at present. The discharge and accumulation of these coal gangue not only takes up a large amount of cultivated land, pollutes the environment, but also causes harm to crops and human beings, and has become a problem that the coal industry needs to solve urgently. Biomass ash is the ash left after the biomass briquette fuel is fully burned, and a large amount of biomass ash will pollute the environment. 4A molecular sieve is a kind of synthetic molecular sieve, which is widely used in petroleum, chemical industry, metallurgy, electronic technology, medical and health departments in my country. [0003] The synthesis of 4A ...

Claims

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Application Information

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IPC IPC(8): C01B39/14C01B37/00
CPCC01B37/005C01B39/14
Inventor 李艳红李根明訾昌毓张静赵文波
Owner KUNMING UNIV OF SCI & TECH
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