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A kind of method utilizing beta molecular sieve mother liquor to synthesize beta molecular sieve

A technology of β molecular sieve and mother liquor, which is applied in the field of synthesizing β molecular sieve by using β molecular sieve mother liquor, can solve the problems of high initial gel viscosity of the solution, waste of raw materials, difficulty in stirring, etc., shorten crystallization induction period, reduce synthesis cost, shorten crystallization The effect of chemical cycle

Active Publication Date: 2016-03-02
SHANDONG QILU HUAXIN HIGH TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] In the process of synthesizing β molecular sieve by hydrothermal method, the template agent plays a guiding role. If the amount of template agent added is small, the initial gel viscosity of the solution is high, and it is difficult to stir, resulting in unstable product quality; some production processes increase the product quality by prolonging the crystallization time. The stability of quality, the crystallization time is usually about 50 hours to 15 days, and the crystallization time is too long, which seriously increases the production cycle of β molecular sieve products. Therefore, in industrial production, a large amount of template agent and excessive silicon source are generally used. Promote the realization of the crystallization process, so the β molecular sieve mother liquor after crystallization contains a large amount of unreacted silicon source and template agent. If the mother liquor is directly discharged, it will not only lead to waste of raw materials, but also lead to COD and COD in water. Ammonia nitrogen NH3-N seriously exceeds the standard, causing pollution to the environment

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0051] A method for synthesizing a β molecular sieve using a β molecular sieve mother liquor, the steps are as follows:

[0052] (1) For the SiO of the β molecular sieve mother liquor in the mother liquor recovery storage tank 2 and Na 2 O content analysis, SiO in β molecular sieve mother liquor 2 The content is 4.76%, Na 2 The content of O is 1.11%, and the β molecular sieve mother liquor is heated to 45 °C; the gel accelerator and water are mixed into a solution, and added to the glue tank for later use. The gel accelerator is polyethylene glycol and polyferric sulfate by mass The ratio is 3:1 mixed composition;

[0053] (2) Mix dilute sulfuric acid with a mass fraction of 8% and β molecular sieve mother liquor heated to a temperature of 45°C into the gel-forming tank containing the gel accelerator solution in step (1) to obtain a sol Standby, the pH when the β molecular sieve mother liquor and dilute sulfuric acid are mixed is 6.0, and the quality of the gel accelerator...

Embodiment 2

[0060] A method for synthesizing a β molecular sieve using a β molecular sieve mother liquor, the steps are as follows:

[0061] (1) For the SiO of the β molecular sieve mother liquor in the mother liquor recovery storage tank 2 and Na 2 O content analysis, SiO in β molecular sieve mother liquor 2 The content is 4.50%, Na 2 The content of O is 1.21%, and the β molecular sieve mother liquor is heated to 55 ° C; the gel accelerator and water are mixed into a solution, and added to the glue tank for later use. The gel accelerator is polyethylene glycol and polyferric sulfate by mass The ratio is 5:1 mixed composition;

[0062] (2) Mix dilute sulfuric acid with a mass fraction of 12% and β molecular sieve mother liquor heated to a temperature of 55°C into the gel forming tank containing the gel accelerator solution in step (1) to obtain a sol Standby, the pH when the β molecular sieve mother liquor and dilute sulfuric acid are mixed is 8.0, and the quality of the gel accelerat...

Embodiment 3

[0069] A method for synthesizing a β molecular sieve using a β molecular sieve mother liquor, the steps are as follows:

[0070] (1) For the SiO of the β molecular sieve mother liquor in the mother liquor recovery storage tank 2 and Na 2 O content analysis, SiO in β molecular sieve mother liquor 2 The content is 4.65%, Na 2 The content of O is 1.15%, and the β molecular sieve mother liquor is heated to 50°C; the gel accelerator and water are mixed into a solution, and added to a glue tank for later use, and the gel accelerator is polyethylene glycol and polyferric sulfate by mass The ratio is 4:1 mixed composition;

[0071] (2) Mix dilute sulfuric acid with a mass fraction of 9% and β molecular sieve mother liquor heated to a temperature of 48°C into the gel-forming tank containing the gel accelerator solution in step (1) to obtain a sol Standby, the pH when the β molecular sieve mother liquor and dilute sulfuric acid are mixed is 7.0, and the quality of the gel accelerato...

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Abstract

The invention discloses a method for synthesizing a beta molecular sieve by utilizing a beta molecular sieve mother solution. The method comprises the following steps: performing equal-pH coprecipitation on a crystallized mother solution and dilute acid parallel flow to synthesize silica gel in bottom water containing a gel accelerator, adding a template-agent-containing BETA molecular sieve milled by a colloid mill to serve as a seed crystal, and performing hydrothermal crystallization to synthesize the BETA molecular sieve according to the ratio of low addition amount of organic template agents. According to the production method disclosed by the invention, the batching amount of a fresh silicon source and the template agent in beta molecular sieve synthesis is reduced, and due to the existence of a molecular sieve microcrystal, the crystallization process of the molecular sieve is accelerated, and the crystallization period is shortened. Moreover, the synthesized beta molecular sieve is high in crystallinity degree, the milled seed crystal contains lots of micro grains and organic template agents with secondary structures, the crystallization induction period can be effectively shortened, and the use amount of the template agent is reduced. Therefore, the synthetic cost is greatly reduced.

Description

technical field [0001] The invention relates to the technical field of molecular sieve synthesis, in particular to a method for synthesizing a beta molecular sieve mother liquor. Background technique [0002] In the process of synthesizing β molecular sieve by hydrothermal method, the template agent plays a guiding role. If the amount of template agent added is small, the initial gel viscosity of the solution is high, and it is difficult to stir, resulting in unstable product quality; some production processes increase the product quality by prolonging the crystallization time. The stability of quality, the crystallization time is usually about 50 hours to 15 days, and the crystallization time is too long, which seriously increases the production cycle of β molecular sieve products. Therefore, in industrial production, a large amount of template agent and excessive silicon source are generally used. Promote the realization of the crystallization process, so the β molecular s...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B39/04
CPCC01B39/04
Inventor 刘环昌明曰信陈文勇刘伟耿庆琳张勇彭立
Owner SHANDONG QILU HUAXIN HIGH TECH
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