Method for recycling molecular sieve mother solution

A molecular sieve and mother liquor technology, which is applied in molecular sieve catalysts, chemical instruments and methods, chemical/physical processes, etc., can solve the problems of increasing water-to-silicon ratio and reducing the yield of single-pot synthesis of molecular sieves, and achieve the effect of saving consumption

Inactive Publication Date: 2011-09-21
EAST CHINA NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

If you continue to add more water-containing silicon source, aluminum source or template solution in the molecular sieve synthesis

Method used

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  • Method for recycling molecular sieve mother solution
  • Method for recycling molecular sieve mother solution
  • Method for recycling molecular sieve mother solution

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] With 790 milliliters of crystallization mother liquors in comparative example 1 (SiO 2 : 65.0g / L; Na 2 O: 38.8g / L) mixed with 500ml of water, add 4.7g of sodium hydroxide, 22.8g of sodium metaaluminate and 8.8g of tetrapropylammonium bromide to dissolve, add 360g of silica gel (Qingdao Ocean Chemical Factory, 40-120 order, the burnt residual solid content is 95%), transferred to a 2-liter autoclave after stirring evenly, crystallized at 175°C for 24 hours, filtered, washed and dried after cooling, the XRD crystal phase diagram of the product obtained is as follows: figure 2As shown, it is a ZSM-5 structure, its relative crystallinity is 102%, and its BET surface area is 340m2 / g. The filtered crystallization mother liquor was collected for the synthesis in Example 2. The yield of the obtained ZSM-5 molecular sieve sample is about 92% relative to the solid silicon source.

Embodiment 2

[0029] With 898 milliliters of crystallization mother liquors in embodiment 1 (SiO 2 : 46.9g / L; Na 2 O: 23.5g / L) mixed with 300ml of water, add 14.4g of sodium hydroxide, 22.8g of sodium metaaluminate and 8.8g of tetrapropylammonium bromide to dissolve, add 360g of silica gel (Qingdao Ocean Chemical Factory, 40-120 purpose, the residual solid content after burning is 95%), transferred to a 2-liter autoclave after stirring evenly, crystallized at 175°C for 24 hours, filtered, washed and dried after cooling, the XRD crystal phase diagram of the product obtained was the same as figure 2 Similarly, the ZSM-5 structure has a relative crystallinity of 105%. The filtered crystallization mother liquor was collected for the synthesis of ZSM-5. The yield of the obtained ZSM-5 molecular sieve sample is about 93% relative to the solid silicon source.

Embodiment 3

[0031] With 820 milliliters of crystallization mother liquors in embodiment 2 (SiO 2 : 46.0g / L; Na 2 O: 39.8g / L) was mixed with 400 ml of water, 14.4 g of sodium hydroxide, 22.8 g of sodium metaaluminate and 8.8 g of tetrapropylammonium bromide were added to dissolve, and 360 g of silica gel (Qingdao Ocean Chemical Factory, 40-120 purpose, the residual solid content after burning is 95%), transferred to a 2-liter autoclave after stirring evenly, crystallized at 175°C for 24 hours, filtered, washed and dried after cooling, the XRD crystal phase diagram of the product obtained was the same as figure 2 Similarly, the ZSM-5 structure has a relative crystallinity of 105%. The filtered crystallization mother liquor was collected for the synthesis of ZSM-5. The yield of the obtained ZSM-5 molecular sieve sample is about 93% relative to the solid silicon source.

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Abstract

The invention discloses a method for recycling molecular sieve crystallization mother solution, which comprises the following steps of: (1) preparing a material for synthesizing a molecular sieve, gelatinizing, crystallizing, filtering, and collecting all molecular sieve crystallization mother solution; (2) using the obtained all molecular sieve crystallization mother solution for synthesis of the molecular sieve directly, mixing with a solid silicon source, an aluminum source and alkali, and adding or not adding molecular sieve seed crystals and a template agent to obtain a reaction mixture; and (3) crystallizing the obtained reaction mixture according to the conventional hydrothermal method, obtaining a filter cake, namely a molecular sieve product, and filtering and collecting all molecular sieve crystallization mother solution, wherein the obtained all molecular sieve crystallization mother solution can be circularly utilized according to the sequence of steps (2) and (3). In the synthesis of the molecular sieve, alkaline waste liquor is not discharged basically, the total silicon utilization rate is more than or equal to 90 percent, and the yield of the molecular sieve product is over 90 percent.

Description

technical field [0001] The invention relates to the technical field of molecular sieve synthesis, and more specifically relates to a method for recycling molecular sieve synthesis by using the molecular sieve crystallization mother liquor synthesized by silicon-aluminum molecular sieves. Background technique [0002] Molecular sieves are important catalysts or catalyst active components in petroleum refining and chemical processes. In the prior art, when synthesizing silica-alumina molecular sieves, silicon-containing compounds (water glass, silica sol, and organosilicon ester, etc.), aluminum-containing compounds (hydrated alumina, aluminum salts, etc.), alkalis (sodium hydroxide, potassium hydroxide, etc.) ) and water in an appropriate proportion, adding or not adding an organic template and heating in an autoclave for a certain period of time to obtain molecular sieve crystals. Under alkaline conditions, some silicon will remain in the mother liquor and not be fully util...

Claims

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Application Information

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IPC IPC(8): C01B39/02C01B39/04B01J29/06
Inventor 王一萌刘树萍薛腾何鸣元
Owner EAST CHINA NORMAL UNIV
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