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Rapid synthesis of high crystallinity sapo-34 molecular sieves

A SAPO-34, high crystallinity technology, applied in the direction of molecular sieve and alkali exchange phosphate, molecular sieve characteristic silicoaluminophosphate, etc., can solve the problems of long crystallization time, low cost, low crystallinity of molecular sieve, etc., to achieve the required The effect of short time, high crystallinity and excellent thermal stability

Active Publication Date: 2016-02-03
WUXI WEIFU ENVIRONMENT PROTECTION CATALYST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The present invention aims at using triethylamine, tetraethylammonium hydroxide and other templates to synthesize SAPO-34 molecular sieves with low crystallinity and long crystallization time, etc., and adopts relatively less volatile organic amines as auxiliary templates. Synthesis of mixed-template molecular sieves with high crystallinity and low cost in a short period of time

Method used

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  • Rapid synthesis of high crystallinity sapo-34 molecular sieves
  • Rapid synthesis of high crystallinity sapo-34 molecular sieves

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Example 1, (1) Mixing: first fully stir 1 mol of pseudo-boehmite in 50 mol of deionized water, then slowly add 0.9 mol of phosphoric acid with a mass concentration of 84% to completely peptize the pseudo-boehmite; After completion, add 0.6mol40wt.% silica sol and stir evenly, then add 2mol tetraethylammonium hydroxide and 0.5mol diethylenetriamine auxiliary templating agent, and stir vigorously;

[0019] (2) Crystallization: After stirring for 4 hours, put it into a stainless steel reaction kettle lined with tetrafluoroethylene or p-polystyrene; put the reaction kettle at 190 o C crystallized for 2 days;

[0020] (3) Drying and roasting: After the crystallization is completed, the obtained product is centrifuged and washed 5 times, and the obtained solid product is dried in an oven at 90°C for 4 hours; then the dried product is heated to 550°C at 5°C / min and roasted for 6 hours to obtain The product is a high crystallinity SAPO-34 molecular sieve synthesized rapidly. ...

Embodiment 2

[0023] Example 2, (1) Mixing: First, fully stir 1 mol of pseudo-boehmite in 60 mol of deionized water, then slowly add 0.9 mol of phosphoric acid with a mass concentration of 86% to completely peptize the pseudo-boehmite; After completion, add 0.5mol40wt.% silica sol and stir evenly, then add 2.5mol triethylamine and 0.4mol diethylenetriamine mixed tablet and stir vigorously;

[0024] (2) Crystallization: Stir the mixed solution in step (1) for 5 hours and put it into a stainless steel reactor lined with tetrafluoroethylene or p-polystyrene; crystallize the reactor at 195°C for 1.5 days;

[0025] (3) Drying and roasting: After the crystallization is completed, the obtained product is centrifuged and washed 5 times, and the obtained solid product is dried in an oven at 90°C for 4 hours; then the dried product is heated to 550°C at 3°C / min and roasted for 6 hours to obtain The product is a high crystallinity SAPO-34 molecular sieve synthesized rapidly.

[0026] figure 2 The S...

Embodiment 3

[0027] Example 3, (1) Mixing: First, fully stir 1 mol of pseudo-boehmite in 50 mol of deionized water, then slowly add 0.9 mol of phosphoric acid with a mass concentration of 85% to completely peptize the pseudo-boehmite; After completion, add 0.6mol fumed silicon and stir evenly, then add 2mol tetraethylammonium hydroxide and 0.5mol diethylenetriamine auxiliary templating agent and stir vigorously;

[0028] (2) Crystallization: Stir the mixed solution in step (1) for 4 hours and put it into a stainless steel reactor lined with tetrafluoroethylene or p-polystyrene; crystallize the reactor at 190°C for 2 days;

[0029] (3) Drying and roasting: After the crystallization is completed, the obtained product is centrifuged and washed 5 times, and the obtained solid product is dried in an oven at 90°C for 4 hours; then the dried product is heated to 650°C at 0.5°C / min and roasted for 3 hours to obtain The product is a high crystallinity SAPO-34 molecular sieve synthesized rapidly.

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Abstract

The invention relates to a preparation method for a molecular sieve. The SAPO-34 molecular sieve with a high crystallinity is obtained in a relatively short time by adopting a mixed template agent. The preparation method comprises the following steps: stirring pseudo-boehmite in deionized water fully; slowly adding phosphoric acid to peptize the pseudo-boehmite fully; adding silicon source to stir uniformly; adding an organic amine mixed template agent and stirring tempestuously; enclosing the obtained solution into a stainless steel reaction kettle with a tetrafluoroethylene or para-polyphenyl inner lining after stirring; conducting crystallization on the reaction kettle; taking out and cooling the reaction kettle after crystallization; washing the product until the washing solution is neutral; drying the obtained solid product in a drying oven; torrefying the obtained dried product to obtain the molecular sieve of the product. The template agent for synthesizing the molecular sieve is inexpensive, easy to obtain, and low in poisonousness; the molecular sieve is adjustable in ratio of silicate to aluminum; the molecular sieve after torrefying is high in crystallinity, specific surface area, and hydrothermal stability.

Description

technical field [0001] The invention relates to a preparation method for rapidly synthesizing SAPO-34 molecular sieve with high crystallinity at low cost, and belongs to the field of inorganic chemical synthesis and preparation. Background technique [0002] SAPO-34 is a microporous molecular sieve with Chabazite (CHA) structure containing silicon, phosphorus, aluminum and oxygen. Due to its good thermal stability, suitable acidity and pore structure, it is especially suitable for methanol-to-olefins (MethanolToOlefins, MTO) and vehicle exhaust NOx Selective Catalytic Reduction (NOxSelectiveCatalyticReduction, NOx-SCR) reactions. A key that limits its large-scale application is that the tetraethylammonium hydroxide template required in the synthesis process is expensive, and it takes a long time to synthesize SAPO-34 with high crystallinity; It will be deactivated due to rapid coking, and when used in NOx-SCR reaction, the molecular sieve skeleton collapses easily under the...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B39/54C01B37/08
Inventor 贾莉伟金炜阳岳军赵德鹏王家明
Owner WUXI WEIFU ENVIRONMENT PROTECTION CATALYST
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