Low cost method for rapidly synthesizing ITQ-13 molecular sieve

A molecular sieve, low-cost technology, applied in the field of low-cost and rapid synthesis of ITQ-13 molecular sieve, can solve the problems of long time and achieve the effects of reducing loss, low price, and shortening crystallization time

Active Publication Date: 2013-07-31
TAIYUAN DACHENG ENVIRONMENTAL ENERGY CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Xiaolong Liu et al. (Microporous and Mesoporous Materials 156 (2012) 257–261) announced a method for synthesizing ITQ-13 molecul

Method used

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  • Low cost method for rapidly synthesizing ITQ-13 molecular sieve
  • Low cost method for rapidly synthesizing ITQ-13 molecular sieve
  • Low cost method for rapidly synthesizing ITQ-13 molecular sieve

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] First, weigh 2g of hexamethonium bromide solid and dissolve it in 2ml of deionized water, add 4ml of accelerator (0.3wt%), 0.4gNaOH, 0.05gGeO 2 , 0.2g NaAlO 2 , 0.1g seed crystal, after mixing evenly, slowly add 2.14g white carbon black, add 0.75gNH under stirring 4 F, continue to stir until a uniform silicon germanium gel is formed, then transfer to a stainless steel reactor, and conduct static crystallization at 180°C for 2 days. The molar ratio of the reaction raw materials is 0.30NaOH: 0.015GeO 2 : 0.024Al 2 o 3 : SiO 2 : 0.17 R (hexamethyldiammonium bromide): 0.59NH 4 F: 10H 2 O. After the reaction kettle was cooled to room temperature, the product was suction-filtered, washed with water until neutral, and dried at 100°C to obtain product A. The XRD of product A is attached figure 1 , It can be seen from the figure that product A has the characteristic peak of ITQ-13, and the crystallinity is very high.

Embodiment 2

[0039] First, weigh 2g of hexamethonium bromide and dissolve it in 6ml of deionized water, add 0.01g of accelerator, 0.35g of NaOH, 0.15g of GeO 2 , 0.30g NaAlO 2 , after mixing evenly, add 6.86ml of silica sol (30wt%), add 0.7g of ammonium fluoride under stirring, continue to stir until a uniform silicon germanium gel is formed, then transfer to a polytetrafluoroethylene reactor, 175 ° C static Response 3 days. The molar ratio of the reaction raw materials is 0.27NaOH: 0.044GeO 2 : 0.036Al 2 o 3 : SiO 2 : 0.17R (hexamethyldiammonium bromide): 0.55NH 4 F: 18H 2 O. After the reaction kettle was cooled to room temperature, the product was suction-filtered, washed with water until neutral, and dried at 100°C to obtain product B. The XRD of product B is attached figure 2 , It can be seen from the figure that the product B has the characteristic peak of ITQ-13, and has a high degree of crystallinity without miscellaneous crystals.

Embodiment 3

[0041] First, weigh 2g of hexamethonium bromide and dissolve it in 4ml of deionized water, add 0.01g of accelerator, 0.35g of NaOH, 0.15g of GeO 2 , 0.30g of NaAlO 2 , 0.1g seed crystal, after mixing evenly, add 6.86ml of silica sol, add 0.8g of ammonium fluoride under stirring, continue to stir until a uniform silicon germanium gel is formed, then transfer to a polytetrafluoroethylene reactor, 200 ° C Static reaction for 2 days. The molar ratio of the reaction raw materials is 0.27NaOH: 0.044GeO 2 : 0.036Al 2 o 3 : SiO 2 : 0.17R (hexamethyldiammonium bromide): 0.63NH 4 F: 15H 2 O. After the reactor was cooled to room temperature, the product was suction filtered, washed with water until neutral, and dried at 100°C to obtain product C. The XRD of product C is attached image 3 , it can be seen from the figure that the product C has the characteristic peak of ITQ-13, and has a high degree of crystallinity without miscellaneous crystals.

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Abstract

The invention relates to a low cost method for rapidly synthesizing an ITQ-13 molecular sieve. The method comprises the steps of dissolving a template in deionized water; adding a promoter, an alkali source, germanium dioxide, an aluminium source and crystal seeds; adding a silicon source and a fluorine source successively when the above materials are dissolved; stirring to form a uniform gel; crystallizing for 0.5-8 days under self-generated pressure and at a crystallization temperature of 100-220 DEG C; shock cooling with cold water; fully washing a crystallization product with the deionized water; and drying to obtain molecular sieve raw powder. The synthetic method has the advantages of simpleness, rapidity, easiness and low cost.

Description

technical field [0001] The invention belongs to a method for synthesizing molecular sieves, in particular to a method for rapidly synthesizing ITQ-13 molecular sieves at low cost. Background technique [0002] ITQ-13 molecular sieve is a new three-dimensional microporous material invented by Mobil in 2002, which has intersecting channels of nine-membered rings and ten-membered rings. The straight channels of the nine-membered ring intersect vertically with a set of straight channels of the ten-membered ring to form another set of sinusoidal ten-membered ring channels, which is very similar to the channel type of ZSM-5. The unique structure creates a unique type selectivity, making it suitable for catalytic cracking, aromatization, xylene isomerization, toluene disproportionation, methanol to olefins, alkylation, lubricating oil dewaxing, lubricating oil modification, etc. The reaction showed good catalytic performance. [0003] There are not many synthesis methods of I...

Claims

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Application Information

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IPC IPC(8): C01B39/48C01B37/02
Inventor 李晓峰贾妙娟潘瑞丽徐丹张燕挺窦涛
Owner TAIYUAN DACHENG ENVIRONMENTAL ENERGY CHEM TECH
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