Method for preparing meso-microporous pure silicon molecular sieve with high specific surface area based on silica white

A high specific surface area, pure silicon molecular sieve technology, applied in molecular sieve compounds, molecular sieves and alkali exchange compounds, chemical instruments and methods, etc., to achieve the effect of large pore volume, controllable specific surface area, and good application prospects

Active Publication Date: 2012-06-20
BEIJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there is no literature or patent report on the synthesis of high specific surface area pure silicon molecular sieves with mesoporous and microporous (mesoporous) structures using white carbon black as a silicon source.

Method used

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  • Method for preparing meso-microporous pure silicon molecular sieve with high specific surface area based on silica white
  • Method for preparing meso-microporous pure silicon molecular sieve with high specific surface area based on silica white
  • Method for preparing meso-microporous pure silicon molecular sieve with high specific surface area based on silica white

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Embodiment 1: Take by weighing 1.067g NaOH, 4.533g cetyltrimethylammonium hydroxide (CTAOH) and 1.23g triblock copolymer (F127), be placed in 150mL beaker, add 80mL deionized water, in After stirring at 50 °C for 1 h, a homogeneous solution was formed. Add 1.5g of white carbon black under strong stirring, continue to stir at room temperature for 1h, transfer the obtained amorphous gel to a 100mL reactor lined with polytetrafluoroethylene, seal it, and conduct hydrothermal treatment at 120°C for 12h, and the hydrothermal treatment is completed Afterwards, the mixture was washed, suction-filtered, and dried at 80°C for 12h, then the obtained white solid powder was placed in a muffle furnace, raised to 550°C at a rate of 1°C / min and kept at this temperature for 4h, and finally A mesoporous silica molecular sieve with a high specific surface area is obtained. The specific surface area is 1090m 2 / g, the pore volume is 0.89cm 3 / g, the mesopore diameter is 3.3nm.

Embodiment 2

[0016] Example 2: Weigh 1.067g NaOH, 4.533g CTAOH and 1.23g F127, place in a 150mL beaker, add 80mL deionized water, and stir at 50°C for 1 hour to form a homogeneous solution. Add 1.5g of white carbon black under strong stirring, continue to stir at room temperature for 1h, transfer the obtained amorphous gel to a 100mL reaction kettle lined with polytetrafluoroethylene and seal it, and hydrothermally treat it at 120°C for 24h, and the hydrothermal treatment ends Afterwards, the mixture was washed, suction-filtered, and dried at 80°C for 12h, then the obtained white solid powder was placed in a muffle furnace, raised to 550°C at a rate of 1°C / min and kept at this temperature for 4h, and finally A mesoporous silica molecular sieve with a high specific surface area is obtained. The specific surface area is 1405m 2 / g, the pore volume is 0.76cm 3 / g, the mesopore diameter is 2.2nm.

Embodiment 3

[0017] Example 3: Weigh 1.067g NaOH, 4.533g CTAOH and 1.23g F127, place in a 150mL beaker, add 80mL deionized water, and stir at 50°C for 1 hour to form a homogeneous solution. Add 1.5g of white carbon black under strong stirring, continue to stir at room temperature for 1h, transfer the obtained amorphous gel to a 100mL reaction kettle lined with polytetrafluoroethylene, seal it, and conduct hydrothermal treatment at 120°C for 48h, and the hydrothermal treatment is completed Afterwards, the mixture was washed, suction-filtered, and dried at 80°C for 12h, then the obtained white solid powder was placed in a muffle furnace, raised to 550°C at a rate of 1°C / min and kept at this temperature for 4h, and finally A mesoporous silica molecular sieve with a high specific surface area is obtained. The specific surface area is 1186m 2 / g, the pore volume is 0.74cm 3 / g, the mesopore diameter is 2.5nm.

[0018] The XRD spectrogram of the mesoporous silica molecular sieve sample obtain...

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Abstract

The invention discloses a method for preparing a meso-microporous pure silicon molecular sieve with high specific surface area based on silica white and belongs to the technical field of molecular sieves. The method comprises the following steps of: mixing deionized water, CTAOH (cetyl trimethyl ammonium hydroxide), F127 and sodium hydroxide, stirring at 50 DEG C to form a clear solution; adding silica white; stirring for 1 hour at room temperature to obtain an amorphous gel; transferring the gel to a polytetrafluoroethylene-lined reaction kettle, wherein the molar ratio of NaOH to SiO2 to CTAOH to F127 to H2O is 1:0.94:0.56:0.0036:166.30; performing hydrothermal treatment at 120 DEG C for 12 to 48 hours; subjecting the mixture to washing, suction-filtering and drying; and putting the resulting molecular sieve in a muffle furnace, and heating up to 550 DEG C at a rate of 1 DEG C and maintaining for 4 hours. The molecular sieve prepared by the invention is advantageous in larger specific surface area and pore volume, uniform pore distribution and adjustable pore diameter.

Description

technical field [0001] The present invention relates to a preparation method of mesoporous silica molecular sieve with high specific surface area, in particular to the preparation of mesoporous silica with high specific surface area by using commercially available white carbon black with low specific surface area as silicon source The molecular sieve method belongs to the technical field of molecular sieves. Background technique [0002] The advantages of mesoporous molecular sieves lie in their adjustable pore size, stable framework structure, easy-to-modify inner surface, amorphous framework with a certain wall thickness and easy doping, and high specific surface area, which can be used as functional materials, adsorbents , catalyst and carrier, not only make up for the deficiency of microporous zeolite molecular sieve, but also use ordered mesopores as "microreactors" to prepare nanomaterials with special optical, electrical, magnetic and other properties. Therefore, in t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/00C01B37/00
Inventor 戴洪兴刘雨溪邓积光张磊石凤娟赵振璇
Owner BEIJING UNIV OF TECH
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