Preparation method for optical transparent ordered inter-aperture silica single block

A mesoporous silicon oxide, optically transparent technology, applied in the directions of silicon oxide, silicon dioxide, chemical instruments and methods, etc., can solve the problems of high cost, difficult industrial production, long processing time, etc., achieve low cost, reduce drying and cracking , the effect of short production cycle

Inactive Publication Date: 2005-08-17
WUHAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

These methods either require special equipment or reagents, or the processing time is too long and the cost is high, which has caused great difficulties in its industrial production in batches.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Dissolve 2.0g of Brij56 in 4.0g of TMOS, stir vigorously in a water bath at 40°C, add 2.0g of HCl (pH=1.0) dropwise, wait until the solution is mixed into a homogeneous phase, continue stirring for 10 minutes, and then vacuum for 5 minutes. Put the sol into a hydrothermal kettle, seal it with a plastic wrap, and let it stand in a constant temperature drying oven at 40°C for 24 hours to gel and age. Inject 10.0mL of 1M HCl, seal the hydrothermal kettle tightly, and after hydrothermal treatment at 80°C for 72 hours, the gel will be released naturally and has good mechanical strength. Brij56 in the gel can be completely removed by extraction with 30 mL of isopropanol for 16 h. Finally, the gel was quasi-sealed in a beaker with a microporous plastic wrap, and dried at a temperature of 40-110° C. to obtain an ordered mesoporous silicon oxide monolith with a size of Φ30.0×3.0 mm.

Embodiment 2

[0020] Dissolve 3.2g of Brij56 in 8.0g of TMOS, stir vigorously in a water bath at 40°C, add 4.0g of HCl (pH=2.0) dropwise, wait until the solution is mixed into a homogeneous phase, continue stirring for 10 minutes, and then vacuum for 10 minutes. Put the sol into a hydrothermal kettle, seal it with a plastic wrap, and let it stand in a constant temperature drying oven at 40°C for 24 hours to gel and age. Inject 10.0mL of 1M HCl, seal the hydrothermal kettle tightly, and after hydrothermal treatment at 80°C for 72 hours, the gel will be released naturally and has good mechanical strength. Brij56 in the gel can be completely removed by extraction with 60 mL of isopropanol for 24 hours. Finally, the gel was quasi-sealed in a beaker with a microporous plastic wrap, and dried at a temperature of 40-110° C. to obtain an ordered mesoporous silicon oxide monolith with a size of Φ30.0×6.0 mm.

[0021] Example 2:

[0022] Dissolve 2.8g of Brij56 in 4.0g of TMOS, stir vigorously in a...

Embodiment 4

[0024] Mix 2.0g Tween40 and 4.0g TMOS, stir vigorously in a water bath at 40°C, add 2.0g HCl (pH=2.0) dropwise, wait until the solution is mixed into a homogeneous phase, continue stirring for 10 minutes, and then vacuumize for 15 minutes. Put the sol into a hydrothermal kettle, seal it with a plastic wrap, and let it stand in a constant temperature drying oven at 40°C for 24 hours to gel and age. Inject 10.0mL of 1M HCl, seal the hydrothermal kettle tightly, and after hydrothermal treatment at 100°C for 48 hours, the gel will be released naturally and has good mechanical strength. Extract with isopropanol for 16 hours to completely remove Tween40 in the gel. Finally, the gel was quasi-sealed in a beaker with a microporous plastic wrap, and dried at a temperature of 40-110° C. to obtain an ordered mesoporous silicon oxide monolith with a size of Φ30.0×3.0 mm.

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PUM

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Abstract

The preparation process of ordered mesoporous monolithic silica includes the following steps: 1) selecting material including non-ionic surfactant, hydrochloric acid of pH value 0.5-2 and methyl metasilicate in the mass ratio of 0.5-2 to 1 to 1-4; 2) mixing the materials through stirring; 3) vacuum pumping for 5-20 min to obtain sol; 4) setting the sol in hydrothermal reactor to obtain gel, processing the gel with deionized water or solution of acid, alkali or salt at 60-120 deg.c for 12-72 hr, and extracting with ethanol or isopropanol to eliminate surfactant; and 5) heating at 40-110 deg.c for 10-48 hr to obtain optically transparent ordered mesoporous monolithic silica. The present invention has the features of short production period, simple process, high repeatability, etc. and the prepared mesoporous monolithic silica may be used as optical functional material, and other fields.

Description

technical field [0001] The invention belongs to the technical field of chemistry and inorganic materials, and in particular relates to a preparation method of an ordered mesoporous silicon oxide monolith. Background technique [0002] Functional mesoporous composites loaded with specific functional molecules or nano-ion clusters show attractive application prospects, and a lot of research has been carried out in energy storage, nonlinear optics, low dielectric constant, chemical sensing, etc., especially nonlinear Optical composite materials require optically uniform and transparent amorphous ordered mesoporous monolithic matrix materials. In addition, traditional zeolite molecular sieves have a pore size in the micropore range (<2nm), and large-sized molecules cannot enter. Under the background of the depletion of petroleum resources, it has always been a molecular sieve synthesis task to find a catalyst carrier suitable for the heavy oil catalytic industry. dreamer. O...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J21/08C01B33/18
Inventor 雷家珩刘丹郭丽萍赵俊巫辉
Owner WUHAN UNIV OF TECH
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