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Process for synthesizing mesoporous silicon oxide molecular sieve material by ultrasonic system

A technology of mesoporous silica and synthesis method, applied in chemical instruments and methods, molecular sieves and alkali exchange compounds, inorganic chemistry, etc., can solve the problems of poor emulsifying and dispersing ability of oily substances, poor dispersing ability of TEOS, difficult synthesis, etc. Achieve performance improvement, shorten synthesis time, and reduce synthesis difficulty

Inactive Publication Date: 2004-02-04
FUDAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, for F108, F98, F127, Brii35, Tetronic 1107, etc., which are all surfactants with large HLB values, their emulsifying and dispersing ability for oily substances is poor, that is, their dispersing ability for TEOS is poor, so in this system It is impossible or difficult to synthesize three-dimensional ordered mesoporous materials

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Embodiment 1, 0.5 gram of Pluronic F108 (EO 132 PO 50 EO 132 ) was dissolved in 30 grams of 2M hydrochloric acid aqueous solution, and after the surfactant was dissolved, 2.08 grams of TEOS was added to the solution. The solution is immediately placed in an ultrasonic tank (with a constant temperature water tank), ultrasonicated at 40°C for 2 to 4 hours, and undergoes a sol-gel chemical process and a cooperative self-assembly process to form a three-dimensional highly ordered organic-inorganic composite material. After the three-dimensional material is hydrothermally aged at 100°C for 12 hours, it is finally calcined at 550°C for 5 hours to remove the surfactant. Analysis tests such as PXRD, BET and TEM prove that the film material is a silicon oxide material with a high-quality three-dimensional cubic structure (space group is Im-3m). The specific surface area of ​​the material is 620m 2 / g, the pore volume is 0.9cm 3 / g, the pore size is 5.2 nm.

Embodiment 2

[0019] Embodiment 2, 0.8 gram of Pluronic P103 (EO 17 PO 56 EO 17 ) was dissolved in 30 grams of 2M hydrochloric acid aqueous solution, and after the surfactant was dissolved, 2.08 grams of TEOS was added to the solution. The solution is immediately placed in an ultrasonic tank (with a constant temperature water tank), and ultrasonicated at 40°C for 2 to 4 hours. After the chemical process of sol and gel and the process of cooperative self-assembly, a two-dimensional highly ordered organic-inorganic composite material is formed. The two-dimensional material was hydrothermally aged at 100° C. for 12 hours, and finally calcined at 550° C. for 5 hours to remove the surfactant. Analysis tests such as PXRD, BET and TEM prove that the film material is a high-quality two-dimensional hexagonal silicon oxide material. The specific surface area of ​​the material is 720m 2 / g, the pore volume is 1.1cm 3 / g, the pore size is 6.7 nm.

Embodiment 3

[0020] Example 3, 0.9 g of Pluronic P103 (EO17PO56EO17) was dissolved in 35 g of 2M hydrochloric acid aqueous solution, and after the surfactant was dissolved, 2.08 g of TEOS was added into the solution. The solution is immediately placed in an ultrasonic tank (with a constant temperature water tank), and ultrasonically operated at 45°C for 2 to 4 hours. After the sol, gel chemical process and cooperative self-assembly process, a two-dimensional highly ordered organic-inorganic composite material is formed. The two-dimensional material was hydrothermally aged at 100° C. for 12 hours, and finally calcined at 550° C. for 5 hours to remove the surfactant. Analysis tests such as PXRD, BET and TEM prove that the film material is a high-quality silicon oxide material with a two-dimensional hexagonal structure (space group p6mm). The specific surface area of ​​the material is 730m 2 / g, the pore volume is 1.0cm 3 / g, the pore size is 6.6 nm.

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Abstract

A process for synthesizing mesoporous silicon oxide as molecular sieve features that an ultrasonic system is used and the non-ionic surfactant is used as structure guide agent to effectively and quickly synthesize 2-D and 3-D mesoporous silicon oxide. Its advantages are high sequential pore channel structure, and greater specific surface area and porous volume.

Description

technical field [0001] The invention belongs to the technical field of inorganic nanometer materials, in particular to a method for synthesizing two-dimensional and three-dimensional mesoporous silicon oxide molecular sieve materials. technical background [0002] In M41S and SBA-n series mesoporous molecular sieves, MCM-41 and SBA-15 are the two main members, both of which have similar one-dimensional channels, high specific surface area and excellent thermal stability. Their unique structure endows them with broad application prospects and great significance in catalysis and separation. However, there are few studies on materials with three-dimensional channel structure, but their interconnected channel structure is more conducive to the mass transfer process in the channel, so the in-depth study of it has more practical significance. However, the synthesis conditions of almost all three-dimensional mesoporous materials are relatively harsh, which undoubtedly poses a grea...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B39/00
Inventor 田博之刘晓英屠波赵东元
Owner FUDAN UNIV
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