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Method for preparing functionalization and hybridization of sulfonic acid material with special structure

A technology of hybrid materials and special structures, which is applied in the field of preparation of organic/inorganic hybrid materials to achieve high reactivity, environmental protection, and high hydrothermal stability

Inactive Publication Date: 2009-03-11
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, these two methods also have many defects of their own, which limit their application to a certain extent.

Method used

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  • Method for preparing functionalization and hybridization of sulfonic acid material with special structure
  • Method for preparing functionalization and hybridization of sulfonic acid material with special structure
  • Method for preparing functionalization and hybridization of sulfonic acid material with special structure

Examples

Experimental program
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Effect test

Embodiment 1

[0032] Under stirring at 40°C, dissolve 1.0g p123 in 1.69g absolute ethanol and 28g buffer solution of pH=4.4HAc-NaAc (pH=4.4, 0.52mol / L HAc, 0.27mol / L NaAc), after the solution is clarified , add 0.40g (EtO) 3SiCH 2 CH 2 CH 2 SSCH 2 CH 2 CH 2 Si(OEt) 3 and 2.33g (MeO) 4 Si, stirred at 40°C for 20h, and aged at 100°C for 24h. After the product was filtered, washed with water and dried, it was extracted with a mixed solution of absolute ethanol and HCl at 70°C for 24 hours. get -CH 2 CH 2 CH 2 SSCH 2 CH 2 CH 2 - Organic / inorganic hybrid materials. Sample after N 2 Adsorption / desorption, TEM characterization confirmed a mixed structure of two-dimensional hexagonal phase and cysts. The BET specific surface area of ​​the material is 724m 2 / g; the pore volume is 1.09cm 3 / g; the channel size is 7.3nm. Place 1 g of the above materials in a 100 mL beaker at room temperature, slowly add 10 g of concentrated nitric acid, and stir for 20 min. After the product is w...

Embodiment 2

[0034] Adopt the preparation process of embodiment 1, add 0.81g (EtO) 3 SiCH 2 CH 2 CH 2 SSCH 2 CH 2 CH 2 Si(OEt) 3 and 2.07g (MeO) 4 Si serves as a silicon source. The obtained material has a mixed structure of layered nanotubes and cysts, and the specific surface area of ​​the material is 570m 2 / g; the pore volume is 0.98cm 3 / g; the channel size is 8.3 and 25nm. According to the oxidation process of Example 1, the organic / inorganic hybrid material TSS20-SO functionalized with sulfonic acid was obtained 3 H. The BET specific surface area of ​​the material after oxidation is 670m 2 / g; the pore volume is 1.18cm 3 / g; the acid content is 0.86mmol H + / g.

Embodiment 3

[0036] Adopt the preparation process of embodiment 1, add 1.21g ((EtO) 3 SiCH 2 CH 2 CH 2 SSCH 2 CH 2 CH 2 Si(OEt) 3 and 1.81g (MeO) 4 Si serves as a silicon source. The obtained material has a pore structure dominated by cysts and foams, and the specific surface area of ​​the material is 432m 2 / g; the pore volume is 0.84cm 3 / g; the channel size is 8.8 and 17nm. According to the oxidation process of Example 1, the organic / inorganic hybrid material TSS30-SO functionalized with sulfonic acid was obtained 3 H. The BET specific surface area of ​​the material after oxidation is 594m 2 / g; the pore volume is 1.06cm 3 / g; the acid content is 0.89mmol H + / g.

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Abstract

The invention provides a method for preparing a sulfonic acid functionalized hybrid material with special structure. In a buffer solution system, a nonionic copolymer as a template agent and (EtO)3SiCH2CH2CH2SSCH2CH2CH2Si(OEt)3 as a mixed silicon source are stirred and crystallized, so as to obtain an organic / inorganic hybrid material with a multistage pore structure. The material synthesized through the method has a special pore path structure, and the acid content of the sulfonic acid functionalized hybrid material which is prepared by use of a simple nitric acid oxidation method and has the multistage pore structure can be adjusted in the range between 0.78 and 0.89 mmol H<+>g<-1>. The oxidized material shows great reaction performance in the esterification of ethanol and the fatty acids with different chain length. The multistage pore structure of the material is beneficial to the diffusion of reactants, and especially shows the unique advantages of the multistage pore structure for the reaction in which macromolecules participate.

Description

technical field [0001] The invention relates to an organic / inorganic hybrid mesoporous material, in particular to a method for preparing an organic / inorganic hybrid material with a hierarchical pore structure and post-oxidation to generate a sulfonic acid center. Background technique [0002] In the past ten years, mesoporous silica materials functionalized with organic groups have potential applications in the field of heterogeneous catalysis. Generally speaking, there are two methods for riveting organic groups on the surface of mesoporous silica: grafting method (post-synthesis method) and co-condensation method (direct synthesis method). However, these two methods also have many defects of their own, which limit their application to a certain extent. Silanes (R'O) bridged by organic groups reported in the late 1990s 3 SiCH 2 CH 2 Si(OR) 3 The synthesis of organic / inorganic hybrid mesoporous materials as precursors has attracted widespread attention in the materials ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08L101/12C08K9/00C08J3/20
Inventor 杨启华李聪明刘健
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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