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Mesoporous polymer-titanium silicon oxide nano composite material and preparation method thereof

A composite material and polymer technology, applied in the field of mesoporous materials, can solve the problems of uneconomical synthesis of bridged organosilicon sources, expensive surfactants, difficult molecular sieves, etc., and achieves low preparation costs, low equipment requirements, and raw material sources. wide range of effects

Inactive Publication Date: 2010-03-10
SHANGHAI NORMAL UNIVERSITY +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The functionalization of mesoporous silicone is divided into the synthesis of organosilicon source containing organic groups and ethyl orthosilicate as precursor or functionalized surfactant as structure directing agent. The disadvantage of this method is that the raw materials used are organic Silicon sources or functionalized surfactants are expensive and difficult to obtain; at the same time, organic functional groups have the disadvantages of random distribution and possible blockage of pores, which limits the further application of this type of material; another obvious disadvantage of this method is that it must first Synthetic Mesoporous Silica Materials
Using bridged bifunctional organosilicon sources as precursors to assemble and synthesize PMOs under the guidance of surfactants, although it is simple and effective to introduce organic groups such as methyl, ethyl, vinyl, phenyl, etc. into the framework, while maintaining open channels and active sites, but the bridging organosilicon source makes the synthesis very uneconomical, and the hydrophobic organic groups lead to phase separation and disordered materials in the case of high organic content, especially This phenomenon is more prominent when the silicon oxide framework contains heteroatoms such as titanium, iron, gallium, etc.
Because the heteroatoms in the framework endow mesoporous silica with unique catalytic active centers, this type of material has broad application prospects in catalysis, adsorption, etc., but the synthesis of hybrid mesoporous silica with multifunctional and high organic group content Molecular sieves are very difficult. Therefore, there are no relevant reports on polymer-titanium oxide silicon nanocomposites with mesoporous structures and their preparation methods.

Method used

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  • Mesoporous polymer-titanium silicon oxide nano composite material and preparation method thereof
  • Mesoporous polymer-titanium silicon oxide nano composite material and preparation method thereof
  • Mesoporous polymer-titanium silicon oxide nano composite material and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] a) Add 1.6g of surfactant F127 and 1ml of dilute hydrochloric acid with a concentration of 0.2mol / L into 10ml of absolute ethanol, and stir at 40°C until the surfactant is completely dissolved;

[0028] b) Add 2.08g tetraethyl orthosilicate (TEOS), and continue stirring at 40°C for 2 hours;

[0029] c) Add 0.0568g of isopropyl titanate and continue stirring at 40°C for 1 hour;

[0030] d) Add 1.0 g of water-soluble phenolic resin with a molecular weight of 300 to 500, and continue stirring at 40° C. for 0.5 hours;

[0031] e) Transfer the reaction solution to an evaporating dish, first volatilize at 30°C for 12 hours, then polymerize at 120°C for 20 hours;

[0032] f) Scrape off the reaction product in the evaporating dish, crush it, and bake it at 350°C for 5 hours under an inert atmosphere with a heating rate of 3°C / min to obtain: the polymer content is 50% [calculated by TG], silicon Mesoporous polymer-titanium oxide silicon nanocomposites with a titanium molar rat...

Embodiment 2

[0041] a) Add 1.6g of surfactant F127 and 1ml of dilute hydrochloric acid with a concentration of 2mol / L into 10ml of absolute ethanol, and stir at 40°C until the surfactant is completely dissolved;

[0042] b) Add 4.98g tetraethyl orthosilicate (TEOS), and continue stirring at 40°C for 2 hours;

[0043] c) Add 0.068g of isopropyl titanate, and continue stirring at 40°C for 1 hour;

[0044] d) Add 1.0 g of water-soluble phenolic resin with a molecular weight of 300 to 500, and continue stirring at 40° C. for 0.5 hours;

[0045] e) Transfer the reaction solution to an evaporating dish, first volatilize at 40°C for 4 hours, then polymerize at 80°C for 48 hours;

[0046] f) Scrape off the reaction product in the evaporating dish, crush it, and bake it at 400°C for 3 hours under an inert atmosphere, and the heating rate is 1°C / min to obtain: the polymer content is 50%, the silicon-titanium molar ratio (Si / Ti) is 100 mesoporous polymer-titanium oxide silicon nanocomposites.

[...

Embodiment 3

[0049] a) Add 1.6g of surfactant F127 and 1ml of dilute hydrochloric acid with a concentration of 1mol / L into 10ml of absolute ethanol, and stir at 30°C until the surfactant is completely dissolved;

[0050] b) Add 4.16g tetraethyl orthosilicate (TEOS), and continue stirring at 40°C for 2 hours;

[0051] c) Add 0.568g of isopropyl titanate and continue stirring at 40°C for 1 hour;

[0052] d) Add 1.0 g of water-soluble phenolic resin with a molecular weight of 300 to 500, and continue stirring at 40° C. for 0.5 hours;

[0053] e) Transfer the reaction solution to an evaporating dish, first volatilize at 20°C for 24 hours, then polymerize at 100°C for 24 hours;

[0054] f) Scrape off the reaction product in the evaporating dish, crush it, and bake it at 250°C for 8 hours under an inert atmosphere, with a heating rate of 5°C / min, to obtain: a polymer content of 50%, a silicon-titanium molar ratio (Si / Ti) is 10 mesoporous polymer-titanium oxide silicon nanocomposites.

[0055...

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Abstract

The invention discloses a mesoporous polymer-titanium silicon oxide nano composite material which has two-dimensional hexagonal structure, the space group of p6mm, the pore diameter of 5.0-9.0nm, thepore volume of 0.4-1.0cm<3> / g and the specific surface area of 300-800m<2> / g; polymer and titanium silicon oxide are evenly distributed on a mesoporous framework, and titanium atoms are mainly bondedon a silicon oxide framework in a form of quadridentate; and the polymer is phenolic resin, furan resin or urea resin. The composite material utilizes sol-gel technology to introduce a polymer source,a silicon source and a titanium source into a self-assembly reaction system of surface active agent under the condition of organic solvent, and is prepared by synergistic assembly function, polymerization cross-linking and solvent volatilization self-assembly technology. The preparation method of the nano composite material has the advantages of simple operation, wide sources of raw materials, low requirements for equipment, low preparation cost, being suitable for industrialized production and the like.

Description

technical field [0001] The invention relates to a polymer-titanium oxide silicon nanocomposite material with a mesoporous structure and a preparation method thereof, belonging to the technical field of mesoporous materials. Background technique [0002] Compared with traditional composite materials, the compounding of each component in nanocomposite materials is more uniform, and the performance it possesses is not a simple summation of the properties of each component, but a comprehensive performance synergistically produced on the basis of maintaining the characteristics of each component material . Mesoporous organic-inorganic nanocomposites also have these advantages, and the nano-confined space of the mesoscopic structure endows polymer-silicon oxide and carbon-silicon oxide nanocomposites with unique chemical behaviors. This provides a good opportunity for the synthesis and development of mesoporous materials with special applications such as catalysis, adsorption, op...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08L61/06C08L61/24C08L61/00C08K3/34C08J9/28
Inventor 万颖楚华琴赵东元
Owner SHANGHAI NORMAL UNIVERSITY
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