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Preparation method and application of mesoporous silica material

A technology of mesoporous silica and bisdecyl dimethyl ammonium chloride, applied in chemical instruments and methods, alkali metal oxides/hydroxides, silicon compounds, etc. The process is complicated, the process is complex and other problems, to achieve the effect of obvious effect, simple process, and prolong the volatilization time

Pending Publication Date: 2020-07-17
TAIYUAN UNIVERSITY OF SCIENCE AND TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The choice of template agent in the preparation of mesoporous materials has a great influence on the structure of the material. At present, people mainly use different surfactants to regulate the structure of the material. Double-chain alkyl surfactants have different aggregation forms in the solution. , resulting in different mesoporous silica materials, among which Chinese patents ZL200510012316.3 and ZL200510012318.2 successfully prepared mesoporous silica and double The mesoporous silica material laid the foundation for the application of dialkyl cationic surfactants in mesoporous materials, but the dioctadecyl dimethyl ammonium chloride used in this patent is an insoluble cationic surfactant, and the preparation process It is necessary to use an ultrasonic disperser to disperse for 30 minutes under the condition of 50°C. The preparation process is complicated, and the reaction time and aging time are both greater than 8 hours.
Time-consuming and complicated process

Method used

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  • Preparation method and application of mesoporous silica material
  • Preparation method and application of mesoporous silica material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] According to tetraethyl orthosilicate: didecyl dimethyl ammonium chloride: water molar ratio is 1:0.25:240, weigh 12.9g of didecyl dimethyl ammonium chloride with a content of 70%, add to Stir and dissolve the mixed solution in 432g distilled water, with a concentration of 9molL -1 KOH solution to adjust the pH of the solution to 10, slowly add 20.833g TEOS dropwise under stirring, stir at room temperature for 8 hours, seal and age in an oven at 80°C for 6 hours, filter, wash with water and ethanol, and dry at 120°C for 4 hours to obtain a synthetic product. Raw powder, calcined the raw powder at 450°C for 1 hour to obtain a pore diameter of 4.5nm and a specific surface area of ​​1000cm 2 / g pore volume is 0.3cm 3 / g mesoporous silica material.

[0020] Weigh 5g of the above-mentioned mesoporous silica into a beaker, add 10g of rose essence, ultrasonicate at room temperature for 30min at 250w power to disperse the powder evenly, then vibrate for 2 hours on a constant ...

Embodiment 2

[0023] Carry out according to ethyl orthosilicate: double decyl dimethyl ammonium chloride: water molar ratio is 1: 0.125: 240, weigh 6.45g of double decyl dimethyl ammonium chloride with a content of 70%, add to Stir and dissolve the mixed solution in 432g distilled water, with a concentration of 9molL -1 KOH solution to adjust the pH value of the solution to 12, slowly add 20.833g TEOS dropwise under stirring, stir at room temperature for 6 hours, seal and age in an oven at 60°C for 4 hours, filter, wash with water and ethanol, and dry at 120°C for 1 hour to obtain Synthetic raw powder, the raw powder is calcined at 550°C for 1 hour to obtain a pore diameter of 5nm and a specific surface area of ​​850cm 2 / g pore volume is 0.8cm 3 / g mesoporous silica material.

[0024] Weigh 4g of the above-mentioned mesoporous silica into a beaker, add 8g of rose essence, ultrasonicate at room temperature for 20min at a power of 250w to disperse the powder evenly, then vibrate for 2 hour...

Embodiment 3

[0026] According to tetraethyl orthosilicate: didecyl dimethyl ammonium chloride: water molar ratio is 1:0.1:240, weigh 6.4g of didecyl dimethyl ammonium chloride with a content of 70%, add to Stir and dissolve the mixed solution in 432g distilled water, with a concentration of 9molL -1 KOH solution to adjust the pH value of the solution to 10, slowly add 20.833g TEOS dropwise under stirring, stir at room temperature for 7 hours, seal and age in an oven at 70°C for 5 hours, filter, wash with water and ethanol, and dry at 120°C for 2 hours to obtain Synthetic raw powder, the raw powder is calcined at 500°C for 1 hour to obtain a pore diameter of 8nm and a specific surface area of ​​400cm 2 / g Pore volume is 1.0cm 3 / g mesoporous silica material.

[0027] Weigh 1g of the above-mentioned mesoporous silica into a beaker, add 5g of rose essence, ultrasonicate at room temperature for 10min at 250w power to disperse the powder evenly, then vibrate for 2 hours on a constant temperat...

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Abstract

The invention discloses a preparation method and application of a mesoporous silica material. The pore diameter of the mesoporous silica material is 4.5 to 8 nm; the specific surface area of the mesoporous silica material is 200-1000 cm<2> / g; and the pore volume of the material is 0.2-2.0 cm<3> / g. The material with high specific surface area and large pore volume can be used as a slow-release agent for flavors and fragrances, and overcomes the defects that the flavors and fragrances are easy to decompose and deteriorate, rapid to volatilize and lose, short in fragrance lasting time, poor in thermal stability and the like in the application process. According to the preparation method, soluble didecyl dimethyl ammonium chloride is used as a template agent, ethyl orthosilicate is used as a silicon source, and a composite product is obtained under an alkaline condition; and the composite product is subjected to filtering, washing, drying and calcining so as to obtain the mesoporous silicawith a controllable structure. The method is short in reaction time and aging time, small in template agent usage, simple and convenient in process, capable of saving energy and reducing consumptionand convenient for large-scale production and application.

Description

technical field [0001] The invention relates to a preparation method and application of a mesoporous silica material, belonging to the field of preparation and application of mesoporous materials. Background technique [0002] Since researchers from moble company used cationic quaternary ammonium salt surfactants as templates to prepare M41S series mesoporous silica materials in 1992, people have devoted a lot of energy to research in this area, with different morphological structures and different properties. The requested research on mesoporous silica came into being. The choice of template agent in the preparation of mesoporous materials has a great influence on the structure of the material. At present, people mainly use different surfactants to regulate the structure of the material. Double-chain alkyl surfactants have different aggregation forms in the solution. , resulting in different mesoporous silica materials, among which Chinese patents ZL200510012316.3 and ZL20...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/28B01J20/10B01J20/30B01D15/08
CPCB01J20/28083B01J20/103B01J20/28071B01J20/28073B01J20/28076B01J20/28061B01J20/28064B01J20/28014B01D15/08
Inventor 陈润生
Owner TAIYUAN UNIVERSITY OF SCIENCE AND TECHNOLOGY
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