HRID333045

反应详情

EQUATION

反应方程式

HRID 333045 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
50 °C

PROCEDURE

实验过程

100 g of Ludox TMA® [available from Helm AG; 34% nanosilica dispersion in water] is mixed with 100 ml of ethanol. To this mixture is added 11.7 g (25.6 mmol) of a photoinitiator [see reaction scheme] and 12.7 g (51 mmol) of 3-(trimethoxysilyl)propyl methacrylate at room temperature. The mixture is stirred at 50° C. for 20 hours. The amount of solvent is halved by evaporation in the rotary evaporator. By adding 150 ml of cyclohexane the product precipitates and is separated by centrifugation. After re-dispersing the product in butylacetate (BuOAc) a dispersion with 18.6 wt. % solid content is obtained. The ratio of photoinitiator to methacrylic groups is calculated based on analytical data to be 1 to 1.54. Thermographimetric analysis (TGA; heating rate: 10° C./min from 25° C. to 600° C.): Weight loss: 28.6%, corresponding to the organic material. Elemental analysis: found: C, 18.68%, H, 2.64%, O, 9.52%, S, 1.72: corresponding to an organic content of 32.6%. DLS: Average diameter d=54 nm.

WORKUP

后处理

  1. additionTo this mixture is added
  2. customThe amount of solvent is halved by evaporation in the rotary evaporator
  3. additionBy adding 150 ml of cyclohexane the product
  4. customprecipitates
  5. customis separated by centrifugation
  6. additionAfter re-dispersing the product in butylacetate (BuOAc) a dispersion with 18.6 wt. % solid content
  7. customis obtained
  8. temperatureThermographimetric analysis (TGA; heating rate: 10° C./min from 25° C. to 600° C.)