Reaction equation
O=[Si]=O.C(O)C.[C:7]([O:12][CH2:13][CH2:14][CH2:15][Si](OC)(OC)OC)(=[O:11])[C:8]([CH3:10])=[CH2:9]>O>[C:7]([O:12][CH2:13][CH2:14][CH3:15])(=[O:11])[C:8]([CH3:10])=[CH2:9]Participants
Reactant 3
Product 1
Reagents, catalysts & solvents 1
Conditions
- Temperature
- 50 °C
Procedure
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
- additionTo this mixture is added
- customThe amount of solvent is halved by evaporation in the rotary evaporator
- additionBy adding 150 ml of cyclohexane the product
- customprecipitates
- customis separated by centrifugation
- additionAfter re-dispersing the product in butylacetate (BuOAc) a dispersion with 18.6 wt. % solid content
- customis obtained
- temperatureThermographimetric analysis (TGA; heating rate: 10° C./min from 25° C. to 600° C.)
Sources & evidence
- ORD record
- ord-e775d595658643f4a0cc8803b35ddd53
- Source dataset
- uspto-grants-2014_11
- Patent number
- US08877954B2
Linked notes
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