tetraethyl silicate

Conditions: temp:0.00; pressure:0.00; stir:

Conditions: temp:0.00; pressure:0.00; stir:

Conditions: temp:0.00; pressure:0.00; stir:

Conditions: temp:0.00; pressure:0.00; stir:

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: The nanocomposites possessed a mesoscopically ordered silica framework that was interwoven with an organic resin component. In their syntheses, Pluronic® F127 poly(ethyleneoxide)-poly(propyleneoxide)-poly(ethyleneoxide) triblock copolymer species (EO106PO70EO106), with ethyleneoxide (EO, —OCH2CH2—) and propyleneoxide (PO, —OCH(CH3)CH2—) monomer units, were used as the structure-directing agent in an ethanol solution with water as a cosolvent. Tetraethoxysilane [TEOS, Si(OCH2CH3)4] were used as a network-forming inorganic precursor, and “resol” (an oligomeric compound formed by polymerization of phenol and formaldehyde) were used as a network-forming organic precursor. The procedure involved dissolving the F127 triblock copolymer in an acidic solution of ethanol and water, the subsequent addition of TEOS and resol into the same solution, mixing for 2 hours, and then casting into Petri dishes. The ethanol was allowed to evaporate for 5-8 hours at room temperature, after which the film was thermally polymerized at 100° C. for 24 hours to promote cross-linking of the resin species. After formation of the non-porous mesostructured composite films, the films were removed from their substrates, ground into a powder, and subsequently calcined at 350° C. for 3 hours under N2 to remove the triblock copolymer species, but not the resin component within the silica framework. The powder was then carbonized at 900° C. for 2 hours under N2 and the silica was subsequently removed via immersion in 10 wt % hydrofluoric acid for 24 hours to yield a mesoporous carbon powder product. Zhao and co-workers did not report the preparation of mesoporous silica-resin films, nor did they report mechanical property measurements of any kind. The mechanical implications of incorporating an organic resin component within the silica framework were not discussed, nor optimization or correlations or with other material properties. No data or results were presented to correlate mechanical properties of the materials with the organic resin composition of the frameworks, with compositions of the mesopore surface or inorganic-organic interfaces, or extent of resin polymerization.

Conditions: temp:35.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: 265.2 mL (1.95 mol, 525.353 g) bromopentafluorobenzene, 52.11 g (2.144 mol) magnesium powder and 216 mL (0.975 mol, 203.025 g) tetraethoxysilane are mixed together at room temperature and diethylether is added dropwise to the vigorously stirred solution until an exothermic reaction is observed (˜240 mL). The solution is stirred for 30 minutes after which additional 90 mL of Et2O is carefully added. After stirring at 35° C. for 16 h the mixture is cooled to room temperature and diethylether evaporated. An excess of n-heptane (˜600 mL) is added to precipitate the magnesium salts. Solution is filtrated and evaporated to dryness. The residue is fractionally distilled under reduced pressure to yield di(pentafluorophenyl)diethoxysilane. is carefully added is cooled to room temperature diethylether evaporated An excess of n-heptane (˜600 mL) is added to precipitate the magnesium salts Solution is filtrated evaporated to dryness The residue is fractionally distilled under reduced pressure

Conditions: temp:-80.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: 200 ml of freshly distilled dry Et2O is added to a 500 ml vessel (under an argon atmosphere). The vessel is cooled down to −80° C. and 15 g (0.129 mol) of CF2═CFCl gas is bubbled to Et2O. 100 ml (0.13 mol) of sec-BuLi is added dropwise during three hours. The temperature of the solution is kept below −60° C. all the time. The solution is stirred for 15 minutes and 29 ml (27.08 g, 0.130 mol) of Si(OEt)4 is added in small portions. The solution is stirred for over night allowing it to warm up to room temperature. Formed red solution is filtered and evaporated to dryness to result crude trifluorovinyltriethoxysilane, CF2═CFSi(OEt)3. 200 ml of freshly distilled dry Et2O is added to a 500 ml vessel (under an argon atmosphere) is kept below −60° C. The solution is stirred for over night to warm up to room temperature Formed red solution is filtered evaporated to dryness

Conditions: temp:65.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: 10 ml of tetraethoxysilane (TEOS), 1.2 g of vanadyl acetyl-acetonate (O═V(AcAc)2) and 8 ml of ethanol are successively dissolved into one another, and 2 ml of 8 n HCl are added under stirring. Once the gel formation has been completed, the material is heated to 65° C. at a heating rate of 0.5° C./min, is maintained at 65° C. for 3 h, is heated to 250° C. at a heating rate of 0.2° C./min, and is calcinated at this temperature for another 3 h. The adsorption/desorption isotherms show that the material has a true monomodal distribution of the micropores; BET: 542 m2/g; pore diameter: 0.66 nm. are added is maintained at 65° C. for 3 h is heated to 250° C. at a heating rate of 0.2° C./min

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: Si(O-n-C3H7)4; Si(O—isoC3H7)4; Si(OC2H4OCH3)4; CH3Si(OCH3)3; CH2═CHSi(OCH3)3; CH3Si(OC2H4OCH3)3; ClCH2Si(OC2H5)3; CH2═CHSi(OC2H4OCH3)3.

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: In a 1-liter flask 297 grams (4.798 moles) 2-propanol, 148 grams (2.558 moles) acetone, 123 grams (0.593 moles) TEOS, 104 grams (0.432 moles) phenyltriethoxysilane, 0.6 grams 1.0 M, 10 M and pure acetic acid (added to three separate solutions, respectively) and 72 grams deionized water were combined. In two other solutions containing 10 M acetic acid, 90 g and 110 g of deionized water were added, respectively. The flask was refluxed and/or heated for 1 to 12 hours. To the solution, 57 grams (0.769 moles) of Butanol, 88 grams (1.422 moles) 2-propanol, 44 grams (0.758 moles) of acetone, 59 grams (1.227 moles) of ethanol, 9.5 grams (0.528 moles) deionized water were added. separate solutions In two other solutions containing 10 M acetic acid, 90 g and 110 g of deionized water were added The flask was refluxed heated for 1 to 12 hours were added

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: In a 1-liter flask 297 grams (4.798 moles) 2-propanol, 148 grams (2.558 moles) acetone, 123 grams (0.593 moles) TEOS, 104 grams (0.432 moles) phenyltriethoxysilane, 0.6 grams 1.0 M, 10 M and pure lactic acid (added to three separate solutions, respectively) and 72 grams deionized water were combined. In two other solutions containing 10 M lactic acid, 90 g and 110 g of deionized water were added, respectively. The flask was refluxed and/or heated for 1 to 12 hours. To the solution, 57 grams (0.769 moles) of Butanol, 88 grams (1.422 moles) 2-propanol, 44 grams (0.758 moles) of acetone, 59 grams (1.227 moles) of ethanol, 9.5 grams (0.528 moles) deionized water were added. separate solutions In two other solutions containing 10 M lactic acid, 90 g and 110 g of deionized water were added The flask was refluxed heated for 1 to 12 hours were added

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: In a 1-liter flask 297 grams (4.798 moles) 2-propanol, 148 grams (2.558 moles) acetone, 123 grams (0.593 moles) TEOS, 104 grams (0.432 moles) phenyltriethoxysilane, 0.6 grams 0.1 M, 0.01 M and 1.0 M nitric acid (added to three separate solutions, respectively) and 72 grams deionized water were combined. In two other solutions containing 0.1 M nitric acid, 90 g and 110 g of deionized water were added, respectively. The flask was refluxed and/or heated for 1 to 12 hours. To the solution, 57 grams (0.769 moles) of Butanol, 88 grams (1.422 moles) 2-propanol, 44 grams (0.758 moles) of acetone, 59 grams (1.227 moles) of ethanol, 9.5 grams (0.528 moles) deionized water were added. separate solutions In two other solutions containing 0.1 M nitric acid, 90 g and 110 g of deionized water were added The flask was refluxed heated for 1 to 12 hours were added