triethoxy(methyl)silane

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: Into a 200 mL flask equipped with a stirrer, a thermometer, and a condenser tube, 4.07 g of a 35% by weight tetramethylammonium hydroxide aqueous solution and 28.94 g of acetone were charged to prepare a reaction solvent. A mixture solution of 6.02 g (70 mol % in all silanes) of methyl triethoxysilane, 4.18 g (30 mol % in all silanes) of methylsulfonyl methylphenyl trimethoxysilane, and 4.18 g of acetone was prepared. While the reaction solvent was stirred with a magnetic stirrer, the mixture solution was added dropwise into the reaction solvent at room temperature. After the completion of the addition, while maintaining the temperature of the resultant reaction mixture at 40° C. using an oil bath, the reaction was progressed for 240 minutes and then the reaction mixture was cooled down to room temperature, followed by adding 2 mol % hydrochloric acid to the reaction mixture to neutralize the reaction mixture. To the reaction liquid, 70 mL of ethyl acetate and 70 mL of water were added and the resultant reaction mixture was shaken, followed by subjecting the reaction mixture to phase separation into two phases. Further, the organic phase was washed with 70 mL of water three times. To the resultant organic phase, 12 g of propylene glycol monomethyl ether acetate was added and from the organic phase, methanol and ethanol as reaction by-products and water were distilled off under reduced pressure. The resultant reaction mixture was concentrated to obtain a hydrolysis-condensation product (polymer) propylene glycol monomethyl ether acetate solution. To the obtained solution, propylene glycol monoethyl ether was added to adjust the resultant solution to contain a solid residue in a proportion of 20% by weight at 160° C. The obtained polymer (corresponding to Formula (F-4)) had a weight-average molecular weight measured by GPC of Mw 6,200 in terms of polystyrene. Into a 200 mL flask equipped with a stirrer to prepare a reaction solvent the mixture solution was added dropwise into the reaction solvent at room temperature After the completion of the addition while maintaining the temperature of the resultant reaction mixture at 40° C. were added the resultant reaction mixture was shaken to phase separation into two phases Further, the organic phase was washed with 70 mL of water three times To the resultant organic phase, 12 g of propylene glycol monomethyl ether acetate was added and from the organic phase, methanol and ethanol as reaction by-products and water were distilled off under reduced pressure The resultant reaction mixture was concentrated

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

Procedure: A sample of 90% hydrolyzed ethyl silicate/methyltriethoxy silane co-condensate was prepared by adding water (11 grams) containing a trace of sulfuric acid to a solution of tetraethyl orthosilicate (37.5 grams) and methyl triethoxy silane (37.5 grams) in anhydrous ethanol (75 grams). Ethocel (4.5 grams) was added to thicken the solution. To a portion (11.5 grams) of the solution was added a 60% total solids TiO2 dispersion in isopropanol (40.3 grams) and a dispersing aid, Nuosperse 657 (3.5 grams). A 2 mil dry coating was prepared on a three by six inch steel Q panel and conditioned for 15 minutes at 200° C. The coated panel was then placed in a muffle furnace at 510° C. and its condition checked after 1, 2, 3, and 4 hours. At all times, the coating remained white, uncracked and adhered to the substrate. In comparison with the results contained in Control B and Examples 1-9, this demonstrates the usefulness of the highly filled co-condensate in this elevated temperature application. was then placed in a muffle furnace at 510° C. after 1, 2, 3, and 4 hours

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

Procedure: 54.56 g (70 mol %) of tetraethoxysilane, 9.81 g (14.7 mol %) of methyltriethoxysilane, 7.74 g (5 mol %) of 3-(triethoxysilylpropyl)diallylisocyanurate, 7.42 g (10 mol %) of phenyltrimethoxysilane, 0.31 g (0.3 mol %) of N-(3-triethoxysilylpropyl)-4,5-dihydroimidazole, and 105.03 g of acetone were charged into a 300-mL flask and while stirring the mixture solution with a magnetic stirrer, 24.95 g of a 0.10-mol/L hydrochloric acid was dropped into the mixture solution. After the dropping, the flask was placed into an oil bath controlled to 85° C. and under warming-reflux, the reaction was effected for 240 minutes. Then, the reaction solution was cooled down to room temperature and to the reaction solution, 142 g of propylene glycol monoethyl ether was added. From the resultant reaction mixture, ethanol and methanol, which were reaction by-products, water, and hydrochloric acid were distilled off under reduced pressure and the resultant reaction mixture was concentrated to obtain a hydrolysis-condensation product (polymer) propylene glycol monomethyl ether acetate solution. To the obtained solution, propylene glycol monoethyl ether and propylene glycol monomethyl ether acetate were added to adjust the resultant solution to have a solid residue concentration at 140° C. of 15% by weight while a solvent ratio of propylene glycol monomethyl ether acetate/propylene glycol monoethyl ether became 20/80. The weight average molecular weight of the obtained polymer of Formula (3-7) measured by GPC was Mw 1,500 in terms of polystyrene. After the dropping, the flask was placed into an oil bath controlled to 85° C. under warming-reflux was added were distilled off under reduced pressure the resultant reaction mixture was concentrated

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

Procedure: 4.92 g of phenyltrimethoxysilane, 72.42 g of tetraethoxysilane, 22.05 g of methyltriethoxysilane, 0.61 g of the 30% methanol solution of trimethoxysilylpropyltrimethylammonium trifluoromethanesulfonate, and 150 g of acetone were charged into a 500 mL flask to be dissolved and the resultant mixed solution was warmed while stirring the mixed solution with a magnetic stirrer to reflux. Next, 33.11 g of 0.01 M hydrochloric acid was added to the mixed solution. The mixed solution was subjected to the reaction for 240 minutes and then the resultant reaction solution was cooled down to room temperature. Then, 200 g of propylene glycol monoethyl ether was added to the reaction solution, and ethanol and methanol as reaction by-products, acetone, water, and hydrochloric acid were distilled off under reduced pressure to obtain a hydrolysis-condensation product. The polymer thus obtained corresponded to Formula (VII-30): to be dissolved the resultant mixed solution was warmed to reflux The mixed solution was subjected to the reaction for 240 minutes the resultant reaction solution were distilled off under reduced pressure to obtain a hydrolysis-condensation product The polymer thus obtained

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

Procedure: 4.93 g of phenyltrimethoxysilane, 72.47 g of tetraethoxysilane, 22.06 g of methyltriethoxysilane, 0.54 g of the 30% methanol solution of trimethoxysilylpropyldimethylammonium maleate, and 150 g of acetone were charged into a 500 mL flask to be dissolved and the resultant mixed solution was warmed while stirring the mixed solution with a magnetic stirrer to reflux. Next, 33.14 g of 0.01 M hydrochloric acid was added to the mixed solution. The mixed solution was subjected to the reaction for 240 minutes and then the resultant reaction solution was cooled down to room temperature. Then, 200 g of propylene glycol monoethyl ether was added to the reaction solution, and ethanol and methanol as reaction by-products, acetone, water, and hydrochloric acid were distilled off under reduced pressure to obtain a hydrolysis-condensation product. The polymer thus obtained corresponded to Formula (VII-26): to be dissolved the resultant mixed solution was warmed to reflux The mixed solution was subjected to the reaction for 240 minutes the resultant reaction solution were distilled off under reduced pressure to obtain a hydrolysis-condensation product The polymer thus obtained

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

Procedure: 4.92 g of phenyltrimethoxysilane, 72.39 g of tetraethoxysilane, 22.04 g of methyltriethoxysilane, 0.56 g of the 30% methanol solution of trimethoxysilylethylmethylpyridinium trifluoromethanesulfonate, and 150 g of acetone were charged into a 500 mL flask to be dissolved and the resultant mixed solution was warmed while stirring the mixed solution with a magnetic stirrer to reflux. Next, 33.13 g of 0.01 M hydrochloric acid was added to the mixed solution. The mixed solution was subjected to the reaction for 240 minutes and then the resultant reaction solution was cooled down to room temperature. Then, 200 g of propylene glycol monoethyl ether was added to the reaction solution, and ethanol and methanol as reaction by-products, acetone, water, and hydrochloric acid were distilled off under reduced pressure to obtain a hydrolysis-condensation product. The polymer thus obtained corresponded to Formula (VII-22): to be dissolved the resultant mixed solution was warmed to reflux The mixed solution was subjected to the reaction for 240 minutes the resultant reaction solution were distilled off under reduced pressure to obtain a hydrolysis-condensation product The polymer thus obtained

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

Procedure: 4.92 g of phenyltrimethoxysilane, 72.39 g of tetraethoxysilane, 22.04 g of methyltriethoxysilane, 0.56 g of the 30% methanol solution of trimethoxysilylethylmethylpyridinium trifluoromethanesulfonate, and 150 g of acetone were charged into a 500 mL flask to be dissolved and the resultant mixed solution was warmed while stirring the mixed solution with a magnetic stirrer to reflux. Next, 33.13 g of 0.01 M hydrochloric acid was added to the mixed solution. The mixed solution was subjected to the reaction for 240 minutes and then the resultant reaction solution was cooled down to room temperature. Then, 200 g of propylene glycol monoethyl ether was added to the reaction solution, and ethanol and methanol as reaction by-products, acetone, water, and hydrochloric acid were distilled off under reduced pressure to obtain a hydrolysis-condensation product. The polymer thus obtained corresponded to Formula (VII-22): to be dissolved the resultant mixed solution was warmed to reflux The mixed solution was subjected to the reaction for 240 minutes the resultant reaction solution were distilled off under reduced pressure to obtain a hydrolysis-condensation product The polymer thus obtained

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

Procedure: 4.93 g of phenyltrimethoxysilane, 72.46 g of tetraethoxysilane, 22.06 g of methyltriethoxysilane, 0.56 g of the 30% methanol solution of trimethoxysilylethylmethylpyridinium methanesulfonate, and 150 g of acetone were charged into a 500 mL flask to be dissolved and the resultant mixed solution was warmed while stirring the mixed solution with a magnetic stirrer to reflux. Next, 33.13 g of 0.01 M hydrochloric acid was added to the mixed solution. The mixed solution was subjected to the reaction for 240 minutes and then the resultant reaction solution was cooled down to room temperature. Then, 200 g of propylene glycol monoethyl ether was added to the reaction solution, and ethanol and methanol as reaction by-products, acetone, water, and hydrochloric acid were distilled off under reduced pressure to obtain a hydrolysis-condensation product. The polymer thus obtained corresponded to Formula (VII-21): to be dissolved the resultant mixed solution was warmed to reflux The mixed solution was subjected to the reaction for 240 minutes the resultant reaction solution were distilled off under reduced pressure to obtain a hydrolysis-condensation product The polymer thus obtained

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

Procedure: 4.93 g of phenyltrimethoxysilane, 72.46 g of tetraethoxysilane, 22.06 g of methyltriethoxysilane, 0.56 g of the 30% methanol solution of trimethoxysilylethylmethylpyridinium methanesulfonate, and 150 g of acetone were charged into a 500 mL flask to be dissolved and the resultant mixed solution was warmed while stirring the mixed solution with a magnetic stirrer to reflux. Next, 33.13 g of 0.01 M hydrochloric acid was added to the mixed solution. The mixed solution was subjected to the reaction for 240 minutes and then the resultant reaction solution was cooled down to room temperature. Then, 200 g of propylene glycol monoethyl ether was added to the reaction solution, and ethanol and methanol as reaction by-products, acetone, water, and hydrochloric acid were distilled off under reduced pressure to obtain a hydrolysis-condensation product. The polymer thus obtained corresponded to Formula (VII-21): to be dissolved the resultant mixed solution was warmed to reflux The mixed solution was subjected to the reaction for 240 minutes the resultant reaction solution were distilled off under reduced pressure to obtain a hydrolysis-condensation product The polymer thus obtained