A kind of preparation method of siliceous body precursor organosilane
A technology of organosilane and siliceous body, which is applied in the field of preparation of siliceous body precursor organosilane, can solve the problems of many experimental steps, high production cost, and long consumption time, and achieve simple process, low production cost, and high product yield. high rate effect
- Summary
- Abstract
- Description
- Claims
- Application Information
AI Technical Summary
Problems solved by technology
Method used
Image
Examples
preparation example Construction
[0019] The preparation method of siliceous body precursor organosilane comprises the following steps: first cetyl alcohol and cetylamine react to obtain dihexadecanylamine (compound 2), dihexadecanylamine reacts with succinic anhydride and further reacts with aminopropyl tris Reaction of ethoxysilanes yields siliceous precursor organosilanes (compound 1).
[0020]
[0021] Specifically, the method includes: catalyzing the reaction of cetyl alcohol and cetylamine at a certain temperature in a closed reactor by a bimetallic platinum-titanium or platinum-nickel catalyst to obtain dihexadecylamine (compound 2); Add dihexadecylamine and succinic anhydride into dry solvent I, heat to dissolve, stir at room temperature for a certain period of time, add catalyst and absolute ethanol, stir for 2 to 4 hours, then add molecular sieves and aminopropyltriethoxysilane, The mixture was further stirred and reacted at room temperature for a certain period of time, the solvent was removed by...
Embodiment 1
[0025] In a 1000 ml sealable reactor, add cetyl alcohol (24.24 g, 100 mmol), cetylamine (24.15 g, 100 mmol), catalyst platinum-titanium / γ-alumina (30 g, of which platinum mass The percentage content is 0.5%, the molar ratio of metal platinum and titanium is 1:15), dodecane (200 ml) and a magnetic stirrer, and after replacing the reaction system with nitrogen, the reaction tube is closed. The oil bath was heated to 180° C., stirred for 12 hours, cooled, and the reaction mixture was centrifuged to remove the catalyst, and the recovered catalyst could be recycled. Silica gel column chromatography (flushing agent: petroleum ether: ethyl acetate = 10:1), the product was confirmed by nuclear magnetic resonance and mass spectrometry to obtain dihexadecylamine (compound 2), with a yield of 91.0%.
[0026] Dihexadecylamine (6.0 g, 12.9 mmol) and succinic anhydride (1.94 g, 19.4 mmol) were added to dry tetrahydrofuran (200 ml), heated to dissolve, stirred at room temperature for 8 hours...
Embodiment 2
[0028] In 1000 milliliters of sealable reactors, add cetyl alcohol (24.24 grams, 100 millimoles), hexadecanol (25.36 grams, 105 millimoles), catalyst platinum-nickel / titanium oxide (25 grams, wherein platinum mass percent Content is 2%, the molar ratio of metal platinum and nickel is 1: 10), xylene (200 milliliters) and magnetic stirrer, after nitrogen replacement reaction system, seal reaction tube. The oil bath was heated to 140° C., stirred for 24 hours, cooled, and the reaction mixture was centrifuged to remove the catalyst, and the recovered catalyst could be recycled. Silica gel column chromatography (flushing agent: petroleum ether: ethyl acetate = 10:1), the product was confirmed by nuclear magnetic resonance and mass spectrometry to obtain dihexadecylamine (compound 2), with a yield of 85%.
[0029] Dihexadecylamine (6.0 g, 12.9 mmol) and succinic anhydride (1.94 g, 19.4 mmol) were added to dry dichloromethane (200 ml), dissolved by heating, and stirred at room temper...
PUM
Login to View More Abstract
Description
Claims
Application Information
Login to View More