Synthetic method for di-tert-butoxydiacetoxysilane
A technology of di-tert-butoxydiacetoxysilane and tetraacetoxysilane, which is applied in the field of synthesis of organosilicic acidic crosslinking agents, can solve problems such as difficulty in achieving large-scale production, and reduce production costs and reduce production costs , Reduce the effect of impurity interference
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example 1
[0016] Put 600 kilograms of glacial acetic acid and 340 kilograms of silicon tetrachloride into the reaction kettle at room temperature, and stir for ten minutes. The temperature was raised in the water bath, and the temperature was controlled for 3 hours to slowly increase the internal temperature of the reactor from 35°C to 60°C. Nitrogen gas was continuously fed in, and the reaction was kept at 60°C for 1 hour. It was detected that almost no HCL gas was emitted. Distill excess glacial acetic acid under reduced pressure until the pH value of the material is 5-6. At this moment, a large amount of crystallization of material was separated out, and 100 kilograms of glacial acetic acid was added to make it dissolve and clarify, weighing 618.3 kilograms. The content of tetraacetoxysilane in the sampling kilogram C analysis material is 78.86%, which is 487.6 kilograms of tetraacetoxysilane. Control the temperature at 17~20°C, add tert-butanol dropwise with measured molar mass, an...
example 2
[0018] The reaction device is the same as before. Add 300 kg of glacial acetic acid at room temperature, reclaim 300 kg of glacial acetic acid and 340 kg of silicon tetrachloride, and stir for ten minutes. The temperature was raised in the water bath, and the temperature was controlled for 3 hours to slowly increase the internal temperature of the reactor from 35°C to 60°C. Nitrogen gas was continuously fed in, and the reaction was kept at 60°C for 1 hour. It was detected that almost no HCL gas was emitted. Distill excess glacial acetic acid under reduced pressure until the pH value of the material is 5-6. Now material becomes turbid or a large amount of crystallization is separated out, add 150 kilograms of glacial acetic acid to make it dissolve clarification, weigh 667.4 kilograms. The tetraacetoxysilane content in the sampling kilogram C analysis material is 72.85%, which is 486.2 kilograms of tetraacetoxysilane. Control the temperature at 17~20°C, add dropwise tert-buta...
example 3
[0020] 400 kilograms of glacial acetic acid, 800 kilograms of reclaimed glacial acetic acid and 680 kilograms of silicon tetrachloride were dropped into the reactor, and stirred for ten minutes. The temperature was raised in the water bath, and the temperature was controlled for 4 hours to slowly increase the internal temperature of the reactor from 35°C to 60°C. Nitrogen gas was continuously introduced, and the reaction was kept at 60°C for 1.5 hours. It was detected that almost no HCL gas was emitted. Distill excess glacial acetic acid under reduced pressure until the pH value of the material is 5-6. This moment, a large amount of material crystallized out, added 300 kilograms of glacial acetic acid to make it dissolve and clarified, weighing 1352.8 kilograms. The content of tetraacetoxysilane in the sampling kilogram C analysis material is 72.75%, which is 984.2 kilograms of tetraacetoxysilane. Control the temperature at 17~20°C, add dropwise tert-butanol with measured mol...
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