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ChemicalBook CAS DataBase List Bis(triethoxysilylpropyl) disulfide

Bis(triethoxysilylpropyl) disulfide synthesis

11synthesis methods
-

Yield:56706-10-6 97.88%

Reaction Conditions:

with potassium sulfide;tetrabutylammomium bromide at 75 - 90; for 4 h;Temperature;

Steps:

1-6 Example 3:

The preparation method of bis-[3-(triethoxysilyl)-propyl]-disulfide includes the following steps: Step 1. Add a total of 80 g of an aqueous solution containing 36.34 g of potassium hydroxide to a 500 mL flask to obtain a potassium hydroxide solution;Step 2: Add 27.55g potassium carbonate and 23.92g sulfur powder to the potassium hydroxide solution, control the reaction temperature to 80°C, and under this temperature condition, the reaction time is 2h, and react to obtain a potassium disulfide solution;Step 3. Add 2g of tetrabutylammonium bromide to the potassium disulfide solution, stir for about 10 minutes, and then add 120g of 3-chloropropyltriethoxysilane dropwise while controlling the reaction temperature at 75°C. Add time is 2h.After the dropwise addition of 3-chloropropyltriethoxysilane is completed, the heat preservation reaction is carried out, and the heat preservation reaction temperature is 90° C., and the heat preservation reaction is carried out under this temperature condition for 4 hours.After the reaction is completed, liquid separation, suction filtration, and post-distillation treatment are performed, and finally 115.83 g of a colorless to pale yellow transparent liquid is obtained, that is, bis-[3-(triethoxysilyl)-propyl]-disulfide.The calculated yield of 3-chloropropyltriethoxysilane is 97.88%, the total sulfur content is 14.27%, the chlorine content is 0.25%, and the impurity content is 2.93%, which meets the industry standard requirements.

References:

CN112920216,2021,A Location in patent:Paragraph 0022-0059

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