固体超强酸催化制备小分子羟基硅油工艺研究

Study on the Preparation of Low Molecular Weight Hydroxyl-silicone Oil Catalyzed by Solid Super Acid Catalyst

以六甲基环三硅氧烷(D3)为原料,在催化剂作用下通过开环、缩聚及水解反应制备小分子羟基硅油。研究了催化剂种类、催化剂用量、反应温度、脱低温度及催化剂重复使用性等工艺参数对产品收率及品质的影响。结果表明:相对于其它种类的催化剂而言,S2O82-/ZrO2-NiO催化制备的产物综合性能最佳;其最佳的工艺条件为:S2O28-/ZrO2-NiO质量用量为2%,反应温度为40℃,脱低温度为115℃,此时小分子羟基硅油的羟值为9.13%,产率可达87.2%。催化剂经重复使用3次及再生后仍具有较高的催化活性。

A low molecular weight hydroxyl -silicone oil was prepared using hexamethyleyclotrisiloxane （D3） as raw material through ring opening, condensation polymerization and hydrolysis reaction in the present of a catalyst. The effects of the kind of catalyst, the dosage of catalyst, the reaction temperature, the temperature of removal of low molecular and the resusability of catalyst on the yield and quality of product were discussed. Experimental results showed that the S2O8^2-/ZrO2-NiO had better catalyst performance than other pattern catalysts. The optimal technology was that the mass amount of S2O8^2-/ZrO2-NiO was 2%, the reaction temperature was 40℃, and the temperature of removal of low molecular was 115℃. The yield of low molecular hydroxyl- silicone could reach to 87.2% and its hydroxyl value was 9.13% under the optimal technology condition. When S2O8^2-/ZrO2-NiO was used for three times and regenerated, it also could have good catalytic activity again.