松油醇生产中副产物化学组成分析及利用

Study on the chemical composition of by-product from terpineol production and its utilization

用气相色谱-质谱联用(GC-MS)分析了一步法松油醇生产中副产物的化学组成,共鉴定出22个化学成分,主要成分有苧烯、异松油烯、α-蒎烯和1,8-桉叶素等。研究了松油醇生产中副产物在SO42-/TiO2-ZrO2型固体超强酸催化剂作用下的反应规律,分析了催化剂的焙烧温度、反应温度、反应时间及催化剂用量等因素对其催化性能的影响。考察了催化剂放置时间对异构产物的影响和催化剂重复使用情况。结果表明,该催化剂对松油醇副产物的反应有较高的催化活性。通过GC-MS分析,其主产物为对伞花烃,副产物主要是异松油烯和α-松油烯。适宜的催化剂制备条件是:M(钛)∶M(锆)=3∶1,650℃焙烧温度。在此制备条件下松油醇生产中副产物反应的适宜工艺条件为:反应时间6 h、反应温度130℃、催化剂用量3%。所得产物中对伞花烃含量为60.60%。

The chemical composition of by-product from terpineol production was analyzed by GC - MS, and 22 components were identified. The main components are limonene,isoterpinolene,α - pinene and eucalyptol etc. Reaction of terpineol production by-product which was catalyzed with SO4z-/TiO2 - ZrO2 solid superaeid were studied. The effects of conditions for preparation of SO4^2 -/TiO2 - ZrO2 catalysts, such as ratio of Ti to Zr, calcination temperature, reaction temperature, reaction time, catalyst dosage, on its catalytic activity was investigated. Furthermore, the effect of storage time of the catalysts on the reaction was discussed, and the experiments of catalyst repeat use were carried out. The products of reaction were identified by GC - MS. In the reaction, the main product was p - cymene, and the by-products were terpinolene and α - terpinene, as well. The results showed that the optimum conditions for the preparation of SO4^2-/TiO2 - ZrO2 catalysts were the ratio of Ti to Zr 3 tool/tool, and calcinations temperature 650℃. At these conditions, the main factors affecting the reaction were investigated in the work. The optimum conditions for by-product reaction from terpineol production were as follows： reaction time 6 h, reaction temperature 130℃ , and catalyst dosage 3%. Under these conditions, the content of p -cymene was 60.60%.