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采用多聚甲醛二甲基醚(PODE_n)代替甲醛与苯酚(Ph)在磷酸(PA)催化下反应合成双酚F。结果显示,随着n(n=1~5)的增加,双酚F的收率呈现为抛物线型,先增加后减小。当n为2时,双酚F的收率达到最大,为95.8%。而双酚F的选择性随n的增加而逐渐减小。与传统的以甲醛为原料合成双酚F相比,以PODEn为原料合成双酚F具有显著的高选择性优点。综合比较,PODE_n同系物中PODE_2最适合代替甲醛合成双酚F。该文还考察了苯酚投料比n(Ph)∶n(PODE_2)、磷酸投料比n(PA)∶n(PODE_2)、反应温度(θ)和反应时间(Time)对以PODE_2为原料合成双酚F的收率、选择性和产物分布的影响。在单因素实验基础上,采用响应面法优化,建立了双酚F收率的二次线性回归方程,获得了最佳的工艺条件。在反应温度90℃、n(Ph)∶n(PODE_2)=16.4∶1和n(PA)∶n(PODE_2)=5.49∶1操作条件下,双酚F的收率和选择性分别可达99.0%和95.8%。
Bisphenol F was synthesized by using PODE_n instead of formaldehyde and phenol (Ph) under the catalysis of phosphoric acid (PA). The results showed that with the increase of n (n = 1 ~ 5), the yield of bisphenol F showed a parabolic curve, increasing first and then decreasing. When n is 2, the yield of bisphenol F reaches the maximum of 95.8%. The selectivity of bisphenol F decreases with the increase of n. Compared with the traditional synthesis of bisphenol F from formaldehyde, the synthesis of bisphenol F from PODEn has the obvious advantages of high selectivity. Comprehensive comparison, PODE_n homologue PODE_2 most suitable for the synthesis of bisphenol F instead of formaldehyde. In this paper, we also investigated the synthesis of bisphenol from PODE_2 by using PODE_2 as the raw material, and the reaction conditions of reaction temperature (θ) and reaction time (Time) F yield, selectivity and product distribution. On the basis of single factor experiment, using the response surface method to optimize, a quadratic linear regression equation of bisphenol F yield was established, and the optimum technological conditions were obtained. Under the reaction conditions of n (Ph): n (PODE_2) = 16.4:1 and n (PA): n (PODE_2) = 5.49:1, the yield and selectivity of bisphenol F reached 99.0 % And 95.8%.