使用高效液相色谱仪对腰果双酚醚化闭环后制备出产品进行定性定量分析。按n(酚羟基):n(ECH):n(四乙基溴化铵)=1:9:0.003的摩尔比称取腰果酚,环氧氯丙烷,四乙基溴化铵(催化剂用等质量的去离子水溶解)加入四口烧瓶中,置于油浴锅中100℃回流搅拌10min,加入5g的33 wt.%的NaOH溶液使PH呈碱性,恒温40min。降温至75℃,逐滴滴加33 wt.%的NaOH溶液,其中n(NaOH)/n(腰果酚)=1.3:1。保持回流分水,测试回收水量,当其达到理论量后,停止反应。调整温度至75℃后,真空脱除环氧氯丙烷与水共沸物1h。将脱除水和大部分环氧氯丙烷的粗产物先抽滤,随后在转速为8000r/min,时间为10min的条件下离心除盐。取滤液,在125℃条件下,进一步真空脱除环氧氯丙烷1-2h后,得到产品环氧化腰果酚。使用液相色谱仪在25℃温度下,以甲醇为流动相测精制后E-Cardol的液相色谱图。使用甲醇稀释样品至780倍,测其液相色谱图,确定环氧化腰果酚除氯程度。重复测试。
Qualitative and quantitative analysis of the product prepared by etherification of cashew bisphenol using high-performance liquid chromatography. Weigh cashew phenol, epichlorohydrin, and tetraethyl ammonium bromide in a molar ratio of n (phenolic hydroxyl): n (ECH): n (tetraethyl ammonium bromide)=1:9:0.003, and add them to a four necked flask. Place them in an oil bath at 100 ℃ and stir for 10 minutes under reflux. Add 5g of 33 wt.% NaOH solution to make the pH alkaline, and maintain the temperature for 40 minutes. Lower the temperature to 75 ℃ and add 33 wt.% NaOH solution dropwise, where n (NaOH)/n (cashew phenol)=1.3:1. Maintain reflux water separation, test the recovered water volume, and stop the reaction when it reaches the theoretical amount. After adjusting the temperature to 75 ℃, vacuum remove the azeotrope of epichlorohydrin and water for 1 hour. The crude product that removes water and most of the epichlorohydrin is first filtered by suction, and then centrifuged for desalination at a speed of 8000r/min and a time of 10 minutes. Take the filtrate and further vacuum remove epichlorohydrin at 125 ℃ for 1-2 hours to obtain the product epoxidized cashew phenol. Use a liquid chromatograph at 25 ℃ to measure the liquid chromatography of refined E-Cardol using methanol as the mobile phase. Dilute the sample to 780 times with methanol, measure its liquid chromatography, and determine the degree of chlorine removal by epoxidized cashew phenol.