尼龙酸薄荷酯的合成及其热裂解  

Synthesis and Pyrolysis of Nylon Acid Menthyl Ester

作　　者：陈芝飞 芦昶彤 陈瑨[2] 蔡莉莉 霍萃萌[2] 孙志涛 宋金勇 赵永德[2] 

机构地区：[1]河南中烟工业有限责任公司技术中心,河南郑州450000 [2]河南省科学院化学研究所,河南郑州450002

出　　处：《精细化工》2016年第10期1118-1124,共7页Fine Chemicals

摘　　要：以尼龙酸和L-薄荷醇为原料合成了清凉剂尼龙酸薄荷酯,采用单因素实验优化了合成工艺,并对产物的主要成分进行了分析和结构表征;利用热重-微商热重（TG-DTG）和在线裂解气相色谱/质谱联用（Py-GC/MS）法分别对尼龙酸薄荷酯的热失重和热裂解行为进行了考察。得到最佳合成条件为：当尼龙酸酐的投料量为0.1mol时,催化剂4-二甲氨基吡啶（DMAP）的用量为尼龙酸酐质量的0.4%、反应温度为70℃、反应时间为9.0 h、薄荷醇和尼龙酸酐的摩尔比为1.2∶1、环己烷用量50 mL,在该条件下产品收率达到89.3%。尼龙酸薄荷酯在301.5℃时失重速率最快为-19.17%/min,341.6℃时总失重率为99.72%;在300~450℃下尼龙酸薄荷酯的主要裂解产物为L-薄荷醇,随着裂解温度的提高,薄荷醇的释放量降低。Menthyl nylon acid was synthesized from nylon acid and L-menthol. The synthesis process was optimized through single-factor experiment. The main components of the product were analyzed and characterized. The thermal weight loss and pyrolysis properties of menthyl nylon acid were investigated by thermogravimetry-derivative thermogravimetry analysis（TG-DTG）,pyrolysis gas chromatography/mass spectrometry（Py-GC/MS）. The results showed that the optimal synthetic conditions were that dosage of 4-（dimethylamino） pyridine（DMAP） as a catalyst was 0. 4%（based on mass of nylon acid anhydride）,reaction temperature was 70 ℃,reaction time was 9. 0 h,mole ratio of L-menthol to nylon acid anhydride was 1. 2∶1 and cyclohexane was 50 m L,when nylon acid anhydride was 0. 1 mol. The yield of the product reached 89. 3% under the above conditions. Menthyl nylon acid had the fastest weight loss rate of-19. 17%/min at 301. 5 ℃,and its total weight loss reached 99. 72% at 341. 6℃. The main pyrolysis product of menthyl nylon acid was L-menthol in the range of 300 ℃ and 450℃. With the increase of pyrolysis temperature,L-menthol reduced.

关 键 词：尼龙酸薄荷酯 尼龙酸 L-薄荷醇 热裂解 食品与饲料用化学品 

分 类 号：TS42[农业科学—烟草工业]