三羟甲基丙烷-二庚酸-单丙烯酸酯的合成  

STUDY ON SYNTHESIS OF TMP-DIHEPTYLATE-ACRYLATE

作　　者：蔡国星[1,2] 张乐涛[1] 马莉[1] 古丽米热.吐尔地 吾满江.艾力 

机构地区：[1]中国科学院新疆理化技术研究所,新疆乌鲁木齐830011 [2]中国科学院大学,北京100049

出　　处：《精细石油化工》2014年第5期19-23,共5页Speciality Petrochemicals

基　　金：新疆维吾尔自治区重大专项计划(201130113-3)

摘　　要：以三羟甲基丙烷（TMP）、庚酸和丙烯酸（AA）为原料,对甲苯磺酸为催化剂,在无溶剂条件下采用两步直接酯化法合成三羟甲基丙烷-二庚酸-单丙烯酸酯,并优化了合成条件。结果表明：在反应温度为105℃、真空度为0.025MPa的条件下,反应6h,首先得到TMP-二庚酸酯;再按照TMP-二庚酸酯与丙烯酸摩尔比1∶1.25的比例,在温度为75℃,真空度为0.05MPa的条件下,反应8h,得到TMP-二庚酸-单丙烯酸酯。粗产物采用质量分数为2%~3%的碳酸钠和1%的活性白土吸附后,得到收率为93%~94%的产物,酸值（KOH）低于0.2mg/g、羟值（KOH）为0.85mg/g、碘值为60.6g/100g。Trimethylolpropane （TMP）, heptanoic acid and acrylic acid （AA） were used as raw materi- als to synthesize TMP-diheptylate-acrylate through two step direct esterification process under solvent-free conditions over toluene sulfonic acid catalyst, and the synthesis conditions were optimized. The results showed that TMP-diheptylate was obtained first at temperature of 105 ℃, vacuum pressure of 0. 025 MPa and reaction time of 6 h. TMP-diheptylate-acrylate was synthesized then at tem- perature of 75 ℃, vacuum pressure of 0.05 Mpa, reaction time of 8 h and molar ratio of TMP-diheptylate to acrylic acid of 1 ： 1.25. After crude product was treated by 2%- 3% （mass fraction） sodium carbonate and 1% （mass fraction） activated clay, the product with yield of 93 %-94% was obtained, of which acid value is less than 0.2 mg（KOH）/g, hydroxyl value is 0.85 mg/g and iodine value is 60.6 g/100 g.

关 键 词：三羟甲基丙烷-二庚酸-单丙烯酸酯 无溶剂 酯化反应 

分 类 号：TQ314.248[化学工程—高聚物工业]