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.
出处
《精细石油化工》
CAS
CSCD
北大核心
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)