催化加氢法合成高品质季戊四醇的研究  

Study on the Synthesis of High Grade of Pentaerythritol with Catalytic Hydrogenation Method

作　　者：施以军 夏家信 陶长文 耿庆保 沈健伟 张慧 古静娴 王永贵[2] SHI Yijun;XIA Jiaxin;TAO Changwen;GENG Qingbao;SHEN Jianwei;ZHANG Hui;GU Jingxian;WANG Yonggui

机构地区：[1]安徽金禾实业股份有限公司研发中心,安徽滁州239200 [2]滁州学院材料与化学工程学院,安徽滁州239000

出　　处：《淮南师范学院学报》2021年第2期130-133,共4页Journal of Huainan Normal University

基　　金：安徽省科技重大专项项目“三氯蔗糖生产中含酸溶剂制高纯DMAC核心技术开发与产业化”(201903c08020007);安徽省高校自然科学研究项目“有机硅环氧改性水性丙烯酸树脂涂料的机理及性能研究”(KJ2017B05);安徽省大学生创新训练项目“水性UV固化上光油的研制与性能”(S201910377121)。

摘　　要：文章以甲醛、乙醛、三乙胺和高纯氢为原料,通过雷尼镍RTH-311型加氢催化剂合成季戊四醇,探讨了物料比、反应温度、反应时间及pH值对季戊四醇收率的影响。研究表明,最佳工艺条件是:羟醛缩合反应温度为30℃,甲醛:乙醛:三乙胺(摩尔比)为5.8:1:0.4,反应时间为1.5 h,反应过程中pH值为8.5,合成的季戊四醇的收率高达94.6%,经结晶、离心、干燥后的季戊四醇纯度可达到97.1%。在最佳工艺条件下,三乙胺、过剩的甲醛在反应后可回收循环使用。Pentaerythritol was obtained taken formaldehyde,acetaldehyde and triethylamine as raw materials,and then hydrogenation catalyst was carried out using Raney nickel RTH-311 type.The effects of material ratio,reaction temperature,reaction time and pH value on the yield of pentaerythritol were discussed.The results showed that the optimum technological conditions for the aldol condensation reaction were at 30℃for 1.5 h,with the molar ratio of formaldehyde,acetaldehyde and triethylamine of 5.8:1:0.4,and the pH value in the reaction start and process was 8.5.Under this condition,the yield of pentaerythritol was 94.6%,the purity of pentaerythritol after crystallization,centrifugation and drying could reach 97.1%.Test results showed that,under the optimal conditions,triethylamine,excessive formaldehyde can be recycled in the reaction after use.

关 键 词：季戊四醇 催化加氢 三羟甲基乙醛 羟醛缩合 合成工艺 

分 类 号：O622.3[理学—有机化学]