摘要
通过羟醛缩合、加氢催化两步反应,对三羟甲基丙烷(TMP)的合成进行了研究。重点研究了影响羟醛缩合反应、加氢还原的有关因素,如羟醛缩合反应中的催化剂用量、滴加温度、反应温度和时间、催化加氢中的催化剂性能、溶剂的选择等。采用1H-NMR与色质谱联用(GC-MS)剖析了中间体2,2-二羟甲基丁醛的结构性能,气相色谱分析了TMP纯度。确定了有关技术参数,找到了一条很有发展潜力的合成路线。
The
synthesis of trimethylolpropane with aldol condensation and catalytic hydrogenation via
two step was studied in the present paper.The reaction conditions,including the
quantities of triethylamine,the reaction temperature and time in aldol condensation stage
and the nature of catalysts , solvent etc.in catalytic hydrogenation stage were
investigated systematically when the reaction was carried out via two steps.The aldol
condensation product was analyzed with 1 H-NMR and GC-MS.It is proved that it is
unstable and can be converted to its dimer and trimer.The reaction parameters were
optimum.Thus,a novel route to synthesize TMP by aldol condensation and catalytic
hydrogenation was established.
出处
《河北化工》
1999年第2期1-4,共4页
Hebei Chemical Industry
关键词
三羟甲基丙烷
氢化
催化
合成
trimethylolpropane(TMP),2,2-dihyroxymethylbutanal,hydrogenation catalysis,synthesid,aldol
condensation,solvent effects