摘要:2 ,2 ,4-三甲基-1 ,3-戊二醇(以下簡稱TMPD) ,是一種重要的精細化工中間體。常用于不飽和樹脂、醇酸樹脂、聚氨基甲酸乙酯、多酯增塑劑、印刷油墨、合成香料、表面活性劑如纖維柔軟劑,以及驅蟲劑等產品的合成中。由于國內對TMPD的合成工藝、產品深加工及應用開發不夠,很難尋到國產TMPD的商品。以工業異丁醛和氫氧化鈉為原料合成了2 ,2 ,4-三甲基-1 ,3-戊二醇。優化的工業生產條件為:異丁醛∶20%氫氧化鈉溶液∶50%氫氧化鈉溶液=10∶1∶4.3(mol) ,第一階段反應溫度28~52 ℃,時間1~2 h ,第二階段反應溫度90~140℃ , 反應時間8 h ,90℃反應3h,120℃反應3h,140℃反應2h。第二階段催化劑的加入方式為分批加入的方式。產率為50.22%。同時提出了提高產品質量的后處理方法。
關鍵詞:2 ,2 ,4-三甲基-1 ,3-戊二醇;異丁醛;合成;研究。
Abstract:2 ,2 ,4 - Trimethylpentane - l , 3 - diol. (Hereinafter referred to as TMPD) Is an important fine chemical intermediates. Commonly used in the unsaturated resin, alkyd resin, polyurethane, and more ester plasticizers, printing inks, synthetic fragrances, surfactants, such as fabric softeners, as well as the synthesis of insect repellant products. As the synthesis of domestic TMPD, product processing and application development is not enough, difficulty of finding someone made TMPD goods.The technology for the synthesis of 2 ,2 ,4 - trimethylpen2tane - 1 , 3 - diol using industrial isobutyraldehyde and sodiumhydroxide is presented. The optimum reaction condition is thatthe mole ratio of reactants isobutyraldehyde : sodium hydroxide :sodium hydroxide = 10 : 1 : 4.3 ,reaction temperature 28~52 ℃for 1~2h in frist step , and 90~140 ℃for 8h in second step,90 ℃ reaction for 3h,120 ℃ reaction for 3h,140℃ reaction for 2h.Yield was 50.22%The methods of purifying products aredeveloped too.
Key words : 2 ,2 ,4 - trimethylpentane - 1 , 3 - diol ; isobu2tyraldehyde ; synthesis