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第 39 卷第 2 期Vol. 39 No. 2
2009 年 4 月Apr 2009

所屬欄目:有機合成原料

連續酯化制備1,6-己二酸二甲酯
石鳴彥 (中國石油 遼陽(yáng)石化分公司研究院,遼寧 遼陽(yáng) 111003)
摘 要:以DNW-Ⅰ型強酸型陽(yáng)離子交換樹(shù)脂(DNW-Ⅰ型催化劑)為催化劑,己二酸和甲醇為原料,經(jīng)間歇酯化和連續酯化反應后通過(guò)精餾可制備選擇性為100%的1,6-己二酸二甲酯。結果表明,當DNW-Ⅰ型催化劑用量為5%(以己二酸計,m/m,下同)時(shí),己二酸間歇及連續酯化后轉化率分別大于68%和98%。優(yōu)化實(shí)驗條件為:間歇酯化:催化劑用量5%,n(甲醇)∶n(己二酸)=2.5∶1.0,反應溫度80~85℃,反應時(shí)間4 h;連續酯化:間歇酯化產(chǎn)物進(jìn)料為30~70 mL/h,甲醇進(jìn)料為95~210 mL/h,醇酸摩爾比>60。
關(guān)鍵詞:1,6-己二酸;甲醇;1,6-己二酸二甲酯;酯化反應
中圖分類(lèi)號:TQ225.24+2  文獻標識碼:A  文章編號:1009-9212(2009)02- 0047-03
Preparation of Dimethylene Adipate by Continuous Esterification
SHI Ming-yan (Research Institute of Liaoyang Petrochemical Company,Sinopetro,Liaoyang 111003,China)
Abstract:1,6-Dimethyl adipate was synthesized from adipic acid and methanol with 100% selectivity in a batch-continuous esterification process. DNW-I strong-acid cation exchange resin was used as catalyst. The results showed that the conversion of adipic acid in the batch step and the continuous step were more than 68% and 98%,respectively,at the catalyst level of 5%. The optimum conditions were as following:for the batch process,the mass fraction of catalyst 5%,methanol/adipic acid(mole ratio)2.5∶1.0,temperature 80~85℃,time 4 h;for the continuous step,the flow rate of the batch process product 30~70 mL/h,methanol 95~210 g/h,methanol/adipic acid(mole ratio)more than 60.
Key words:adipic acid;methanol;1,6-dimethyl adipate;esterification
作者簡(jiǎn)介:石鳴彥(1974-),女,山東萊州人,工程師,主要從事精細石油化工產(chǎn)品技術(shù)研發(fā)。(E-mail:shimy@petvcchina.com.cn)
收稿日期: 2008-11-1
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