连续萃取催化精馏制备高纯度甲缩醛.pdf

化工进展
1620
CHEMICAL INDUSTRY AND ENGINEERING PROGRESS
2012年第31卷第7期
mexenone ser
应用技术
连续萃取催化精嵋制备高纯度甲缩醛
刘洪忠2,马昱博,沈鑫权2,高志贤13,吾满江艾力
1中国科学院新疆理化技术研究所,新疆乌鲁木齐8300112中国科学院研究生院,北京10009
3中国科学院山西煤炭化学研究所,山西太原030001)
摘要:研究了以甲醇和甲醛为原料,大孔径阳离子交换树脂为催化荆,通过将萃取精馏和催化精馏相耦合的方
法制备高纯度甲缩醛,证明了这种工艺的可行性。在内径为35mm、高为2700mm的玻璃反应精馏塔内进行实
验,考察了总进料量、萃取剂进料位置、醛摩尔比、回流比以及用甲醛溶液作为萃取剂对甲醛转化率和甲缩醛
纯度的影响。在选定的实验条件下,甲醛的转化率可达到97.82%以上,甲缩醛纯度可达到97.64%(含甲醛0.79%
水1.419%、甲醇0.20%)。
关键词:萃取精馏;催化精馏;甲缩醛;甲醇;甲醛
中图分类号:TQ5
文献标志码:A
文章编号:1000-6613(2012)07-1620-05
Continuous extractive catalytic distillation to synthesize high-purity
methylal
LIU Hong hong, MA Yubo, SHEN Xinquan GAO Zhixi Wma- i
Xinjiang Technical Inistitute of Physics and Chemistry, Chineseacademy of Sciences, Urumqi830011, injiang,
China:; Graduate School of Chinese Academy of Sciences, Beijing 100039, China; ' Shanxi Institute of Coal Chemistry
Chinese Academy of Sciences, Taiyuan 030001, Shanxi, China)
Abstract: An integrated continuous process combining catalytic distillation and extractive distillation
in one column was investigated for the synthesis of high-purity methylal from methanol and
formaldehyde in the presence of cation-exchange resin catalyst. The experiments were carried out in a
2700 mm glass reactive distillation column( diameter of 35 mm) the effects of operating parameters
such as total feed rate, extractant feeding location, reflux ratio, formalin used as extractant on the
continuous synthesis of methylal were studied. The results showed that formaldehyde conversion and
purity of methylal in the distillate could reach 97. 8% and 97.6%, respectively
Key words extractive distillation; catalytic distillation; methylal; methanol; formaldehyde
甲缩醛又称二甲氧基甲烷(DMM),是一种无其低温启动性能12。甲缩醛经氧化可获得浓度高达
色、无毒同时对环境友好的化工原料。因其良好的70%的甲醛溶液;而传统的甲醇氧化法得到甲醛的
理化性能,具有非常广泛的应用前景。由于甲缩醛浓度只能达到55%,高浓度的甲醛可以用于生产缩
具有良好的去油污能力和挥发性,可以作为清洁剂醛树酯1。
来替代F11、F13及含氯溶剂,是替代氟里昂、减
合成甲缩醛的传统方法是通过醇醛缩合反应,
少挥发性有机物( VOCS排放、降低対大气污染收稿日期,2012015;:修改稿日期:202023
的全新的环保型产品;甲缩醛本身是一种含氧燃料,
第一作者:刘洪忠(1985一),男,硕士研究生,从事甲醇下游产品技
作为柴油添加剂使用时,可以明显减少柴油机有害
术研究与开发。E-mailliuhongzhong0210163.com。联系人:高志贤,
研究员,博士生导师。E-mailgaozx@SXICC.ac.cn。吾满江艾力,研究员,
物的排放;甲醇汽油中加入一定量的甲缩醛可改善博士生导师, E-mail wumj(@ms xjb ac cn