宝鸡文理学院学报(自然科学版) ,第 27 卷 ,第 3 期 ,第 198‐202 ,205 页 ,2007 年 9 月
Journal of Baoji University of Arts and Sciences (Natural Science) ,Vol .27 ,No .3 ,
pp
.198‐202 ,205 ,Sept .2007
Catalytic synthesis of 4‐methyl‐2‐
p
henyl‐1 ,3‐dioxolane with H
4
SiW
12
O
40
‐PAn
倡
YANG Shui‐
j
in ,TONG Wen‐long
(Department of Chemistry and Environmental Engineering , Hubei Normal U niversity ,Huangshi 435002 ,Hubei ,China)
Abstract :Aim To prepare a new environmental friendly catalyst ,H
4
SiW
12
O
40
‐PAn and it is used
to organic synthesis reactions .Method FT‐IR ,XRD and TG/DTA were used to identify the new
environmental friendly catalyst ,then it was used to the catalytic synthesis reaction of 4‐methyl‐2‐
p
he‐
nyl‐1 ,3‐dioxolane from benzaldehyde and 1 ,2‐
p
ropanediol . The factors influencing the synthesis
were discussed and the best conditions were found out .Results The optimum conditions are :molar
ratio of benzaldehyde to 1 ,2‐
p
ropanediol is 1 ∶ 2 .0 ,the quantity of catalyst is equal to 0 .5% of feed
stocks ,and the reaction time is 45 min and its yield can reach 87 .4 % .Conclusion H
4
SiW
12
O
40
‐PAn
is an excellent catalyst for synthesizing 4‐methyl‐2‐
p
henyl‐1 ,3‐dioxolane .
Key words :4‐methyl‐2‐
p
henyl‐1 ,3‐dioxolane ;12‐tungstosilicic acid ;
p
olyaniline ;catalyst
CLC number :TQ426 .91 ;TQ413 .26 Document code :A Artile ID :1007‐1261(2007)03‐0198‐05
H
4
SiW
12
O
40
‐PAn 催 化 剂 催 化 合 成
4‐甲 基‐2‐苯基‐1 ,3‐二 氧 戊 烷
杨水金 ,童文龙
(湖北师范学院 化学与环境工程系 ,湖北 黄石 435002)
摘 要 :目的 自制 H
4
SiW
12
O
40
(硅钨酸)‐PAn (聚苯胺)环境友好催化剂并进行有机物合成应用
研究 。 方法 通过 FT‐IR ,XRD 和 TG/DTA 手段对自制催化剂进行表征 ,以苯甲醛和 1 ,2‐丙二醇为
原料合成 4‐甲基‐2‐苯基‐1 ,3‐二氧戊烷 ,探讨 H
4
SiW
12
O
40
‐PAn 催化剂对缩醛反应的催化活性 ,较系统
地研究了原料量比 ,催化剂用量 ,反应时间诸因素对产品收率的影响 。 结果 在 n
(苯甲醛 )
/n
(1 ,2‐丙 二 醇 )
=
1/2 .0 ,催化剂用量为反应物料总质量的 0 .5% ,环己烷为带水剂 ,反应时间 45 min 的优化条件下 ,4‐甲
基‐2‐苯基‐1 ,3‐二氧戊烷的收率可达 87 .4 % 。 结论 实验结果表明 ,H
4
SiW
12
O
40
‐PAn 是合成苯甲醛
1 ,2‐丙二醇缩醛的良好催化剂 。
关键词 :4‐甲基‐2‐苯基‐1 ,3‐二氧戊烷 ;硅钨酸 ;聚苯胺 ;催化
中图分类号 :TQ426 .91 ;T Q413 .26 文献标志码 :A 文章编号 :1007‐1261(2007)03‐0198‐05
1 INTRODUCTION
Acetals and ketals are among the most important perfume materials and industrial materials of or‐
g
anic synthesis .Up to now ,there are many methods to synthesize them .Conventionally H
2
SO
4
is
used as catalyst in factories
[1]
,but it causes many problems ,such as the erosion of equipment ,diffi‐
culty for after‐treatment ,low quality of the products ,etc .With higher standard of living ,the re‐
q
uirements for the quality of perfume materials and environmental protection become higher and high‐
倡
Received data :2007‐04‐06
Foundation item :Supported by the Natural Science Foundation of Hubei Province (2005ABA053 ) and
the National Natural Science Foundation of China (20471044) .
Biography :YA NG Shui‐
j
in (1964‐) ,male ,born in Wuxue City ,Hubei Province ,China ,
p
rofessor ,doctor .He mainly w orks at
teaching inorganic chemistry and researching chemistry of tungsten and inorganic function materials .
E‐mail :
y
angshuijin@ 163 .com