Citation:
Zhang Tianyong, Liu Qian, Li Bin, Zhang Guoling, Chen Song, An Jing, Wang Shuhua. Study on Water Removal Control in Synthesis and Purification of Bisphenol S[J]. Chemistry,
;2016, 79(3): 259-263,237.
-
The effects of different refluxing and water removal time on the synthesis of bisphenol S are studied when one water distributor or two water distributors are installed. The water removal efficiency can be significantly improved with two water distributors. The refluxing time can be reduced and the crude yield can also be increased. The preferred conditions are as follows: 492.5g phenol, 500g mesitylene and 25g 2,6-naphthalene disulfonic acid are mixed, then 256g concentrated sulfuric acid is dropped, after which refluxing is kept for 6.5h. The crude yield is more than 99% and the mass fraction of bisphenol S is 96.69%. In the purification of bisphenol S, a single alcohol-mesitylene and mixed alcohol-mesitylene system are compared. Taking the cost, yield, color and other aspects into accounts, the mixed alcohol including isopropanol and isoamyl alcohol is better than a single isopropanol. In the selection of the decolorants, the activated carbon for sugar is much better. The preferred conditions of a single alcohol-mesitylene system are as follows: 11.1g crude wet product is dissolved in 44.4g isopropanol, after 66.6g mesitylene and 1.11g activated carbon for sugar are added, the whole system is stirred and decolored under 60℃ for 1h. The yield is 97.0% and the mass fraction of bisphenol S is 99.89%. The preferred conditions of mixed alcohol-mesitylene system are as follows:10g crude product is dissolved in 40g mixed alcohol(isopropanol:isoamyl alcohol=1:1), after 60g mesitylene and 1g activated carbon are added, the whole system is stirred and decolored under 60℃ for 1h. The final yield is 90.6% and the mass fraction of bisphenol S is 99.87%.
-
Keywords:
- Bisphenol S,
- Purification,
- Alcohol,
- Mesitylene
-
-
-
[1]
[1] 章思规,章伟. 精细有机化工制备手册(上). 北京:化学工业出版社,2004.
-
[2]
[2] 张翠润. 上海化工,1990,15(5):45~47.
-
[3]
[3] 金范龙,衣守志,王广铨等. 吉林化工学院学报,1996,1(13):18~20.
-
[4]
[4] 沈俊杰. CN:104312157A, 2015.
-
[5]
[5] 何宗发. CN:104292760A. 2015.
-
[6]
[6] 高社章. CN:104293270A. 2015.
-
[7]
[7] 王寿高. CN:104212392A. 2014.
-
[8]
[8] V Claus, K Hartmut, Q Annett et al. React. Funct. Polym., 2011, 71(8):828~842.
-
[9]
[9] L Nadia, C Martino, F Maurizio et al. J.Appl. Polym. Sci., 2013, 128(1):416~423.
-
[10]
[10] L Nadia, C Martino, F Maurizio et al. Polymer, 2011, 52(4):904~911.
-
[11]
[11] 邵红飞.天津大学学位论文,2006.
-
[12]
[12] 邱明艳. 天津大学学位论文,2005.
-
[13]
[13] 金范龙,赵哲山. 化工时刊,1997,6(11):21~22.
-
[14]
[14] 张天永,朱佳佑,李彬等. 化工进展,2013,32(11):2719~2722.
-
[15]
[15] 陈锡如,章书兰,石成凤. 成都科技大学学报,1991,(4):21~28.
-
[16]
[16] 张天永,朱佳佑,李彬等. 现代化工,2014,34(2):113~116.
-
[17]
[17] A B Ernst, G Caspari. US:4996367A, 1991.
-
[18]
[18] A Josef. CS:257071B1, 1988.
-
[19]
[19] H Tomoya. WO:2002102720, 2002.
-
[20]
[20] T W Sauls, C Park. US:2833828, 1958.
-
[21]
[21] G C Vegter, M M De Brabander. US:3065274, 1962.
-
[1]
-
-
-
[1]
Aili Feng , Xin Lu , Peng Liu , Dongju Zhang . Computational Chemistry Study of Acid-Catalyzed Esterification Reactions between Carboxylic Acids and Alcohols. University Chemistry, 2025, 40(3): 92-99. doi: 10.12461/PKU.DXHX202405072
-
[2]
Yajin Li , Huimin Liu , Lan Ma , Jiaxiong Liu , Dehua He . Photothermal Synthesis of Glycerol Carbonate via Glycerol Carbonylation with CO2 over Au/Co3O4-ZnO Catalyst. Acta Physico-Chimica Sinica, 2024, 40(9): 2308005-0. doi: 10.3866/PKU.WHXB202308005
-
[3]
Yufang GAO , Nan HOU , Yaning LIANG , Ning LI , Yanting ZHANG , Zelong LI , Xiaofeng LI . Nano-thin layer MCM-22 zeolite: Synthesis and catalytic properties of trimethylbenzene isomerization reaction. Chinese Journal of Inorganic Chemistry, 2024, 40(6): 1079-1087. doi: 10.11862/CJIC.20240036
-
[4]
Yiling Wu , Peiyao Jin , Shenyue Tian , Ji Zhang . The Star of Sugar Substitutes: An Interview of Erythritol. University Chemistry, 2024, 39(9): 22-27. doi: 10.12461/PKU.DXHX202404034
-
[5]
Zhanggui DUAN , Yi PEI , Shanshan ZHENG , Zhaoyang WANG , Yongguang WANG , Junjie WANG , Yang HU , Chunxin LÜ , Wei ZHONG . Preparation of UiO-66-NH2 supported copper catalyst and its catalytic activity on alcohol oxidation. Chinese Journal of Inorganic Chemistry, 2024, 40(3): 496-506. doi: 10.11862/CJIC.20230317
-
[6]
Xinhao Yan , Guoliang Hu , Ruixi Chen , Hongyu Liu , Qizhi Yao , Jiao Li , Lingling Li . Polyethylene Glycol-Ammonium Sulfate-Nitroso R Salt System for the Separation of Cobalt (II). University Chemistry, 2024, 39(6): 287-294. doi: 10.3866/PKU.DXHX202310073
-
[7]
Yifeng TAN , Ping CAO , Kai MA , Jingtong LI , Yuheng WANG . Synthesis of pentaerythritol tetra(2-ethylthylhexoate) catalyzed by h-MoO3/SiO2. Chinese Journal of Inorganic Chemistry, 2024, 40(11): 2155-2162. doi: 10.11862/CJIC.20240147
-
[8]
Zhaoxuan ZHU , Lixin WANG , Xiaoning TANG , Long LI , Yan SHI , Jiaojing SHAO . Application of poly(vinyl alcohol) conductive hydrogel electrolytes in zinc ion batteries. Chinese Journal of Inorganic Chemistry, 2025, 41(5): 893-902. doi: 10.11862/CJIC.20240368
-
[9]
Yuanyuan Ping , Wangqing Kong . 光催化碳氢键官能团化合成1-苯基-1,2-乙二醇. University Chemistry, 2025, 40(6): 238-247. doi: 10.12461/PKU.DXHX202408092
-
[10]
Mengyang LI , Hao XU , Zhonghao NIU , Chunhua GONG , Weihui ZHONG , Jingli XIE . Highly effective catalytic synthesis of β-amino alcohols by using viologen-polyoxometalate hybrid materials. Chinese Journal of Inorganic Chemistry, 2025, 41(7): 1294-1300. doi: 10.11862/CJIC.20250080
-
[11]
Yinjie Xu , Suiqin Li , Lihao Liu , Jiahui He , Kai Li , Mengxin Wang , Shuying Zhao , Chun Li , Zhengbin Zhang , Xing Zhong , Jianguo Wang . Enhanced Electrocatalytic Oxidation of Sterols using the Synergistic Effect of NiFe-MOF and Aminoxyl Radicals. Acta Physico-Chimica Sinica, 2024, 40(3): 2305012-0. doi: 10.3866/PKU.WHXB202305012
-
[12]
Jin Yan , Chengxia Tong , Yajie Li , Yue Gu , Xuejian Qu , Shigang Wei , Wanchun Zhu , Yupeng Guo . Construction of a “Dual Support, Triple Integration” Chemical Safety Practical Education System. University Chemistry, 2024, 39(7): 69-75. doi: 10.12461/PKU.DXHX202405008
-
[13]
Linghua Chen . 基于双联动“三学”模式的食品专业分析化学教学改革. University Chemistry, 2025, 40(8): 78-91. doi: 10.12461/PKU.DXHX202409095
-
[14]
Ronghao Zhao , Yifan Liang , Mengyao Shi , Rongxiu Zhu , Dongju Zhang . Investigation into the Mechanism and Migratory Aptitude of Typical Pinacol Rearrangement Reactions: A Research-Oriented Computational Chemistry Experiment. University Chemistry, 2024, 39(4): 305-313. doi: 10.3866/PKU.DXHX202309101
-
[15]
Zhuoming Liang , Ming Chen , Zhiwen Zheng , Kai Chen . Multidimensional Studies on Ketone-Enol Tautomerism of 1,3-Diketones By 1H NMR. University Chemistry, 2024, 39(7): 361-367. doi: 10.3866/PKU.DXHX202311029
-
[16]
Asif Hassan Raza , Shumail Farhan , Zhixian Yu , Yan Wu . Double S-Scheme ZnS/ZnO/CdS Heterostructure Photocatalyst for Efficient Hydrogen Production. Acta Physico-Chimica Sinica, 2024, 40(11): 2406020-0. doi: 10.3866/PKU.WHXB202406020
-
[17]
Hailian Tang , Siyuan Chen , Qiaoyun Liu , Guoyi Bai , Botao Qiao , Liu Fei . Stabilized Rh/hydroxyapatite Catalyst for Furfuryl Alcohol Hydrogenation: Application of Oxidative Strong Metal-Support Interactions in Reducing Conditions. Acta Physico-Chimica Sinica, 2025, 41(4): 2408004-0. doi: 10.3866/PKU.WHXB202408004
-
[18]
Zhiwen HUANG , Qi LIU , Jianping LANG . W/Cu/S cluster-based supramolecular macrocycles and their third-order nonlinear optical responses. Chinese Journal of Inorganic Chemistry, 2025, 41(1): 79-87. doi: 10.11862/CJIC.20240184
-
[19]
Kaihui Huang , Dejun Chen , Xin Zhang , Rongchen Shen , Peng Zhang , Difa Xu , Xin Li . Constructing Covalent Triazine Frameworks/N-Doped Carbon-Coated Cu2O S-Scheme Heterojunctions for Boosting Photocatalytic Hydrogen Production. Acta Physico-Chimica Sinica, 2024, 40(12): 2407020-0. doi: 10.3866/PKU.WHXB202407020
-
[20]
Huafeng SHI . Construction of MnCoNi layered double hydroxide@Co-Ni-S amorphous hollow polyhedron composite with excellent electrocatalytic oxygen evolution performance. Chinese Journal of Inorganic Chemistry, 2025, 41(7): 1380-1386. doi: 10.11862/CJIC.20240378
-
[1]
Metrics
- PDF Downloads(0)
- Abstract views(603)
- HTML views(123)