中华医学超声杂志

应用化学 ›› 1994, Vol. 0 ›› Issue (1): 88-91.

• 研究论文 • 上一篇    下一篇

4,4'－二氯二苯砜部分水解制取4－氯－4'－羟基二苯砜

杨柏, 张天元, 沈家骢   

  1. 吉林大学化学系 长春 130023
  • 收稿日期:1993-03-20 修回日期:1993-08-16 出版日期:1994-02-10 发布日期:1994-02-10

Preparation of 4-Chloro-4'-hydroxyldiphenylsulfone from 4,4'- DichlorodiphenyI Sulfone by PartiaI Hydrolysis

Yang Bai, Zhang Tianyuan, Shen Jiacong   

  1. Department of Chemistry, Jilin University, Changchun 130023
  • Received:1993-03-20 Revised:1993-08-16 Published:1994-02-10 Online:1994-02-10

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摘要： 用高效液相色谱法(HPLC)对4,4'-二氯二苯砜(双氯),4,4'二羟基二苯砜(双酚)及4-氯-4'-羧基二苯砜(单酚)进行了完全的分离,研究双氯部分水解制单酚发现,NaOH用量越大、反应温度越高,水解速度越快,极值产率却越低;副产物双酚的含量随着反应时间增加,超过极值单酚产率后,由于副产物的增加,产率相对降低。最佳水解条件为水解温度135～140℃,NaOH/双氯(摩尔比)为3.25:1,水解时间2.5～3小时,产率90%以上。另外,还对水解过程中的缩聚现象及产物的纯化条件进行了讨论。

关键词: 二氯二苯砜, 氯羟基二苯砜, 水解, 制备

Abstract: In this paper,4,4'-dichlorodiphenylsulfone,4,4'-dihydroxyldiphenylsulfone and4-chloro-4'-hydroxyldiphenylsulfone were separated completely by HPLC. From the rela-tions between the reacting conditions and yields of 4-chloro-4'-hydroxyldiphenylsulfone byhydrolysis of 4,4'-dichlorodiphenylsulfone,it was found that the larger the amount of NaOHand the higher the temperature, the faster the hvdrolvsis and the lower the yield. Theamount of the by product 4,4'-dihydroxyldiphenylsulfone increases with reaction time. Af-ter the highest point the yield of 4-chloro-4' hydroxyldiphenylsulfone decreases as increase ofby-product. The optimum hydrolysis conditions are: 135～140℃, NaOH/4,4'-di-chlorodiphenylsulfone=3. 25 :1(molar ratio), reaction time 2,5～3. 0h. The yield wasabove 90%. The condensation polymerization occurred in the hydrolysis and the purificationof product also has been disctissed.

Key words: dichlorodiphenylsulfone, chlorohydroxyldiphenylsulfone, hvdrolysis, HPLC

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