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| CAS号 [17243-13-9] 生产工艺。 3-羧基-4-羟基苯磺酰氯 |
CAS号 [17243-13-9] 生产工艺。 3-羧基-4-羟基苯磺酰氯
CAS名：Benzoic acid, 5-(chlorosulfonyl)-2-hydroxy-
用途：有机合成。医药。染料：媒介红26. LookChem网登录生产与经营单位30家。
BIOS 1153, 255-256.（=胶卷PB 85687）。 Salicylsulphonyl chloride
(5-Chlorosulphonylsalicylic acid). 英国人译自德文（无资料来源）。
反应式：本人有加注，暂未找到德文原件。
Outline: Salicylic acid is treated with
chlorosulphonic acid at 40-45℃., blown into ice water and filtered.
Plant: 1 Cast
iron kettle 2,000 l., with iron scraping stirrer (65-70 r.p.m.). Gas heatinf and water cooling coil. 1
Container for chlorosulphonic acid.
1 Wooden vat of 10,000 l. capacity. 1 Wooden nutsche of 3,000 l.
capacity. 1 Iron Montejust of 8,000
l. capacity.
Process:
The sulohonation
vessel is charged with 2,000 kg. of chlorosulphonic acid, and heated to 35℃. Over
a period, 285 kg. of salicylic acid are added.
The temperature rises to 45℃. If
there is any tendency to go higher, the batch must be cooled externally.
After the
final addition the pan is stirred for another half-hour and then cooled to 25℃. The
solution is blown to a vat containing 1000 l. of water and 2000 kg. of
ice. Further additions of ice are made
to the vat during the blowing (3000 kg. ice) so that the temperature does not
rise over 15℃. The precipitated sulphonyl chloride is
filtered off on a nutsche and washed with 1000 l. of water. Yield: 76-78% theory.
FIAT 1313,I, 77-78.
（=胶卷PB 85172）。 3-Carboxy-4-hydroxy-benzenesulfonyl chloride (I.G.
Leverkusen). “Salylsulfochlorid”
美国人译自德文（无资料来源）。 （抄注： 其译文与英国人的译文有点差别！）。
Apparatus: 1 –
cast iron kettle, 2000 l with 65-70 r.p.m. propeller agitator. Gas heated and cooled with outside sprinkling
ring.
1 – chlorsulfonic acid measuring
vessel. 1 – wood tub, 100000 l. 1 – wood nutsch, 3000 l. 1 – brick-lined cast iron blowcase, 8000 l.
Materials: 1 –
285 kg (143 NaNO2 equivalent) salicylic acid.
2 – 2000 kg chlorsulfonic acid.
3 – 5000 kg ice.
Procedure:
Charge
sulfonator with (2). Heat to 35℃ and add slowly dry ground (1). Temperature goes to 45℃. Do
not let temperature go above 45℃. Stir 1/2 hour (1) is in. Cool to 25℃ and blow onto 1000 l. water and 2000 kg
ice. Add 3000 kg more ice during blowing
to keep temperature under 15℃. Filter, wash with 1000 l.
cold water and centrifuge. Yield: 76-78%
of theoretical. Lab. Yield – 78% of
theory..
张澍声 《精细化工中间体工业生产技术》 1996年。 P. 159. 3-羧基-4-羟基苯磺酰氯。 译自FIAT 1313, I, 77.
在磺化釜中加入2000 kg 氯磺酸，加热到35℃，缓慢加入285 kg 干燥的研磨过的水杨酸（相当于143 kg NaNO2），温度上升到45℃，但不允许超过45℃。 水杨酸加完后搅拌0.5小时，冷却到25℃，加入1000 L水和2000 kg冰，再加入3000 kg冰，以保持温度在15℃以下。过滤，用1000 L冷水洗涤，离心脱水。收率76-78%。
学习与思考：
同样是德文资料“Salylsulfochlorid”，同样是“Leverkusen 厂”的生产工艺，为什么译文有差别？本人不再说了！因为本人暂未找到德文原件。再说到“资料整理和编目”，本人认为，这相当于部队的通讯兵和情报人员，7月7日上网的《苯甲酸》，完全可以说明我们的不足！当然，参与这一工作的人员，要想评二院院士是不可能的。也就是分工有不同。这就是本过来人上网的努力目标和理想！奋斗是幸福的！
陈忠源 2018年7月9日 （一位义务搬运科技文献资料的老者！）。
文章作者：陈忠源 |
