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| CAS号 [1562-00-1] 生产工艺。 β-羟基乙烷磺酸钠盐 |
CAS号 [1562-00-1] 生产工艺。 β-羟基乙烷磺酸钠盐
CAS名：Ethanesulfonic acid, 2-hydroxy-, sodium salt. 历史参考文献：Beil. 4. E3, 42.
用途：印染助剂。CAS号[107-36-8]. LookChem网登录生产与经营单位76家。 CAS号 [1562-00-1]. LookChem网登录100家。
BIOS 986, 227-229.（=胶卷PB 77764）。 2-Hydroxyethane sodium
sulphonate (Oxyethanschwefelsäure salz natrium). (I. G. Hoechst).
英国人译自德文，无资料来源。德文原件，本人未抄录。今将英国人的译文抄录如下：
This was formerly made by the reaction of ethylene oxide with sodium
bisulphite in the Acetone / Acetic acid Department, but it is now made in the
intermediates Department from ethanol and sulphuric acid with subsequent
hydrolysis with caustic soda. The
impression was given by the staff of the first named department that the
present route is superior to the old one, but according to the Intermediates
Deparment the ethylene oxide route was abandoned only because of the impossible
of obtaining supplies of ethylene oxide during the war since it was being used
for ersatz dynamite. Ethylene oxide was
formerly made at a Buna works near Leverkusen and at Gendorf, and since it had
been not possible to restart delivery to Hoechst manufacture of oxyethansalz
had continued from ethanol.
Ethylene oxide was cheaper than ethanol in Germany, and this, together
with the simpler process and the considerable consumption of oleum of the
ethanol route, made the ethylene oxide route much the more attractive. However, where ethylene oxide is obtained
from ethanol, the ethanol route is worthy of assessment. The ethanol route is givev in detail below
and the ethylene oxide route is described in the report of the Auxiliary
Products Mission.
Process: Ethyl alcohol is sulphated to ethyl hydrogen sulphate and the
latter then sulphated to the sulphate ester which is hydrolysed to
hydroxyethane sulfonic acid. 反应式本人有加注，酸式CAS号 [107-36-8]。抄录如下：
Sulphation stages:
500 kg. alcohol (10.88 mols) and 950 kg. oleum 100% (SO3 11.88 mols)
are added alternately in ten lots to the sulphation pan (1) at a temperature
not exceeding 12℃. The
ethyl sulphuric acid is then sulphonated with SO3 in sulphonator (4) by running
in 830 kg. oleum 100% (SO3 10.375 mols) at 50-55℃. over 10-12 hours. After all
the SO3 has been introduced stir for a further 4-5 hours.
The sulphonated product is then blown at 60℃. into the hydrolysis vessel (6) containing 2300 l. water. 1500 l. 33%
NaOH (680 kg. NaOH 100% 17 mols) is now added at such a rate that the
temperature does not exceed 60℃. Heat
to gently boiling for 3-4 hours. Cool to
approximately 70℃. and add 1500 l. 33% NaOH (17 mols).
Now cool in item (8) to 30℃. in about 10
hours, when 2/3 of the total Na2SO4 crystallises out. The mass is then cooled to 20℃. and finally to 0℃. for precipitation of as much Na2SO4 as
possible, and filtered on a nutsch; wash with 400 l. cold water. The filtrate is stirred with carboraffin for
12 hours and filtered through a press.
Yield: 1350-1375 kg. 2-hydroxyethane sodium sulphonate dry = 84.5% theory
or ethylalcohol.
Plant:
(1) Sulphation vessel. C.I. 600 gallon capacity, internal surfaces
phenytalised (resin of phthalic anhydride and benzyl alcohol) with agitation,
condenser and cooling coil.
(2) Measure vessel. (3) (5)
(7).
(4) C.I. phenytalised sulphonator, 3 cu. m. with coil for warm water
heating and water cooling.
(6) Tile-lined hydrolysis vessel with lead coil and lead-covered
agitator. 7.5 cu. m.
(8) Iron cooling pan with iron coil and stirrer 7.5 cu. m.
张澍声 《精细化工中间体工艺生产技术》。1996年。《染料工业》编辑部 出版。 P. 274. β-羟基乙烷磺酸钠。译自BIOS 986,227.
β-羟基乙烷磺酸钠最初是由环氧乙烷与亚硫酸氢钠来制备，后来改变路线，由乙醇与硫酸反应，随后用氢氧化钠水解。一种说法是新的路线比旧的路线优越，另一种说法是放弃环氧乙烷路线仅仅因为得不到环氧乙烷供应，环氧乙烷用作黄色炸药代用品。
环氧乙烷在德国比乙醇便宜，加之工艺比较简单，而乙醇路线大量消耗发烟硫酸，因而环氧乙烷路线更有吸引力。这里介绍乙醇路线。反应式见英文译文。（抄注：这里不再抄录）。
在硫酸化锅中，在≤12℃温度下将500 kg 乙醇（10.88摩尔）和950 kg 100% 发烟硫酸（SO3 11.88 摩尔）分为10批交替加入。然后在50-55℃ 于10-12小时内于磺化锅内将乙基硫酸用830 kg 100% 发烟硫酸（SO3 10.375 摩尔）进行磺化。当所有发烟硫酸加入后再搅拌4-5小时。磺化产物在60℃压入装有2300 L水的水解锅中，加入1500 L33% 氢氧化钠溶液（含680 kg 100% 氢氧化钠，17摩尔），其速度要使温度不超过60℃，在缓和沸腾下加热3-4小时，冷却至70℃，并加入1500 L 33% 氢氧化钠溶液。
于约10小时内冷却到30℃，硫酸钠总量的2/3 结晶出来。将物料冷却到20℃，然后逐步冷却到0℃，尽可能多的测定出硫酸钠，抽滤，用400 L冷水洗涤。滤液用活性炭搅拌12小时，压滤。
得到1350-1375 kg 干的β-羟基乙烷磺酸钠，以乙醇计，收率84.5%。
PB 25623, 180-182. Oxyethansulfosäuren
Na. 这是氯乙醇路线的德文生产工艺，未抄录。
细田豊 《理论制造染料化学》。1957年。 P. 696. ヒドロキシエタンスルホン酸ナトリウムの制法。译自PB 25630.
水4.5 m3, エチレンクロルヒドリン（抄注：CAS号 [107-07-3]）37% 3 t ，Na2SO3. 7H2O 97% 3574 kgを徐徐に500に上げ3-4 h後徐徐に90-950に上げ5-6 h後急に温度を上げて蒸发し，1150に达し比重1.4（850）になれば50-600に冷し，NaClを滤過し，水1 m3で洗い洗液は次回の装入に用いる。滤液を蒸发亁固すればヒドロキシエタンスルホン酸ナトリウム2.3 t（NaCl 12-14% を含む）を得る。
PB 70253, 6257-6259. Production
of hydroxyethanesulfonic acid from ethyl alcohol. 1.5美元。
By Hengel. 1941年3月17日。 德文生产工业工程。未抄录。本文生产的游离酸，CAS号 [107-36-8]。
国内出版物：
侯乐山 主编 《中国精细化工产品集 – 原料及中间体10396种》。2006年。 p. 1005.
中国化工信息中心 全国精细化工原料及中间体行业协作组 出版 《版权所有 未经允许 不得翻印》。
前言：
提到2004年第一次出版《中国化工产品目录 – 精细化工原料及中间体分册》。 出版后不但受到国内用户的热力拥护，而且在国外市场如日本，韩国等国家也深受欢迎，…从而出版2006年版。
羟乙基磺酸；
英文名：2-Hydroxyethanwsulfonate;
Hydroxyethanesulfonic acid; Isethionic acid.
分子式：C2H6O4S.
分子量：126.10
CAS： 107-36-8. 物质登记状态：已登记。
生产厂：南京旋光科技有限公司。
羟乙基磺酸钠：2-羟基乙磺酸单钠。
英文名：Ethanesulfonic acid, 2-hydroxy-, monosodium
salt; 2-Hydroxyethanesulfonic acid,
sodium salt; Isethionic acid, sodium salt.
分子式：C2H6NaO4S.
分子量：148.11
CAS：1562-00-1. 物质登记状态：已登记。
生产厂：南京旋光科技有限公司；南通泰利达化工有限公司。
早期国家化美元进口的上述资料，没有参考价值？
陈忠源 2019年7月28日星期日。对本人来说，过一天，少一天。但是仍然希望读者能看到这一过时的历史资料！
文章作者：陈忠源 |
