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| C.I. 冰染重氮组分44 (C.I. 37000) 生产工艺 CAS号[95-51-2] |
C.I. 冰染重氮组分44 (C.I. 37000) 生产工艺 CAS号[95-51-2] 黄色基GC。
CAS名: Benzenamine, 2-chloro-, 参考文献: Beil. 12, 597, E1, 297, E2, 315, E3, 1281, E4, 1115.
发明者: Winther, Laska, Zitscher 1911年。Colour Index: Echtgelb GC Base, Echtgelbsalz GC.
用途: C.I. 酸性黄41, 122。 C.I. 酸性蓝87。C.I. 直接绿10。C.I. 分散橙54。C.I. 颜料黄60, 180。C.I. 颜料橙19, 31。
C.I. 颜料红21。C.I. 荧光增白剂31。
生产工艺文献:
BIOS 986, 64-66. (=胶卷PB 77764) 0-Chloroaniline (I.G. Griesheim) 英国人译自德文。抄录如下。
反应式: 本人有加注。
Prepared by the iron reduction of o-chloronitrobenzene
(No. 53). Iron reduction type 1.
Approx. 100 kg. o-chloronitrobenzene, 15 kg. formic
acid and 1500 kg. iron borings are
charged into 2000 l. boiling water to start the reduction. 4000 kg.
o-chloronitrobenzene is then added slowly at the boil. After 1/2 hr. (1000 kg.) of
the o-chloronitrobenzene has been added a further 1500 kg. iron borings is charged, together with 15 kg. formic acid. When the reaction
slackens a further 1000 kg. iron borings is added. Time for nitro addition 17-20
hrs.
After completion of the reduction the batch is allowed
to settle in the reducer and the crude amine layer is separated from the iron
sludge and allowed to settle for a further period in settling cylinders, very
nearly all the iron being removed in this way. o-Chloroaniline in the sludge
left in the reducer (and in the settling cylinders) is recovered by means of
steam distillation. Total occupation of reducer = 37-38 hr. The crude product is worked up by vacuum distillation,
the water present being distilled over first and then the o-chloroaniline.
(Test for completion of
reduction: after all
the nitro body has been added and the reaction has died down, a sample of the
reaction mixture is distilled in a flask: the distillate should be colourless
if the reduction is complete. If the distillate has a yellow tinge agitation
should be continued and, if necessary, a small amount of iron boring added).
Yield data and materials consumption/ tone of
o-chloroaniline:
o-Chloronitrobenzene 1.3 tone Yield = 95% theory.
Iron borings 1.28 tone. Formic acid 0.01 tone.
Service consymption /tone of product: Electricity 382 K.W.H. Steam 8.9 t.L.P. 2.1 t3 H.P.
Water 125 M3. Air 314 M3
Plant required for output of 40 tone o-chloroaniline /
month: (or 40 tone /month of different
chloroaniline) (See
also 0-anisidine No.16)
1. 1 reducer, 10 M3 C.I. brick-lined,
robust agitator of silicon iron (impeller type, 55 r.p.m.) and reflux cooler
with sight glass to assess the vigour of reaction, as judged by rate of reflux.
2. 2 settling cylinders 10 M3 equipped with agitation.
3. 1 still, 10 M3, with empty column
attached to vacuum receivers and pumps.
Analytical data: o-chloronitrobenzene C.Pt. 31.60C. o-chloroaniline C.Pt. -20C. to -30C.
Production: 1937 60,000 kg. 1943 74,000 kg.
o-Chloroaniline
hydrochloride. (I.G. Griesheim)
600
kg. o-chloroaniline and 2500 l. 7-8%
hydrochloric acid are heated to 700C. then add 470 kg. hydrochloric acid
240Be’ and cool
to 15-200C. The product is filtered on a vacuum filter and
then hydroextracted to further reduce the water content. Dry at 70-750C.
(1-1.5 tones/24 hrs) and grind.
The mother liquor can be reused for 6-7 batches before rejection.
Materials consumption/tone of o-chloroaniline
hydrochloride: o-Chloroaniline 0.775 t. Yield = 100% theory. (C.P. -2 to
-30C.)
Plant for 25 tons/month all hydrochloride of amines:
1. Solution and precipitation vessel 1 x 4 M3 brick-lined tank, Lead
coil Homogeneously lead-covered agitator.
2. Vacuum filter 3 M3 stoneware. 2a.
Vacuum receiver 1 M3 stoneware.
3. Centrifuge. Lead 90 kg. 750 r.p.m. rubber-lined. 4.
Dryer. 5. 2 x 3 M3 Ceramic storage vessels.
Analytical data: o-chloroaniline
C.Pt. -2 to -30C.
日文摘译文。细田豊。《理论制造染料化学》1957年。P. 480 译自PB 77764. 抄录如下。
2-クロルアニリン ( フアストエロ- Gヘ”-ス)
10 m3铸铁还原釜に0-ニトロヘ”ンセ“ン100 kg,義酸15 kg, 铁粉1.5 tを煮沸水2 m3に装入して还原を始め，o-ニトロクロ
ルヘ”ンセ”ン4 tを17-20 hて”加える。その间1/4 h後ニトロ1 tを加えた顷铁粉1.5 t と義酸15 kgを追加し，また反应か”にふ”
れは”铁粉1 tを加える。还原终れは”, 静置してアミン层を分けてさらに静置槽て”铁さ沉降させる。酸化铁残渣は水蒸汽蒸馏
によつてアミンを回收する。粗制品は真空蒸馏する。3160 kg,收率95%。 Cp. -2 - -30
中文摘译文。张澍声。《精细化工中间体工业生产技术》1996年。p. 71. 译自BIOS 986. 抄录如下。
在10000 L 砖衬还原釜中，加入100 kg邻氯硝基苯，15 kg甲酸，1500 kg铁屑和2000 L沸水，开始还原。然后在沸腾下缓
缓加入4000 kg邻氯硝基苯。
15分钟后，已经加入1000 kg邻氯硝基苯时，再加入1000 kg铁屑。硝化物加入时间为17-20小时。
还原反应完毕，反应物在还原器中静置，粗胺层于铁泥分离，再静置并分离。还原器中铁泥内的邻氯苯胺水蒸汽蒸馏回收。
还原器总占据时间37-38小时。粗产品经真空蒸馏，首先蒸出存在的水，然后蒸馏出邻氯苯胺。
还原反应完成的检验 – 当所有硝基物加完，并且反应趋于停滞，取反应混合物样品放入烧瓶中蒸馏。如果反应完成，馏出
物应是无色的；如果馏出物呈黄色，应继续搅拌，必要时加入少量铁屑。邻氯苯胺熔点 -3 - -20C, 收率95%。
每售出1吨邻氯苯胺消耗：邻氯硝基苯1300 kg, 铁屑1280 kg, 甲酸 10 kg。
邻氯苯胺盐酸盐：
600 kg邻氯苯胺和2500 L 7-8%盐酸加热至700C, 然后加470 kg 40% 盐酸，冷却到15-200C,抽滤，脱水器脱水以降低水含量，
70-750C干燥并研磨。母液在弃去前可重复使用6-7次。
PB 70422, 2002-2008. Fast Yellow Salt GC. By Keller. 1937年12月13日。德文。共7页。这是重氮盐。未抄录。
PB 70423, 2806-2812. Echtgelbsalz GC. 这是重氮盐生产工艺。 年份未抄录。未抄录。
国内研究动态:
荆学荣 气相色谱对邻氯苯胺及杂质的分离和含量测定 [J] 染料工业。1992.4.
23-5.
宋东明 李树德 等 （大工） 液相加氢制备邻氯苯胺 [J] 染料工业。1994,4, 19-21.
陈 丹 李树德 （大工） 兰尼镍催化加氢制备邻氯苯胺 [J] 染料工业， 1997, 5, 31-33.
胡拖平 陈宏博 （大工） 单氯代硝基苯加氢还原时脱氯规律的研究 [J] 染料工业， 2000, 6. 11-12.
孙 昱 吴秋洁 等（南大） Ni-B / SiO2 非晶态合金催化加氢制备邻氯苯胺[J]染料与染色，2005, 6, 32-34.
加注：
1. 抄录不同译文，说明译者不同，理解会不同，所以最好看原件。当然读者能看懂外文。
2. 国内期刊这里不再抄录，请看原期刊。
陈忠源 2017年1月5日 于 无锡 明辉国际。
文章作者：陈忠源 |
