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| CAS号 [59-67-6] 生产工艺 吡啶-3-甲酸（烟酸） |
CAS号 [59-67-6] 生产工艺 吡啶-3-甲酸（烟酸）
CAS名: 3-Pyridinecarboxylic acid. 参考文献: Beil. 22, 38; E1, 503; E2, 32; E3/4, 348.
用途: 医药。C.I.活性黄178。 C.I.活性红221。C.I.活性蓝 187, 216。
生产工艺文献:
BIOS Trip No. 1155. 197. Nicotinic Acid. 英国人译自德文。未说明资料来源。抄录如下。
反应式: 本人有加注。暂未找到相应的德文原件。
Quinolinic acid:
A large iron vessel, Provided with stirrer
and jacket for brine cooling and heating, is charged with a mixture of water
(3,000 ltr.), quinoline (13 kg.) and calcium carbonate (26 kg.). The mixture is
stirred and a temperature of 200C maintained during the addition of
potassium permanganate (106 kg.) over a period of 6 hours. When the addition of
permanganate is complete the reaction mixture is warmed to a temperature of 900C
and the manganese dioxide filtered through a press filter. This filtrate is evaporated
in vacuo to a volume of 200 ltr. And the quinolinic acid precipitated from this
concentrate by the addition of hydrochloric acid in a lead-line vessel. The
product is filtered on a rubber-lined centrifuge and dried. Yield: 52-53%.
Nicotinic acid:
The reaction vessel is a steel autoclave which is
provided with V4A or stoneware liner
and has direct gas heating. The vessel is charged with a mixture of qyinolinic
acid (15 kg.) and water (150 kg.) and the mixture heated to a temperature of
1400C (pressure 23 ats.), this temperature being maintained for 3
hours. The reaction liquid is released under pressure into a V2A steel vessel,
where the product crystallizes on cooling. The nicotinic acid is filtered on a vacuum
stoneware filter, washed with water and dried.
Yield: 100%.
上海医药产品生产工艺汇编。1966年。P. 269-270. 烟酸 Acidum Nicotinicum (Niacin)（一）淮海制药厂。 抄录如下。
1. 氧化，脱羧: 配料比 喹啉：硫酸：硝酸：盐酸 = 1: 4.90: 3.9: 0.057
将硫酸，喹啉依次加入搪瓷反应罐内，搅拌加热至150-1600 保温5小时，升温至1800，
缓缓滴加硝酸与盐酸的混酸，温度控制在180-2200，约需36-40小时加完，在200-2300搅拌保温2-3小时，得粗烟酸溶液。
2. 精制: 配料比 喹啉：硫酸铜 = 1: 0.74
将粗制烟酸溶液加1倍量的水稀释，滴加30-33%的液碱至pH 8-9,放冷，甩除硫酸钠与硝酸钠结晶，滤液在搅拌，加热情况下缓缓加入硫酸铜溶液，至烟酸成为铜盐完全沉淀析出，放冷，甩滤得烟酸铜盐，水洗，甩干，将铜盐于适量水相混，通蒸气加热，滴加液碱至pH
9以上，液体不再显绿色，放冷，过滤除去氧化铜。在滤液中，加硫化钠溶液至不再发生黑色沉淀，过滤。滤液浓缩，放冷，加盐酸至pH
3.5-3.9，放冷，甩滤得烟酸粗品。在粗品中加约12倍蒸馏水，活性炭，煮沸，抽滤，放冷，烟酸析出，过滤得成品烟酸。
总收率 39.63% （对喹啉计）。
（二）河北制药厂。 以混合甲基吡啶为原料，略！
加注:
发现一些手册，列有上述产品国内生产工艺，但未注明资料来源？
陈忠源 2017年3月1日 于 无锡 明辉国际。
文章作者：陈忠源 |
