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CAS号 [107-35-7] 生产工艺 - 牛磺酸
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<p class="MsoNormal" align="center" style="font-size:medium;white-space:normal;text-align:center;"> <span lang="EN-US" style="font-size:16pt;">CAS</span><span style="font-size:16pt;font-family:宋体;">号</span><span lang="EN-US" style="font-size:16pt;"> [107-35-7] </span><span style="font-size:16pt;font-family:宋体;">生产工艺</span><span style="font-size:16pt;"> <span lang="EN-US">- </span></span><span style="font-size:16pt;font-family:宋体;">牛磺酸</span><span lang="EN-US" style="font-size:16pt;"><o:p></o:p></span> <br /> <p class="MsoNormal" style="font-size:medium;white-space:normal;"> <span lang="EN-US" style="font-size:12pt;"> </span> <br /> <p class="MsoNormal" align="left" style="font-size:medium;white-space:normal;"> <span style="font-size:12pt;font-family:宋体;">化学</span><span style="font-size:12pt;font-family:宋体;">名称:</span><span lang="EN-US" style="font-size:12pt;">Ethanesulfonic acid, 2-amino- Beil. 4, 528; E2, 554, 950, 1697; E4, 3289.<o:p></o:p></span> <br /> <p class="MsoNormal" style="font-size:medium;white-space:normal;"> <span style="font-size:12pt;font-family:宋体;">用途:医药,染料和食品等</span><span lang="EN-US" style="font-size:12pt;"><o:p></o:p></span> <br /> <p class="MsoNormal" style="font-size:medium;white-space:normal;"> <span lang="EN-US" style="font-size:12pt;">BIOS 986, 427.</span><span style="font-size:12pt;font-family:宋体;">(</span><span lang="EN-US" style="font-size:12pt;">=</span><span style="font-size:12pt;font-family:宋体;">胶卷</span><span lang="EN-US" style="font-size:12pt;">PB 77764</span><span style="font-size:12pt;font-family:宋体;">),</span><span lang="EN-US" style="font-size:12pt;">Taurine. (Hoechst)</span><span style="font-size:12pt;font-family:宋体;">,</span><span style="font-size:12pt;font-family:宋体;">英国人译自德文,无资料来源说明。德文原件暂未找到!</span><span lang="EN-US" style="font-size:12pt;"><o:p></o:p></span> <br /> <p class="MsoNormal" style="font-size:medium;white-space:normal;"> <span style="font-size:12pt;font-family:宋体;">反应过程:羟乙烷磺酸钠</span><span lang="EN-US" style="font-size:12pt;"> [4316-74-9]</span><span style="font-size:12pt;font-family:宋体;">与氨反应合成,得牛磺酸</span><span lang="EN-US" style="font-size:12pt;"> [107-35-7]</span><span style="font-size:12pt;font-family:宋体;">。</span><span style="font-size:12pt;"> </span><span style="font-size:12pt;font-family:宋体;">【结构式】略。</span><span lang="EN-US" style="font-size:12pt;"><o:p></o:p></span> <br /> <p class="MsoNormal" align="left" style="font-size:medium;white-space:normal;"> <span lang="EN-US" style="font-size:12pt;">Manufactured by a continuous process by the reaction of ammonia and oxyethanesulphonic acid sodium salt in the presence of caustic soda at 280 – 285</span><span style="font-size:12pt;font-family:宋体;">℃</span><span lang="EN-US" style="font-size:12pt;"> and 200 atmospheres pressure. Yield: 80% theory. The manufacturing process is essentially the same as that for methyltaurine [107-68-0], described in No. 144. </span><span style="font-size:12pt;font-family:宋体;">(已上传)。</span><span lang="EN-US" style="font-size:12pt;"><o:p></o:p></span> <br /> <p class="MsoNormal" style="font-size:medium;white-space:normal;"> <span lang="EN-US" style="font-size:12pt;"> </span> <br /> <p class="MsoNormal" style="font-size:medium;white-space:normal;"> <span style="font-size:12pt;font-family:宋体;">张澍声</span><span style="font-size:12pt;"> </span><span style="font-size:12pt;font-family:宋体;">编译《精细化工中间体工业生产技术</span><span style="font-size:12pt;"> <span lang="EN-US">– BIOS FIAT PB Report</span></span><span style="font-size:12pt;font-family:宋体;">》,《染料工业》编辑部出版,</span><span lang="EN-US" style="font-size:12pt;">1996</span><span style="font-size:12pt;font-family:宋体;">年,全书共</span><span lang="EN-US" style="font-size:12pt;">296</span><span style="font-size:12pt;font-family:宋体;">页,未见有</span><span lang="EN-US" style="font-size:12pt;">“</span><span style="font-size:12pt;font-family:宋体;">牛磺酸</span><span lang="EN-US" style="font-size:12pt;">”</span><span style="font-size:12pt;font-family:宋体;">的译文。</span><span lang="EN-US" style="font-size:12pt;"><o:p></o:p></span> <br /> <p class="MsoNormal" style="font-size:medium;white-space:normal;"> <span lang="EN-US" style="font-size:12pt;"> </span> <br /> <p class="MsoNormal" style="font-size:medium;white-space:normal;"> <span style="font-size:12pt;font-family:宋体;">候乐山</span><span style="font-size:12pt;"> </span><span style="font-size:12pt;font-family:宋体;">主编《中国精细化工产品集</span><span style="font-size:12pt;"> <span lang="EN-US">– </span></span><span style="font-size:12pt;font-family:宋体;">原料及中间体</span><span lang="EN-US" style="font-size:12pt;">10396</span><span style="font-size:12pt;font-family:宋体;">种》,中国化工信息中心</span><span style="font-size:12pt;"> </span><span style="font-size:12pt;font-family:宋体;">出版,</span><span lang="EN-US" style="font-size:12pt;">2006</span><span style="font-size:12pt;font-family:宋体;">年,</span><span lang="EN-US" style="font-size:12pt;">P. 953</span><span style="font-size:12pt;font-family:宋体;">,</span><span style="font-size:12pt;font-family:宋体;">牛磺酸,摘录如下:</span><span lang="EN-US" style="font-size:12pt;"><o:p></o:p></span> <br /> <p class="MsoNormal" style="font-size:medium;white-space:normal;"> <span style="font-size:12pt;font-family:宋体;">【生产方法】</span><span lang="EN-US" style="font-size:12pt;"><o:p></o:p></span> <br /> <p class="MsoNormal" style="font-size:medium;white-space:normal;"> <span lang="EN-US" style="font-size:12pt;">1. </span><span style="font-size:12pt;font-family:宋体;">将溴乙磺酸钠与浓氨水配成溶液蒸发至干并加热除去最后的水分。将残余物溶于热水,加入</span><span lang="EN-US" style="font-size:12pt;">95% </span><span style="font-size:12pt;font-family:宋体;">乙醇,结晶出牛磺酸,再用</span><span lang="EN-US" style="font-size:12pt;">80% </span><span style="font-size:12pt;font-family:宋体;">乙醇重结晶得成品,收率</span><span lang="EN-US" style="font-size:12pt;">50%</span><span style="font-size:12pt;font-family:宋体;">左右。</span><span lang="EN-US" style="font-size:12pt;"><o:p></o:p></span> <br /> <p class="MsoNormal" style="font-size:medium;white-space:normal;"> <span lang="EN-US" style="font-size:12pt;">2. </span><span style="font-size:12pt;font-family:宋体;">一乙醇胺法:一乙醇胺与盐酸反应生成氢氧化</span><span lang="EN-US" style="font-size:12pt;">-β-</span><span style="font-size:12pt;font-family:宋体;">氯乙胺,再经磺化,酸化,提纯而得。</span><span lang="EN-US" style="font-size:12pt;"><o:p></o:p></span> <br /> <p class="MsoNormal" style="font-size:medium;white-space:normal;"> <span lang="EN-US" style="font-size:12pt;">3. </span><span style="font-size:12pt;font-family:宋体;">丙烯酰胺法:由丙烯酰胺与亚硫酸氢钠磺化生成</span><span lang="EN-US" style="font-size:12pt;">β-</span><span style="font-size:12pt;font-family:宋体;">磺酸丙酰胺盐,然后用次氯酸钠进行氧化和重排而得。</span><span lang="EN-US" style="font-size:12pt;"><o:p></o:p></span> <br /> <p class="MsoNormal" style="font-size:medium;white-space:normal;"> <span style="font-size:12pt;font-family:宋体;">工业生产用乙醇胺于硫酸反应得到</span><span lang="EN-US" style="font-size:12pt;">2-</span><span style="font-size:12pt;font-family:宋体;">氨基乙基硫酸酯,再与亚硫酸钠反应生产牛磺酸(以上均无资料来源!)。</span><span lang="EN-US" style="font-size:12pt;"><o:p></o:p></span> <br /> <p class="MsoNormal" style="font-size:medium;white-space:normal;"> <span lang="EN-US" style="font-size:12pt;"> </span> <br /> <p class="MsoNormal" style="font-size:medium;white-space:normal;"> <span style="font-size:12pt;font-family:宋体;">(日)有机化合物辞典,有机合成化学协会</span><span style="font-size:12pt;"> </span><span style="font-size:12pt;font-family:宋体;">编,</span><span lang="EN-US" style="font-size:12pt;">1985</span><span style="font-size:12pt;font-family:宋体;">年,</span><span lang="EN-US" style="font-size:12pt;">P. 527</span><span style="font-size:12pt;font-family:宋体;">,</span><span style="font-size:12pt;"> </span><span style="font-size:12pt;font-family:宋体;">タウリン</span><span lang="EN-US" style="font-size:12pt;"> Taurine</span><span style="font-size:12pt;font-family:宋体;">,</span><span lang="EN-US" style="font-size:12pt;"> </span><span style="font-size:12pt;font-family:宋体;">摘录如下:</span><span lang="EN-US" style="font-size:12pt;"><o:p></o:p></span> <br /> <p class="MsoNormal" style="font-size:medium;white-space:normal;"> <span style="font-size:12pt;font-family:宋体;">【制法】アミノエタノ</span><span lang="EN-US" style="font-size:12pt;">-</span><span style="font-size:12pt;font-family:宋体;">ルモノ硫酸エステルオ</span><span lang="EN-US" style="font-size:12pt;">-</span><span style="font-size:12pt;font-family:宋体;">トクレ</span><span lang="EN-US" style="font-size:12pt;">-</span><span style="font-size:12pt;font-family:宋体;">ブ中で亚硫酸ナトリウムとともに加热する</span><span lang="EN-US" style="font-size:12pt;">[Brit. Pat. 406,380</span><span style="font-size:12pt;font-family:宋体;">(</span><span lang="EN-US" style="font-size:12pt;">1934</span><span style="font-size:12pt;font-family:宋体;">)</span><span lang="EN-US" style="font-size:12pt;">]</span><span style="font-size:12pt;font-family:宋体;">。</span><span lang="EN-US" style="font-size:12pt;"><o:p></o:p></span> <br /> <p class="MsoNormal" style="font-size:medium;white-space:normal;"> <span lang="EN-US" style="font-size:12pt;"> </span> <br /> <p class="MsoNormal" style="font-size:medium;white-space:normal;"> <span style="font-size:12pt;font-family:宋体;">章思规</span><span style="font-size:12pt;"> </span><span style="font-size:12pt;font-family:宋体;">主编《精细有机化学品技术手册》。科学出版社</span><span style="font-size:12pt;"> </span><span style="font-size:12pt;font-family:宋体;">出版,</span><span lang="EN-US" style="font-size:12pt;">1992</span><span style="font-size:12pt;font-family:宋体;">年,</span><span lang="EN-US" style="font-size:12pt;"> # 30542</span><span style="font-size:12pt;font-family:宋体;">,</span><span style="font-size:12pt;"> </span><span style="font-size:12pt;font-family:宋体;">牛磺酸。(此书本人未收藏)</span><span lang="EN-US" style="font-size:12pt;"><o:p></o:p></span> <br /> <p class="MsoNormal" style="font-size:medium;white-space:normal;"> <span lang="EN-US" style="font-size:12pt;"> </span> <br /> <p class="MsoNormal" style="font-size:medium;white-space:normal;"> <span style="font-size:12pt;font-family:宋体;">张大国</span><span style="font-size:12pt;"> </span><span style="font-size:12pt;font-family:宋体;">编著《精细有机单元反应合成技术手册》。化学工业出版社</span><span style="font-size:12pt;"> </span><span style="font-size:12pt;font-family:宋体;">出版,</span><span lang="EN-US" style="font-size:12pt;">2014</span><span style="font-size:12pt;font-family:宋体;">年,</span><span lang="EN-US" style="font-size:12pt;">P. 325</span><span style="font-size:12pt;font-family:宋体;">,</span><span lang="EN-US" style="font-size:12pt;">#075401</span><span style="font-size:12pt;font-family:宋体;">,</span><span lang="EN-US" style="font-size:12pt;">2-</span><span style="font-size:12pt;font-family:宋体;">氨基乙磺酸(牛磺酸)。</span><span lang="EN-US" style="font-size:12pt;"><o:p></o:p></span> <br /> <p class="MsoNormal" style="font-size:medium;white-space:normal;"> <span style="font-size:12pt;font-family:宋体;">【制法】</span><span lang="EN-US" style="font-size:12pt;">A</span><span style="font-size:12pt;font-family:宋体;">法:</span><span lang="EN-US" style="font-size:12pt;"><o:p></o:p></span> <br /> <p class="MsoNormal" style="font-size:medium;white-space:normal;"> <span style="font-size:12pt;font-family:宋体;">在</span><span lang="EN-US" style="font-size:12pt;">500 ml</span><span style="font-size:12pt;font-family:宋体;">四口瓶中加水</span><span lang="EN-US" style="font-size:12pt;">250 ml</span><span style="font-size:12pt;font-family:宋体;">和亚硫酸钠</span><span lang="EN-US" style="font-size:12pt;">75.6 g</span><span style="font-size:12pt;font-family:宋体;">,在氮气保护及搅拌回流下,缓慢加入</span><span lang="EN-US" style="font-size:12pt;">2-</span><span style="font-size:12pt;font-family:宋体;">氨乙基硫酸氢酯</span><span lang="EN-US" style="font-size:12pt;">28.2 g</span><span style="font-size:12pt;font-family:宋体;">,加完,回流</span><span lang="EN-US" style="font-size:12pt;">10 – 12 h</span><span style="font-size:12pt;font-family:宋体;">。减压蒸除水分。慢慢加入浓盐酸</span><span lang="EN-US" style="font-size:12pt;">100 ml</span><span style="font-size:12pt;font-family:宋体;">,搅拌</span><span lang="EN-US" style="font-size:12pt;">1 h</span><span style="font-size:12pt;font-family:宋体;">。过滤,滤除无机盐,并用浓盐酸</span><span lang="EN-US" style="font-size:12pt;">20 ml</span><span style="font-size:12pt;font-family:宋体;">洗两次。滤液,洗液合并并浓缩至原体积的一半,加入</span><span lang="EN-US" style="font-size:12pt;">95% </span><span style="font-size:12pt;font-family:宋体;">乙醇</span><span lang="EN-US" style="font-size:12pt;">50 ml</span><span style="font-size:12pt;font-family:宋体;">,冷冻</span><span lang="EN-US" style="font-size:12pt;">1 – 2 h</span><span style="font-size:12pt;font-family:宋体;">,过滤,得粗品。用浓盐酸重结晶一次,得</span><span lang="EN-US" style="font-size:12pt;">2-</span><span style="font-size:12pt;font-family:宋体;">氨基乙磺酸</span><span lang="EN-US" style="font-size:12pt;">21.3 g</span><span style="font-size:12pt;font-family:宋体;">,收率</span><span lang="EN-US" style="font-size:12pt;">85%</span><span style="font-size:12pt;font-family:宋体;">。</span><span style="font-size:12pt;"> </span><span style="font-size:12pt;font-family:宋体;">【参考文献】中国医药工业杂志</span><span lang="EN-US" style="font-size:12pt;">, 1995, 26(8): 339</span><span style="font-size:12pt;font-family:宋体;">。</span><span lang="EN-US" style="font-size:12pt;"><o:p></o:p></span> <br /> <p class="MsoNormal" style="font-size:medium;white-space:normal;"> <span lang="EN-US" style="font-size:12pt;">B</span><span style="font-size:12pt;font-family:宋体;">法:配料比:乙烯亚胺</span><span style="font-size:12pt;"> </span><span style="font-size:12pt;font-family:宋体;">:二氧化碳</span><span style="font-size:12pt;"> </span><span style="font-size:12pt;font-family:宋体;">:水</span><span lang="EN-US" style="font-size:12pt;"> =1 </span><span style="font-size:12pt;font-family:宋体;">:</span><span lang="EN-US" style="font-size:12pt;">1.64 </span><span style="font-size:12pt;font-family:宋体;">:</span><span lang="EN-US" style="font-size:12pt;">5</span><span style="font-size:12pt;font-family:宋体;">。将乙烯亚胺水溶液加入反应罐,搅拌,降温至</span><span lang="EN-US" style="font-size:12pt;">0</span><span style="font-size:12pt;font-family:宋体;">℃</span><span style="font-size:12pt;font-family:宋体;">,慢慢通入二氧化硫气体,温度不超过</span><span lang="EN-US" style="font-size:12pt;">10</span><span style="font-size:12pt;font-family:宋体;">℃</span><span style="font-size:12pt;font-family:宋体;">,當二氧化碳达到投料量后,测</span><span lang="EN-US" style="font-size:12pt;">pH= 1</span><span style="font-size:12pt;font-family:宋体;">,停止通二氧化硫,慢慢升温至</span><span lang="EN-US" style="font-size:12pt;">40</span><span style="font-size:12pt;font-family:宋体;">℃</span><span style="font-size:12pt;font-family:宋体;">,并保持此温度反应</span><span lang="EN-US" style="font-size:12pt;">2 h</span><span style="font-size:12pt;font-family:宋体;">。加入适量活性炭,升温</span><span lang="EN-US" style="font-size:12pt;">70</span><span style="font-size:12pt;font-family:宋体;">℃</span><span style="font-size:12pt;font-family:宋体;">脱色半小时,过滤,滤液浓缩,冷却结晶,甩滤,干燥得牛磺酸。收率</span><span lang="EN-US" style="font-size:12pt;">87%</span><span style="font-size:12pt;font-family:宋体;">。</span><span style="font-size:12pt;"> </span><span style="font-size:12pt;font-family:宋体;">【参考文献】特开昭</span><span lang="EN-US" style="font-size:12pt;">40-13007</span><span style="font-size:12pt;font-family:宋体;">,</span><span lang="EN-US" style="font-size:12pt;"> 47-16807</span><span style="font-size:12pt;font-family:宋体;">。</span><span lang="EN-US" style="font-size:12pt;"><o:p></o:p></span> <br /> <p class="MsoNormal" style="font-size:medium;white-space:normal;"> <span lang="EN-US" style="font-size:12pt;"> </span> <br /> <p class="MsoNormal" style="font-size:medium;white-space:normal;"> <span style="font-size:12pt;font-family:宋体;">何岩彬</span><span style="font-size:12pt;"> </span><span style="font-size:12pt;font-family:宋体;">主编《染料品种大全》,沈阳出版社</span><span style="font-size:12pt;"> </span><span style="font-size:12pt;font-family:宋体;">出版,</span><span lang="EN-US" style="font-size:12pt;">2018</span><span style="font-size:12pt;font-family:宋体;">年,</span><span lang="EN-US" style="font-size:12pt;">P. 1852</span><span style="font-size:12pt;font-family:宋体;">,</span><span style="font-size:12pt;font-family:宋体;">中文名称:</span><span lang="EN-US" style="font-size:12pt;">2-</span><span style="font-size:12pt;font-family:宋体;">氨基乙磺酸,别名:牛磺酸。</span><span lang="EN-US" style="font-size:12pt;"><o:p></o:p></span> <br /> <p class="MsoNormal" style="font-size:medium;white-space:normal;"> <span style="font-size:12pt;font-family:宋体;">【可合成的染料】</span><span lang="EN-US" style="font-size:12pt;">C.I. </span><span style="font-size:12pt;font-family:宋体;">酸性黄</span><span lang="EN-US" style="font-size:12pt;">230</span><span style="font-size:12pt;font-family:宋体;">;</span><span lang="EN-US" style="font-size:12pt;">C.I. </span><span style="font-size:12pt;font-family:宋体;">活性橙</span><span lang="EN-US" style="font-size:12pt;">99</span><span style="font-size:12pt;font-family:宋体;">;</span><span lang="EN-US" style="font-size:12pt;">C.I. </span><span style="font-size:12pt;font-family:宋体;">活性橙</span><span lang="EN-US" style="font-size:12pt;">99:1</span><span style="font-size:12pt;font-family:宋体;">;</span><span lang="EN-US" style="font-size:12pt;">C.I. </span><span style="font-size:12pt;font-family:宋体;">活性橙</span><span lang="EN-US" style="font-size:12pt;">133</span><span style="font-size:12pt;font-family:宋体;">;</span><span lang="EN-US" style="font-size:12pt;">C.I. </span><span style="font-size:12pt;font-family:宋体;">活性红</span><span lang="EN-US" style="font-size:12pt;">226</span><span style="font-size:12pt;font-family:宋体;">。</span><span lang="EN-US" style="font-size:12pt;"><o:p></o:p></span> <br /> <p class="MsoNormal" style="font-size:medium;white-space:normal;"> <span lang="EN-US" style="font-size:12pt;"> </span> <br /> <p class="MsoNormal" style="font-size:medium;white-space:normal;"> <span style="font-size:12pt;font-family:宋体;">陈忠源</span><span lang="EN-US" style="font-size:12pt;"> 2021</span><span style="font-size:12pt;font-family:宋体;">年</span><span lang="EN-US" style="font-size:12pt;">7</span><span style="font-size:12pt;font-family:宋体;">月</span><span lang="EN-US" style="font-size:12pt;">6</span><span style="font-size:12pt;font-family:宋体;">日,星期二</span> <br /><br /><br />本文地址:<a href="http://www.陈忠源化学文库.cn/Article.asp?ID=10001598" target="_blank">http://www.陈忠源化学文库.cn/Article.asp?ID=10001598</a>
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