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发 送 文 章     C.I.还原黄31 (C.I. 68405) 生产工艺 [留言][评论][收藏] 收信地址     填写收信人的电子邮箱 邮件主题     填写邮件主题 邮件内容  <p class="MsoNormal"> <span><strong><u>C.I.</u></strong></span><strong><u><span style="font-family:宋体;">还原黄</span><span>31 (C.I. 68405) </span></u></strong><strong><u><span style="font-family:宋体;">生产工艺</span> </u><span><span> </span>CAS</span></strong><strong><span style="font-family:宋体;">号</span><span>:[6871-93-8]</span></strong> <p class="MsoNormal"> <strong><u><span style="font-size:9pt;">CAS</span></u></strong><strong><u><span style="font-size:9pt;font-family:宋体;">名：</span></u></strong><strong><span style="font-size:9pt;"> Benzamide, </span></strong><span style="font-size:9pt;">2,5-dichloro-N-(7-oxo-7H-benzo[e]perimidin-8-yl)-</span> <br /> <p class="MsoNormal"> <strong><u><span style="font-size:9pt;font-family:宋体;">发明者：</span></u></strong><span style="font-size:9pt;"><span>  </span>M. A. Kunz and K. Koeberle<span>  </span>1931</span><span style="font-size:9pt;font-family:宋体;">年。</span><span style="font-size:9pt;"></span> <br /> <p class="MsoNormal"> <strong><u><span style="font-size:9pt;font-family:宋体;">生产工艺文献：</span></u></strong><strong><span style="font-size:9pt;"><span>   </span>BIOS 987, </span></strong><span style="font-size:9pt;">95, 173.<span>   </span></span><span style="font-size:9pt;font-family:宋体;">二手资料，未收藏。</span><span style="font-size:9pt;"></span> <br /> <p class="MsoNormal"> <span style="font-size:9pt;">  <strong>FIAT 764 – Indanthrengelb 4GK.<span>  </span>“</strong>Colour Index.” <span> </span></span><span style="font-size:9pt;font-family:宋体;">如此，未注明</span><span style="font-size:9pt;">PB</span><span style="font-size:9pt;font-family:宋体;">报告号。</span><span style="font-size:9pt;"></span> <p class="MsoNormal"> <strong><span style="font-size:9pt;">  PB 73726, </span></strong><span style="font-size:9pt;">203-206. <strong>Fabrikationsvorschrift fuer Indanthrengelb 4GK </strong>Pulver roh.</span> <p class="MsoNormal"> <span style="font-size:9pt;"><strong>  PB 74778. </strong></span><span style="font-size:9pt;font-family:宋体;">商品化加工配方。</span><span style="font-size:9pt;"><span>           </span></span><span style="font-size:9pt;font-family:宋体;">未抄录。</span><span style="font-size:9pt;"></span> <p class="MsoNormal"> <span style="font-size:9pt;font-family:宋体;"><span style="font-family:Tahoma;">  </span><strong><u>阴丹士林黄</u></strong></span><strong><u><span style="font-size:9pt;">4Gk </span><span style="font-size:9pt;font-family:宋体;">生产工艺规程</span><span style="font-size:9pt;"> </span></u></strong><span style="font-size:9pt;"><span>          </span></span><span style="font-size:9pt;font-family:宋体;">译自</span><strong><span style="font-size:9pt;">PB 73726,</span></strong><span style="font-size:9pt;"> 203-206.</span> <p class="MsoNormal"> <strong><u><span style="font-size:9pt;font-family:宋体;">产品名称，学名，分子式和分子量：</span></u></strong><span style="font-size:9pt;"><span>   </span></span><span style="font-size:9pt;font-family:宋体;">阴丹士林黄</span><span style="font-size:9pt;">4GK. </span><span style="font-size:9pt;font-family:宋体;">其余见反应式。</span><span style="font-size:9pt;"></span> <br /> <p class="MsoNormal"> <strong><u><span style="font-size:9pt;font-family:宋体;">化学过程：</span></u></strong><strong><u><span style="font-size:9pt;"></span></u></strong> <br />   <span style="font-size:9pt;">5-</span><span style="font-size:9pt;font-family:宋体;">氨基</span><span style="font-size:9pt;">-1,9-</span><span style="font-size:9pt;font-family:宋体;">蒽并嘧啶蒽酮，在硝基苯中，在吡啶存在下，用</span><span style="font-size:9pt;">2,5-</span><span style="font-size:9pt;font-family:宋体;">二氯苯甲酰氯苯甲酰化。</span><span style="font-size:9pt;"></span> <p class="MsoNormal"> <strong><u><span style="font-size:9pt;font-family:宋体;">反应式：</span></u></strong><strong><u><span style="font-size:9pt;"></span></u></strong> <br /> <p class="MsoNormal"> <span style="font-size:9pt;"><img alt="" src="data:image/png;base64,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" /></span><span style="font-size:9pt;"></span> <br /> <p class="MsoNormal"> <span style="font-size:9pt;">5-</span><span style="font-size:9pt;font-family:宋体;">氨基</span><span style="font-size:9pt;">-1,9-</span><span style="font-size:9pt;font-family:宋体;">蒽并嘧啶蒽酮</span><span style="font-size:9pt;"><span>  </span>+<span>  </span>2,5-</span><span style="font-size:9pt;font-family:宋体;">二氯苯甲酰氯</span><span style="font-size:9pt;"><span>  </span></span><span style="font-size:9pt;font-family:Wingdings;"><span><span style="font-size:9pt;font-family:宋体;">→</span></span></span><span style="font-size:9pt;"><span>   </span>C.I. </span><span style="font-size:9pt;font-family:宋体;">还原黄</span><span style="font-size:9pt;">31.</span> <br /> <p class="MsoNormal"> <strong><u><span style="font-size:9pt;font-family:宋体;">理论与每百公斤投得量：</span></u></strong><span style="font-size:9pt;"><span>    </span>60 (100%)<span>  </span>+<span>  </span>50.9<span>   </span>=<span>  </span>102<span>  </span>+ 8.9</span> <br /> <p class="MsoNormal"> <span style="font-size:9pt;"><span>                         </span>100<span>        </span>+<span>  </span>84.8<span>   </span>=<span>  </span>170<span>  </span>+ 14.8</span> <br /> <p class="MsoNormal"> <strong><u><span style="font-size:9pt;font-family:宋体;">实际与每百公斤投得量：</span></u></strong><span style="font-size:9pt;"><span>    </span>60 (100%)<span>  </span>+<span>  </span>66<span>    </span>=<span>   </span>72 (100%)</span> <br /> <p class="MsoNormal"> <span style="font-size:9pt;"><span>           </span>100<span>  </span>+<span>  </span>110<span>  </span>=<span>  </span>120<span>  </span>= </span><span style="font-size:9pt;font-family:宋体;">收率：</span><span style="font-size:9pt;">70.6%</span> <br /> <p class="MsoNormal"> <strong><u><span style="font-size:9pt;font-family:宋体;">生产周期与日产量：</span></u></strong><span style="font-size:9pt;"><span>  </span></span><span style="font-size:9pt;font-family:宋体;">约</span><span style="font-size:9pt;">24</span><span style="font-size:9pt;font-family:宋体;">小时。</span><span style="font-size:9pt;">100%</span><span style="font-size:9pt;font-family:宋体;">计，约</span><span style="font-size:9pt;">72</span><span style="font-size:9pt;font-family:宋体;">公斤。</span><span style="font-size:9pt;"></span> <br /> <p class="MsoNormal"> <strong><u><span style="font-size:9pt;font-family:宋体;">设备：</span></u></strong><span style="font-size:9pt;"><span>  </span></span><span style="font-size:9pt;font-family:宋体;">略！</span><span style="font-size:9pt;"></span> <br /> <p class="MsoNormal"> <strong><u><span style="font-size:9pt;font-family:宋体;">操作步骤：</span></u></strong><strong><u><span style="font-size:9pt;"></span></u></strong> <br />   <span style="font-size:9pt;font-family:宋体;">在</span><span style="font-size:9pt;">500</span><span style="font-size:9pt;font-family:宋体;">升搪瓷锅内，先加入</span><span style="font-size:9pt;">500</span><span style="font-size:9pt;font-family:宋体;">公斤无水硝基苯，</span><span style="font-size:9pt;">30</span><span style="font-size:9pt;font-family:宋体;">公斤吡啶，然后加入</span><span style="font-size:9pt;">100%</span><span style="font-size:9pt;font-family:宋体;">计</span><span style="font-size:9pt;">5-</span><span style="font-size:9pt;font-family:宋体;">氨基</span><span style="font-size:9pt;">-1,9-</span><span style="font-size:9pt;font-family:宋体;">蒽并嘧啶蒽酮</span><span style="font-size:9pt;">60</span><span style="font-size:9pt;font-family:宋体;">公斤，加热到内温</span><span style="font-size:9pt;">80<sup>0</sup>C.</span><span style="font-size:9pt;font-family:宋体;">，在</span><span style="font-size:9pt;">30-40</span><span style="font-size:9pt;font-family:宋体;">分钟内，加入</span><span style="font-size:9pt;">66</span><span style="font-size:9pt;font-family:宋体;">公斤</span><span style="font-size:9pt;">2,5-</span><span style="font-size:9pt;font-family:宋体;">二氯苯甲酰氯，在</span><span style="font-size:9pt;">2-3</span><span style="font-size:9pt;font-family:宋体;">小时内升温到</span><span style="font-size:9pt;">125<sup>0</sup>C.</span><span style="font-size:9pt;font-family:宋体;">，保温反应</span><span style="font-size:9pt;">3</span><span style="font-size:9pt;font-family:宋体;">小时。<strong><u>取样</u></strong></span><strong><u><span style="font-size:9pt;">1.</span></u></strong><strong><span style="font-size:9pt;"> </span></strong><span style="font-size:9pt;font-family:宋体;">合格后，停搅拌冷到内温为</span><span style="font-size:9pt;">70-80<sup>0</sup>C.</span><span style="font-size:9pt;font-family:宋体;">，于衬铅吸滤器内吸滤，滤饼用约</span><span style="font-size:9pt;">300</span><span style="font-size:9pt;font-family:宋体;">公斤</span><span style="font-size:9pt;">70<sup>0</sup>C.</span><span style="font-size:9pt;font-family:宋体;">热硝基苯洗涤。<strong><u>取样</u></strong></span><strong><u><span style="font-size:9pt;">2.</span></u></strong><span style="font-size:9pt;"> </span><span style="font-size:9pt;font-family:宋体;">合格后，取二批滤饼，于水蒸汽蒸馏釜内蒸出硝基苯，蒸毕，用木压滤机压滤，滤饼用热水洗到中性后，送到干燥车间烘干。</span><span style="font-size:9pt;"></span> <br />   <strong><u><span style="font-size:9pt;font-family:宋体;">收率：</span></u></strong><span style="font-size:9pt;"><span>  </span></span><span style="font-size:9pt;font-family:宋体;">投入</span><span style="font-size:9pt;">60</span><span style="font-size:9pt;font-family:宋体;">公斤</span><span style="font-size:9pt;">100% 5-</span><span style="font-size:9pt;font-family:宋体;">氨基</span><span style="font-size:9pt;">-1,9-</span><span style="font-size:9pt;font-family:宋体;">蒽并嘧啶蒽酮，得</span><span style="font-size:9pt;">95</span><span style="font-size:9pt;font-family:宋体;">公斤阴丹士林黄</span><span style="font-size:9pt;">4GK</span><span style="font-size:9pt;font-family:宋体;">粗粉，含量约</span><span style="font-size:9pt;">76%</span><span style="font-size:9pt;font-family:宋体;">，合纯染料</span><span style="font-size:9pt;">72</span><span style="font-size:9pt;font-family:宋体;">公斤。</span><span style="font-size:9pt;"></span> <p class="MsoNormal"> <strong><u><span style="font-size:9pt;font-family:宋体;">操作要点及不正常原因：</span></u></strong><strong><span style="font-size:9pt;"></span></strong> <br /> <p class="MsoNormal"> <span style="font-size:9pt;">1.<span>  </span></span><span style="font-size:9pt;font-family:宋体;">缩合温度过高（</span><span style="font-size:9pt;">140-150<sup>0</sup>C.</span><span style="font-size:9pt;font-family:宋体;">）</span><span style="font-size:9pt;">,</span><span style="font-size:9pt;font-family:宋体;">染料发暗，在</span><span style="font-size:9pt;">120<sup>0</sup>C.</span><span style="font-size:9pt;font-family:宋体;">以下，反应慢。</span><span style="font-size:9pt;"></span> <br /> <p class="MsoNormal"> <span style="font-size:9pt;">2.<span>  </span>5-</span><span style="font-size:9pt;font-family:宋体;">氨基</span><span style="font-size:9pt;">-1,9-</span><span style="font-size:9pt;font-family:宋体;">蒽并嘧啶蒽酮必须反应完。</span><span style="font-size:9pt;"></span> <br /> <p class="MsoNormal"> <span style="font-size:9pt;">3.<span>  </span></span><span style="font-size:9pt;font-family:宋体;">缩合完毕，必须停搅拌冷却，这样好过滤。</span><span style="font-size:9pt;"></span> <br /> <p class="MsoNormal"> <span style="font-size:9pt;">4.<span>  </span></span><span style="font-size:9pt;font-family:宋体;">过量约</span><span style="font-size:9pt;">10%2,5-</span><span style="font-size:9pt;font-family:宋体;">二氯苯甲酰氯，是使反应完全所必须的。</span><span style="font-size:9pt;"></span> <br /> <p class="MsoNormal"> <strong><u><span style="font-size:9pt;font-family:宋体;">生产控制：</span></u></strong><strong><u><span style="font-size:9pt;"></span></u></strong> <br />   <u><span style="font-size:9pt;font-family:宋体;">取样</span></u><u><span style="font-size:9pt;">1</span></u><u><span style="font-size:9pt;font-family:宋体;">：</span></u><span style="font-size:9pt;"> </span><span style="font-size:9pt;font-family:宋体;">样品用显微镜观察，应为黄色片状的阴丹士林黄</span><span style="font-size:9pt;">4GK</span><span style="font-size:9pt;font-family:宋体;">，不应该出现蒽并嘧啶蒽酮的，小的红色针状体。</span><span style="font-size:9pt;"></span> <br />   <u><span style="font-size:9pt;font-family:宋体;">取样</span></u><u><span style="font-size:9pt;">2</span></u><u><span style="font-size:9pt;font-family:宋体;">：</span></u><span style="font-size:9pt;"> </span><span style="font-size:9pt;font-family:宋体;">滤饼可含硝基苯，而滤液必须是浅色。</span><span style="font-size:9pt;"></span> <p class="MsoNormal"> <strong><u><span style="font-size:9pt;font-family:宋体;">原料含量，杂质和分析方法：</span></u></strong><strong><u><span style="font-size:9pt;"></span></u></strong> <br />   <span style="font-size:9pt;">5-</span><span style="font-size:9pt;font-family:宋体;">氨基</span><span style="font-size:9pt;">-1,9-</span><span style="font-size:9pt;font-family:宋体;">蒽并嘧啶蒽酮，</span><span style="font-size:9pt;">100%</span><span style="font-size:9pt;font-family:宋体;">计。需通过实验室合成阴丹士林黄</span><span style="font-size:9pt;">4GK</span><span style="font-size:9pt;font-family:宋体;">。</span><span style="font-size:9pt;"> </span><span style="font-size:9pt;font-family:宋体;">其熔点：</span><span style="font-size:9pt;">250-255<sup>0</sup></span> <p class="MsoNormal"> <strong><u><span style="font-size:9pt;font-family:宋体;">溶剂回收：</span></u></strong><span style="font-size:9pt;"><span>  </span></span><span style="font-size:9pt;font-family:宋体;">略！</span><span style="font-size:9pt;"></span> <br /> <p class="MsoNormal"> <strong><u><span style="font-size:9pt;font-family:宋体;">废气和废汽：</span></u></strong><span style="font-size:9pt;"><span>  </span></span><span style="font-size:9pt;font-family:宋体;">少量盐酸气。</span><span style="font-size:9pt;"></span> <br /> <p class="MsoNormal"> <strong><u><span style="font-size:9pt;font-family:宋体;">成品含量，杂质和分析方法：</span></u></strong><strong><u><span style="font-size:9pt;"></span></u></strong> <br />   <span style="font-size:9pt;font-family:宋体;">阴丹士林黄</span><span style="font-size:9pt;">4GK</span><span style="font-size:9pt;font-family:宋体;">粗品含量约</span><span style="font-size:9pt;">76%</span><span style="font-size:9pt;font-family:宋体;">，是通过硫酸处理，测定其不溶物，并经与标准染色比较。</span><span style="font-size:9pt;"></span> <br /> <u><span style="font-size:9pt;font-family:宋体;">纯度测定方法：</span></u><u><span style="font-size:9pt;"></span></u> <br />   <span style="font-size:9pt;">50</span><span style="font-size:9pt;font-family:宋体;">克阴丹士林黄</span><span style="font-size:9pt;">4GK</span><span style="font-size:9pt;font-family:宋体;">粗粉，溶于</span><span style="font-size:9pt;">500</span><span style="font-size:9pt;font-family:宋体;">克</span><span style="font-size:9pt;">87%</span><span style="font-size:9pt;font-family:宋体;">硫酸中，其温度不要超过</span><span style="font-size:9pt;">20<sup>0</sup>C.</span><span style="font-size:9pt;font-family:宋体;">，溶解后倒入加有</span><span style="font-size:9pt;">1.5</span><span style="font-size:9pt;font-family:宋体;">公斤冰的</span><span style="font-size:9pt;">3.5</span><span style="font-size:9pt;font-family:宋体;">公斤水中，加入</span><span style="font-size:9pt;">75</span><span style="font-size:9pt;font-family:宋体;">克碳酸氢钠，加热到</span><span style="font-size:9pt;">90<sup>0</sup>C.</span><span style="font-size:9pt;font-family:宋体;">，冷至</span><span style="font-size:9pt;">70<sup>0</sup>C.</span><span style="font-size:9pt;font-family:宋体;">过滤，用热水洗到中性，并配成约</span><span style="font-size:9pt;">10%</span><span style="font-size:9pt;font-family:宋体;">膏状物。</span><span style="font-size:9pt;"></span> <br /> <u><span style="font-size:9pt;font-family:宋体;">收率：</span></u><span style="font-size:9pt;"><span>  </span></span><span style="font-size:9pt;font-family:宋体;">取约</span><span style="font-size:9pt;">475</span><span style="font-size:9pt;font-family:宋体;">克</span><span style="font-size:9pt;">10%</span><span style="font-size:9pt;font-family:宋体;">膏状物染料与约</span><span style="font-size:9pt;">80%</span><span style="font-size:9pt;font-family:宋体;">标样染色比较。</span><span style="font-size:9pt;"></span> <br /> <span style="font-size:9pt;font-family:宋体;">按硫酸测定不溶物（</span><span style="font-size:9pt;">95%</span><span style="font-size:9pt;font-family:宋体;">），染料强度</span><span style="font-size:9pt;">80%</span><span style="font-size:9pt;font-family:宋体;">计算：</span><span style="font-size:9pt;"><span>  </span>95 x 80 / 100 = <strong>76%</strong></span> <p class="MsoNormal"> <strong><u><span style="font-size:9pt;font-family:宋体;">加注：</span></u></strong><span style="font-size:9pt;"> <br />   </span><span style="font-size:9pt;font-family:宋体;">因读者未见过原件，现利用空间，将本人由缩微胶卷<strong><u>用手</u></strong>抄录的部分原文<strong><u>打字</u></strong>如下：</span><span style="font-size:9pt;"></span>  <br />   <strong><u><span style="font-size:9pt;">Fabrikationsvorschrift fuer Indanthrengelb 4GK Pulver roh </span></u></strong><span style="font-size:9pt;"> </span> <p class="MsoNormal"> <strong><u><span style="font-size:9pt;">Chemischer Vorgang:</span></u></strong> <br />   <span style="font-size:9pt;">Benzoylierung von <strong>Isopyrimidin </strong>mit 2,5-Dichlorbenzoylchlorid in Nitrobenzol bei Gegenwart von Pyridin.</span> <p class="MsoNormal"> <strong><u><span style="font-size:9pt;">Betribsvorschrift:</span></u></strong><span style="font-size:9pt;"></span> <br /> <span style="font-size:9pt;">  Im 500 l. Emaillekessel werden <strong>500</strong> kg. Nitrobenzol wasserfrei und <strong>30 </strong>kg. pyridine Fraktion Ib (Leverkusen) vorgelegt und <strong>60 </strong>kg. <strong>Isopyrimidin </strong>b. 100% eingetragen. Man heist auf <strong>80<sup>0</sup></strong> Innentemperatur und laesst in 30-40 Minuten. <strong>66 </strong>kg. 2,5-Dichlorbenzoylchlorid zulaufen. Dann wird in 2-3 Stunden auf <strong>125<sup>0</sup></strong> Innentemperatur geheizt und der Kesselinhalt <strong>3</strong> Stunden bei dieser Temperatur geruehr <strong><u>Probe 1.</u></strong> Wird die Probe gutgeheissen, laessst man ohne ruehren auf <strong>70-80<sup>0</sup></strong><sup> </sup>Innentemperatur erkalten, saugt auf der verbleiten <strong>Nutsche</strong> ab und waescht mit etwa <strong>300</strong> kg. ca. <strong>70<sup>0</sup></strong> warmem Nitrobenzol aus. <strong><u>Probe 2.</u></strong> Das Nutschgut von 2 Partien wird im ausgesteinten Wasserdampfdestillerer von Nitrobenzol befreit. Wenn alles Nitrobenzol abdestilliert ist, wird in die Holzpresse filtriert und mit warmen Wasser neutral gewaschen. Das Pressgut wird in <strong>Lu 611 </strong>getrocknet.</span> <br /> <p class="MsoNormal"> <strong><u><span style="font-size:9pt;">Ausbeute:</span></u></strong> <br />   <span style="font-size:9pt;">60 kg. Isopyrimidin ber. 100% geben etwa 95 kg. Ind. Gelb 4GK Pulver roh etwa 76%ig = 72 kg. Ind. Gelb 4GK Pulver roh b. 100%.</span> <p class="MsoNormal" style="text-indent:18pt;"> <span style="font-size:9pt;font-family:宋体;">以上供参考。</span><span style="font-size:9pt;"></span> <p class="MsoNormal"> <strong><span style="font-size:9pt;font-family:宋体;">陈忠源</span></strong><span style="font-size:9pt;"><span>    </span>2016</span><span style="font-size:9pt;font-family:宋体;">年</span><span style="font-size:9pt;">3</span><span style="font-size:9pt;font-family:宋体;">月</span><span style="font-size:9pt;">28</span><span style="font-size:9pt;font-family:宋体;">日。</span><span style="font-size:9pt;"></span> <br /><br /><br />本文地址：<a href="http://www.陈忠源化学文库.cn/Article.asp?ID=10000084" target="_blank">http://www.陈忠源化学文库.cn/Article.asp?ID=10000084</a>   填写邮件内容   邮件签名     填写邮件签名 发信地址     填写发信人的电子邮箱 　验证码     填写验证码，单击即可刷新验证码   发送协议 ·欢迎使用本站在线文章发送系统。 ·不得使用本站在线发送邮件系统发送垃圾邮件、广告邮件。 ·如果收信人地址或其服务器出现错误，可能无法成功发送。 ·如果有什么问题，或者意见建议，请联系[网站管理员]。

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