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发 送 文 章     C.I.分散红60 = C.I.溶剂红146 (C.I. 60756)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;">分散红</span><span>60 = C.I.</span></u></strong><strong><u><span style="font-family:宋体;">溶剂红</span><span>146 (C.I. 60756)</span></u></strong><strong><u><span style="font-family:宋体;">生产工艺</span></u><span>    CAS</span></strong><strong><span style="font-family:宋体;">号：</span><span>[17418-58-5]</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;"><span>  </span>9,10-ANthracenedione, </span></strong><span style="font-size:9pt;">1-amino-4-hydroxy-2-phenoxy-</span> <br /> <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 title="" alt="" src="http://www.陈忠源化学文库.cn//chenzhongyuan/Upload/ArticlePicture/IMG_17022016_112519.png" width="509" height="120" /></span><span style="font-size:9pt;"></span> <br /> <p class="MsoNormal"> <span style="font-size:9pt;font-family:宋体;">苯酚  </span><span style="font-size:9pt;font-family:宋体;">苯酚钾盐  </span><span style="font-size:9pt;">1-</span><span style="font-size:9pt;font-family:宋体;">氨基</span><span style="font-size:9pt;">-2-</span><span style="font-size:9pt;font-family:宋体;">溴</span><span style="font-size:9pt;">-4-</span><span style="font-size:9pt;font-family:宋体;">羟基蒽醌  </span><span style="font-size:9pt;font-family:宋体;">分散红</span><span style="font-size:9pt;">60 = </span><span style="font-size:9pt;font-family:宋体;">溶剂红</span><span style="font-size:9pt;">146</span> <p class="MsoNormal"> <strong><u><span style="font-size:9pt;font-family:宋体;">操作步骤：</span></u></strong><span style="font-size:9pt;"></span> <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;">加仑搪玻璃反应锅内，加入</span><span style="font-size:9pt;">1338</span><span style="font-size:9pt;font-family:宋体;">磅<strong>苯酚</strong>，开动搅拌，加入</span><span style="font-size:9pt;">185</span><span style="font-size:9pt;font-family:宋体;">磅<strong>氢氧化钾</strong>，加热到</span><span style="font-size:9pt;">145<sup>0</sup>C.</span><span style="font-size:9pt;font-family:宋体;">，在</span><span style="font-size:9pt;">145-155<sup>0</sup>C.</span><span style="font-size:9pt;font-family:宋体;">保温反应</span><span style="font-size:9pt;">1.5-3</span><span style="font-size:9pt;font-family:宋体;">小时，冷却到</span><span style="font-size:9pt;">120<sup>0</sup>C.</span><span style="font-size:9pt;font-family:宋体;">，然后慢慢加入</span><span style="font-size:9pt;">100%</span><span style="font-size:9pt;font-family:宋体;">计</span><strong><span style="font-size:9pt;">1-</span></strong><strong><span style="font-size:9pt;font-family:宋体;">氨基</span></strong><strong><span style="font-size:9pt;">-2-</span></strong><strong><span style="font-size:9pt;font-family:宋体;">溴</span></strong><strong><span style="font-size:9pt;">-4-</span></strong><strong><span style="font-size:9pt;font-family:宋体;">羟基蒽醌</span></strong><span style="font-size:9pt;">712</span><span style="font-size:9pt;font-family:宋体;">磅，加料时，温度不能低于</span><span style="font-size:9pt;">90<sup>0</sup>C.</span><span style="font-size:9pt;font-family:宋体;">，必要时可加热保持在</span><span style="font-size:9pt;">90-120<sup>0</sup>C.</span><span style="font-size:9pt;font-family:宋体;">，整个过程约需</span><span style="font-size:9pt;">0.5-1</span><span style="font-size:9pt;font-family:宋体;">小时。加毕，加热到</span><span style="font-size:9pt;">145<sup>0</sup>C.</span> <p class="MsoNormal"> <span style="font-size:9pt;font-family:宋体;">在</span><span style="font-size:9pt;">145-155<sup>0</sup>C.</span><span style="font-size:9pt;font-family:宋体;">保温</span><span style="font-size:9pt;">6-8</span><span style="font-size:9pt;font-family:宋体;">小时，取样用</span><span style="font-size:9pt;">TLC</span><span style="font-size:9pt;font-family:宋体;">法测终点。合格后，加入</span><span style="font-size:9pt;">175</span><span style="font-size:9pt;font-family:宋体;">加仑水，并冷却到</span><span style="font-size:9pt;">50<sup>0</sup>C.</span><span style="font-size:9pt;font-family:宋体;">，在</span><span style="font-size:9pt;">50-55<sup>0</sup>C.</span><span style="font-size:9pt;font-family:宋体;">搅拌</span><span style="font-size:9pt;">2</span><span style="font-size:9pt;font-family:宋体;">小时。过滤。</span><span style="font-size:9pt;"></span> <br />   <span style="font-size:9pt;font-family:宋体;">滤饼用</span><span style="font-size:9pt;">550</span><span style="font-size:9pt;font-family:宋体;">加仑</span><span style="font-size:9pt;">80<sup>0</sup>C.</span><span style="font-size:9pt;font-family:宋体;">热水洗涤，每次用</span><span style="font-size:9pt;">225</span><span style="font-size:9pt;font-family:宋体;">加仑，洗到滤饼不再含有游离苯酚为止。滤液和洗液收集后可用来回收苯酚。</span><span style="font-size:9pt;"></span> <br />   <strong><u><span style="font-size:9pt;">TLC </span></u></strong><strong><u><span style="font-size:9pt;font-family:宋体;">：</span></u></strong><span style="font-size:9pt;"> </span><span style="font-size:9pt;font-family:宋体;">取样，用丙酮溶解，用甲苯展开，不再有</span><span style="font-size:9pt;">1-</span><span style="font-size:9pt;font-family:宋体;">氨基</span><span style="font-size:9pt;">-2-</span><span style="font-size:9pt;font-family:宋体;">溴</span><span style="font-size:9pt;">-4-</span><span style="font-size:9pt;font-family:宋体;">羟基蒽醌斑点。</span><span style="font-size:9pt;"></span> <p class="MsoNormal"> <strong><u><span style="font-size:9pt;font-family:宋体;">分散加工：</span></u></strong><span style="font-size:9pt;"> </span><span style="font-size:9pt;font-family:宋体;">仅适用于分散红</span><span style="font-size:9pt;">60.<br />   </span><span style="font-size:9pt;font-family:宋体;">分散剂：</span><span style="font-size:9pt;">Lignosol D-30.<span>   </span></span><span style="font-size:9pt;font-family:宋体;">砂磨介质：</span><span style="font-size:9pt;">Reax 96 A.<span>   </span></span><span style="font-size:9pt;font-family:宋体;">润湿剂：</span><span style="font-size:9pt;">Petrosperse 98 </span><span style="font-size:9pt;font-family:宋体;">或</span><span style="font-size:9pt;"> Igepal CO-880.</span> <br />   <span style="font-size:9pt;font-family:宋体;">防尘剂：</span><span style="font-size:9pt;">Twitchell 6808.</span> <p class="MsoNormal"> <strong><span style="font-size:9pt;font-family:宋体;">陈忠源</span></strong><strong><span style="font-size:9pt;"><span>  </span></span></strong><span style="font-size:9pt;">1986</span><span style="font-size:9pt;font-family:宋体;">年按内部资料编译。</span><span style="font-size:9pt;"></span>   <p class="MsoNormal"> <strong><u><span style="font-size:9pt;font-family:宋体;">上染染料生产工艺汇编：</span></u></strong><span style="font-size:9pt;"> 438-439 (1976)<span>  </span></span><span style="font-size:9pt;font-family:宋体;">抄录。</span><span style="font-size:9pt;"></span> <br />   <strong><u><span style="font-size:9pt;font-family:宋体;">缩合：<br /> </span></u></strong><span style="font-size:9pt;font-family:宋体;">  在锅中加入碳酸钠</span><span style="font-size:9pt;">46</span><span style="font-size:9pt;font-family:宋体;">公斤，苯酚</span><span style="font-size:9pt;">292</span><span style="font-size:9pt;font-family:宋体;">公斤。加热到</span><span style="font-size:9pt;">120<sup>0</sup>C.</span><span style="font-size:9pt;font-family:宋体;">，加入</span><span style="font-size:9pt;">1-</span><span style="font-size:9pt;font-family:宋体;">氨基</span><span style="font-size:9pt;">-2-</span><span style="font-size:9pt;font-family:宋体;">溴</span><span style="font-size:9pt;">-4-</span><span style="font-size:9pt;font-family:宋体;">羟基蒽醌</span><span style="font-size:9pt;">165</span><span style="font-size:9pt;font-family:宋体;">公斤。</span><span style="font-size:9pt;">2</span><span style="font-size:9pt;font-family:宋体;">小时升温到</span><span style="font-size:9pt;">140<sup>0</sup>C.</span><span style="font-size:9pt;font-family:宋体;">，在</span><span style="font-size:9pt;">140-145<sup>0</sup>C.</span><span style="font-size:9pt;font-family:宋体;">保温</span><span style="font-size:9pt;">6-8</span><span style="font-size:9pt;font-family:宋体;">小时。</span><span style="font-size:9pt;"></span> <br />   <span style="font-size:9pt;font-family:宋体;">于</span><span style="font-size:9pt;">140<sup>0</sup>C/160</span><span style="font-size:9pt;font-family:宋体;">毫米汞柱蒸去苯酚，加水</span><span style="font-size:9pt;">400</span><span style="font-size:9pt;font-family:宋体;">升打浆，过滤，洗至中性，滤饼为</span><span style="font-size:9pt;">1-</span><span style="font-size:9pt;font-family:宋体;">氨基</span><span style="font-size:9pt;">-2-</span><span style="font-size:9pt;font-family:宋体;">苯氧基</span><span style="font-size:9pt;">-4-</span><span style="font-size:9pt;font-family:宋体;">羟基蒽醌。</span><span style="font-size:9pt;"></span> <p class="MsoNormal" style="text-indent:17.25pt;"> <strong><u><span style="font-size:9pt;font-family:宋体;">后处理：</span></u></strong><strong><u><span style="font-size:9pt;"></span></u></strong> <br />   <span style="font-size:9pt;font-family:宋体;">在砂磨锅内加入滤饼半批，适量水及</span><span style="font-size:9pt;">165</span><span style="font-size:9pt;font-family:宋体;">公斤扩散剂</span><span style="font-size:9pt;">NNO</span><span style="font-size:9pt;font-family:宋体;">。在</span><span style="font-size:9pt;">90<sup>0</sup>C.</span><span style="font-size:9pt;font-family:宋体;">砂磨</span><span style="font-size:9pt;">14</span><span style="font-size:9pt;font-family:宋体;">小时，干燥，粉碎及标准化，得染料</span><span style="font-size:9pt;">280</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;">抄录说明：</span></u></strong><span style="font-size:9pt;"><span>   </span></span><span 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