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CAS号[1328-18-3]生产工艺-C.I.还原蓝19(C.I. 59805)
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<p class="MsoNormal"> <span style="font-family:宋体;"> </span> <br /> <p class="MsoNormal"> <span style="font-family:宋体;">【</span>CAS<span style="font-family:宋体;">名</span><span style="font-family:宋体;">】</span>Anthra[9,1,2-cde]benzo[rst]pentaphene-5,10-dione, bromo derivs.<o:p></o:p> <br /> <p class="MsoNormal"> <span style="font-family:宋体;">【</span><span style="font-family:宋体;">用途</span><span style="font-family:宋体;">】</span><span style="font-family:宋体;">织物染色</span><o:p></o:p> <br /> <p class="MsoNormal"> BIOS 987(=<span style="font-family:宋体;">胶卷</span><span style="font-family:Calibri;">PB 75960</span>), <i>German Dyestuffs and Intermediates industry Vat dyestuffs and Intermediates</i>.<o:p></o:p> <br /> <p class="MsoNormal"> BIOS 987, 6, Table 5, Indanthrene Navy Blue BF. (<span style="font-family:宋体;">结构式：略</span>)<o:p></o:p> <br /> <p class="MsoNormal"> BIOS 987, 75, Indanthrene Navy Blue BF, This is a monobromodibenzanthrone, [1328-18-3]<o:p></o:p> <br /> <p class="MsoNormal"> <br /> <p class="MsoNormal"> PB 25627, <i>Methods for production of dyestuffs</i>, 1929-1940, 1138<span style="font-family:宋体;">页</span>, Price: Microfilm $6.00, Enlargement print $114.00.<o:p></o:p> <br /> <p class="MsoNormal"> PB 25627, 2667-2668.'Kupenmarineblau 2232' n. d, Price: Microfilm $1.00, Photostat $1.00.<o:p></o:p> <br /> <p class="MsoNormal"> These are only preliminary directions for making a dye corresponding to a competitor’s 'Schwefelblau' and 'Kupenblau 104' from purified 'Violanthren G [116-71-2]', chlorosulfonic acid and sulfur, In German.<o:p></o:p> <br /> <p class="MsoNormal"> <br /> <p class="MsoNormal"> PB 73726, <i>Technical reports on dyestuffs</i>, dye intermediates, 1924-1945, 868<span style="font-family:宋体;">页</span>, Price: Microfilm $6.00, Enlargement print $87.00.<o:p></o:p> <br /> <p class="MsoNormal"> PB 73726, 199-201, Indanthrene marineblau BF, Jun 12, 1943, Price: $1.50, <span style="font-family:宋体;">以下为本人手工抄录文和译文</span>:<o:p></o:p> <br /> <p class="MsoNormal"> Alizarin-abteilung: Fabrikationsvorschrift für Indanthrenmarineblau BF Teig, 12 Juni 1943, <span style="font-family:宋体;">因手工抄的纸张，原文已无法再抄录。</span><o:p></o:p> <br /> <p class="MsoNormal"> <span style="font-family:宋体;">参考译文如下</span>: <o:p></o:p> <br /> <p class="MsoNormal"> C.I.<span style="font-family:宋体;">还原蓝</span><span style="font-family:Calibri;">19</span>(C.I. 59805), (<span style="font-family:宋体;">反应式：略</span>)<o:p></o:p> <br /> <p class="MsoNormal"> <span style="font-family:宋体;">【</span><span style="font-family:宋体;">设备</span><span style="font-family:宋体;">】</span>3.2<span style="font-family:宋体;">立方米溴化锅，配有加热，冷却蛇管；</span><span style="font-family:Calibri;">24</span><span style="font-family:宋体;">立方米衬砖稀释锅；</span><span style="font-family:Calibri;">38-40</span><span style="font-family:宋体;">框大型压滤机；</span><span style="font-family:Calibri;">14</span><span style="font-family:宋体;">立方米脱硫锅，配有加热蛇管；成品压滤机，铁或大型压滤机。</span><o:p></o:p> <br /> <p class="MsoNormal"> <span style="font-family:宋体;">【</span><span style="font-family:宋体;">操作步骤</span><span style="font-family:宋体;">】</span><o:p></o:p> <br /> <p class="MsoNormal"> 1. <span style="font-family:宋体;">溴化</span>: <span style="font-family:宋体;">在</span>3.2<span style="font-family:宋体;">立方米溴化锅内先加入</span><span style="font-family:Calibri;">1600</span><span style="font-family:宋体;">公斤氯磺酸 </span><span style="font-family:Calibri;">[7790-94-5]</span><span style="font-family:宋体;">，在搅拌转速</span><span style="font-family:Calibri;">40</span><span style="font-family:宋体;">转</span><span style="font-family:Calibri;">/</span><span style="font-family:宋体;">分，温度</span><span style="font-family:Calibri;">10 – 16</span>°C<span style="font-family:宋体;">条件下，通过装有可密闭，可转动叶轮的料斗，于</span>1 – 2<span style="font-family:宋体;">小时内加入</span><span style="font-family:Calibri;">200</span><span style="font-family:宋体;">公斤纯紫蒽酮</span><span style="font-family:Calibri;">G</span><span style="font-family:宋体;">粉 </span><span style="font-family:Calibri;">[116-71-2]</span><span style="font-family:宋体;">，同样，通过该</span> <span style="font-family:宋体;">料斗加入</span>130<span style="font-family:宋体;">公斤硫磺粉 </span><span style="font-family:Calibri;">[7704-34-9]</span><span style="font-family:宋体;">，加毕，密闭设备，通过加溴漏斗，加入</span><span style="font-family:Calibri;">100</span><span style="font-family:宋体;">公斤溴素 </span><span style="font-family:Calibri;">[7726-95-6]</span><span style="font-family:宋体;">，再次密闭设备，此时仅开启装有</span><span style="font-family:Calibri;">50</span><span style="font-family:宋体;">公分高的，</span><span style="font-family:Calibri;">96% </span><span style="font-family:宋体;">硫酸液封的可排气液阀，在</span><span style="font-family:Calibri;">2</span><span style="font-family:宋体;">小时内加热到</span><span style="font-family:Calibri;">25</span>°C<span style="font-family:宋体;">，再在</span>2<span style="font-family:宋体;">小时内加热到</span><span style="font-family:Calibri;">40</span>°C<span style="font-family:宋体;">，最后在</span>2<span style="font-family:宋体;">小时内加热到</span><span style="font-family:Calibri;">51–53</span>°C<span style="font-family:宋体;">，并在这一温度反应</span>10<span style="font-family:宋体;">小时，保温完毕，停止加热，通冷水冷却，同时在</span><span style="font-family:Calibri;">1–2</span><span style="font-family:宋体;">小时内加入</span><span style="font-family:Calibri;">800</span><span style="font-family:宋体;">公斤</span><span style="font-family:Calibri;">96% </span><span style="font-family:宋体;">硫酸，使温度维持在</span><span style="font-family:Calibri;">20–25</span>°C<span style="font-family:宋体;">。在</span>24<span style="font-family:宋体;">立方米稀释锅内，加入</span><span style="font-family:Calibri;">18</span><span style="font-family:宋体;">立方米水，然后在开启排气下，压入上述溴化料，充分搅拌后，用铺有硝化滤布的</span><span style="font-family:Calibri;">38–40</span><span style="font-family:宋体;">框大型压滤机过滤，用热水洗到中性。得阴丹士林海军蓝</span><span style="font-family:Calibri;">BF</span><span style="font-family:宋体;">粗制品约</span><span style="font-family:Calibri;">356</span><span style="font-family:宋体;">公斤。</span><o:p></o:p> <br /> <p class="MsoNormal"> 2. <span style="font-family:宋体;">脱硫</span>：<span style="font-family:宋体;">在</span>14<span style="font-family:宋体;">立方米脱硫锅内，加入</span><span style="font-family:Calibri;">9</span><span style="font-family:宋体;">立方米水，然后加入二批上述粗制滤饼，搅拌</span><span style="font-family:Calibri;">3–4</span><span style="font-family:宋体;">小时，再加入</span><span style="font-family:Calibri;">1100</span><span style="font-family:宋体;">公斤无水亚硫酸钠和</span><span style="font-family:Calibri;">380</span><span style="font-family:宋体;">公斤食盐，加热到</span><span style="font-family:Calibri;">90–95</span>°C<span style="font-family:宋体;">，并保温</span>2<span style="font-family:宋体;">小时</span>(<span style="font-family:宋体;">取样测终点</span>)<span style="font-family:宋体;">，取样合格后，再加入</span>380<span style="font-family:宋体;">公斤食盐，密闭设备，物料用铺有棉布和滤纸的压滤机过滤，滤饼用热水洗到中性。得脱硫滤饼约</span><span style="font-family:Calibri;">564</span><span style="font-family:宋体;">公斤，强度平均为</span><span style="font-family:Calibri;">100%</span><span style="font-family:宋体;">，以所投纯紫蒽酮</span><span style="font-family:Calibri;">G</span><span style="font-family:宋体;">计，得率：</span><span style="font-family:Calibri;">141%</span><span style="font-family:宋体;">。</span><o:p></o:p> <br /> <p class="MsoNormal"> 【<span style="font-family:宋体;">操作要点及不正常原因</span>】<span style="font-family:宋体;">纯紫蒽酮</span>G<span style="font-family:宋体;">含量应不低于</span><span style="font-family:Calibri;">95%</span><span style="font-family:宋体;">，否则染料强度达不到</span><span style="font-family:Calibri;">100%</span><span style="font-family:宋体;">。溴化温度不要超过</span><span style="font-family:Calibri;">51–53</span>°C<span style="font-family:宋体;">，否则染料会磺化，这可从溴化物过滤时，滤液的颜色变蓝看出。</span><o:p></o:p> <br /> <p class="MsoNormal"> 【<span style="font-family:宋体;">原料含量测定方法</span>】<span style="font-family:宋体;">染色。</span><o:p></o:p> <br /> <p class="MsoNormal"> 【<span style="font-family:宋体;">成品含量测定方法</span>】1. <span style="font-family:宋体;">染色</span>；2. <span style="font-family:宋体;">游离硫测定：取</span><span style="font-family:Calibri;">250</span><span style="font-family:宋体;">克滤饼，再抽滤，充分水洗。取出滤饼，用</span><span style="font-family:Calibri;">1000</span><span style="font-family:宋体;">毫升水打浆，加入</span><span style="font-family:Calibri;">60</span><span style="font-family:宋体;">克硫酸钠和</span><span style="font-family:Calibri;">25</span><span style="font-family:宋体;">克食盐，搅拌煮沸半小时，过滤，滤液加硫酸应无沉淀物。</span><o:p></o:p> <br /> <p class="MsoNormal"> 【<span style="font-family:宋体;">每批操作时间</span>】(a) <span style="font-family:宋体;">加料溴化</span><span style="font-family:Calibri;">24</span><span style="font-family:宋体;">小时；</span>(b) <span style="font-family:宋体;">洗涤</span><span style="font-family:Calibri;">24</span><span style="font-family:宋体;">小时</span>；(c) <span style="font-family:宋体;">脱硫 </span><span style="font-family:Calibri;">24</span><span style="font-family:宋体;">小时</span><o:p></o:p> <br /> <p class="MsoNormal"> 【<span style="font-family:宋体;">日生产能力</span>】<span style="font-family:宋体;">约</span>282<span style="font-family:宋体;">公斤阴丹士林海军蓝</span><span style="font-family:Calibri;">BF</span>，100%<span style="font-family:宋体;">。</span><o:p></o:p> <br /> <p class="MsoNormal"> <br /> <p class="MsoNormal"> <span style="font-family:宋体;">何岩彬主编《染料品种大全》</span>，<span style="font-family:宋体;">沈阳出版社出版</span>，2018<span style="font-family:宋体;">年</span>，P. 1509，C.I.<span style="font-family:宋体;">还原蓝</span><span style="font-family:Calibri;">19</span>(C.I. 59805)<o:p></o:p> <br /> <p class="MsoNormal"> <br /> <p class="MsoNormal"> <span style="font-family:宋体;">陈忠源</span> 2021<span style="font-family:宋体;">年</span><span style="font-family:Calibri;">9</span><span style="font-family:宋体;">月</span><span style="font-family:Calibri;">24</span><span style="font-family:宋体;">日</span>，<span style="font-family:宋体;">星期五</span><o:p></o:p> <br /> <br /> <br /> <br /> <p class="MsoNormal"> <span style="font-family:宋体;"></span><span style="font-family:宋体;"></span><span style="font-family:Calibri;"></span><span style="font-family:宋体;"></span><span style="font-family:Calibri;"></span><span style="font-family:宋体;"></span><span style="font-family:宋体;"></span><o:p></o:p> <br /><br /><br />本文地址：<a href="http://www.陈忠源化学文库.cn/Article.asp?ID=10001634" target="_blank">http://www.陈忠源化学文库.cn/Article.asp?ID=10001634</a>
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