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发 送 文 章     CAS号 [81-46-9] 生产工艺。 1-氨基-4-苯甲酰氨基蒽醌 [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" align="center" style="text-align:center;"> CAS<span style="font-family:宋体;">号 </span><span style="font-family:Calibri;">[81-46-9] </span><span style="font-family:宋体;">生产工艺。   </span><span style="font-family:Calibri;">1-</span><span style="font-family:宋体;">氨基</span><span style="font-family:Calibri;">-4-</span><span style="font-family:宋体;">苯甲酰氨基蒽醌</span><o:p></o:p> <br /> <p class="MsoNormal"> CAS<span style="font-family:宋体;">名：</span><span style="font-family:Calibri;">Benzamide, N-(4-amino-9,10-dihydro-9,10dioxo-1-anthracenyl)-</span><o:p></o:p> <br /> <p class="MsoNormal"> <span style="font-family:宋体;">用途：还原染料中间体。</span>LookChem<span style="font-family:宋体;">网登录生产与经营单位</span><span style="font-family:Calibri;">8</span><span style="font-family:宋体;">家。</span><o:p></o:p> <br /> <p class="MsoNormal"> BIOS 1484, 4.<span style="font-family:宋体;">（</span><span style="font-family:Calibri;">=</span><span style="font-family:宋体;">胶卷</span><span style="font-family:Calibri;">PB 86139</span><span style="font-family:宋体;">）。 </span><span style="font-family:Calibri;">1-Amino-4-benzoylaminoanthraquinone</span><span style="font-family:宋体;">（</span><span style="font-family:Calibri;">Leverkusen</span><span style="font-family:宋体;">）。英国人译自德文。</span><o:p></o:p> <br /> <p class="MsoNormal"> <img src="http://www.陈忠源化学文库.cn//chenzhongyuan/Upload/ArticlePicture/QQ截图20210610094333.jpg" alt="" style="white-space:normal;" /><br /> Plant: (1)  1000 l. enamelled C. I. pan with jacket.   (2)  4 sq. m. pressure filter.    (3)  3 cbm. Venuleth. <br /> <p class="MsoNormal"> <o:p></o:p> <br /> <p class="MsoNormal"> Method:<o:p></o:p> <br /> <p class="MsoNormal"> 100 kg. of leuco 1,4-diaminoanthraquinone is added to 700 l. of nitrobenzene at 100℃.  1 l. of piperidine is added as catalyst and the charge heated to 150℃.  After cooling to 15℃., 60 kg. of soda ash and 2 l. of water are added, followed by 100 l. of benzoyl chloride.  The temperature must not be higher than 45℃.  The batch is cooled to 25℃., filtered on the pressure filter and washed twice with 250 l. of nitrobenzene.  The cake is stirred with 250 l. of hydrochloric acid and 800 l. of water, filtered, washed four times with 500 l. warm water at 50℃. and dried in the Venuleth.<o:p></o:p> <br /> <p class="MsoNormal"> Yield = 90% of theory.<o:p></o:p> <br /> <p class="MsoNormal">   <br /> <p class="MsoNormal"> FIAT 1313, II, 25-6.<span style="font-family:宋体;">（</span><span style="font-family:Calibri;">=</span><span style="font-family:宋体;">胶卷</span><span style="font-family:Calibri;">PB 85172</span><span style="font-family:宋体;">）。 </span><span style="font-family:Calibri;">1-Amino-4-benzoyl amino anthraquinone</span><span style="font-family:宋体;">。  美国人译自德文。</span><o:p></o:p> <br /> <p class="MsoNormal"> This product is manufactured at Leverkusen by benzoylation of 1,4-diamino anthraquione, with benzoyl chloride in nitrobenzene.  A brief description of the operating method is given below.<o:p></o:p> <br /> <p class="MsoNormal"> 1000 kg. of leuco-1,4-diamino anthraquinone,  700 liters of nitrobenzene,  1 liter of piperidine.<o:p></o:p> <br /> <p class="MsoNormal"> The above ingredients are charged into a 1000 liter enamelled, jacketed, agitated kettle, equipped with steam and water for heating and cooling.  The mixture is heated to 1500 and held under agitation until a sample examined under the microscope shows that oxidation is complete.  When satisfactory the charge is cooled down to 150 and to the mixture are then added.  60 kg. of sodium carbonate,  2 liters of water.<o:p></o:p> <br /> <p class="MsoNormal"> The temperature of the mixture is now raised to 50 – 55℃., and the following previously prepared mixture of  70 kg. of benzoyl chloride,  140 kg. of nitrobrnzene is run in slowly during 2 – 3 hours, under agitation, keeping the temperature between 50 - 550 after which temperature is slowly raised to 600 and held at this point for 1 hour longer when the charge is tested for completion of the reaction, which is done by comparison of a sample dissolved in 50 : 50 mixture of pyridine and alcohol with that of satisfactory material similarly treated.  This is also checked by microscopic examination.<o:p></o:p> <br /> <p class="MsoNormal"> When the reaction is satisfactory the charge is cooled to 250 and filtered off in an proof brick lined agitated pressure nutsch.  The nutsch layer is first washed with two 250 liter washes of nitrobenzene and then slurried in the nutsch with 250 liters of hydrochloric acid(31%), 800 liters of water.<o:p></o:p> <br /> <p class="MsoNormal"> This slurry is then filtered and the nutsch layer repeatedly rinsed with four 500 liter water washes at 500, after which it is slurried with water and transferred to a 3 cubic meter Venuleth where it is dried.<o:p></o:p> <br /> <p class="MsoNormal"> Yield= 139 kg. of 1-amino-4benzoylamino anthraquinone. (90%) = 125 kg. of 1-amino-4-benzoyl anthraquinone (100% equiv.) = 87% of theory.<o:p></o:p> <br /> <p class="MsoNormal">   <br /> <p class="MsoNormal"> <span style="font-family:宋体;">张澍声《精细化工中间体工业生产技术》。《染料工业》编辑部</span> <span style="font-family:宋体;">出版。</span>1996<span style="font-family:宋体;">年。</span>P. 233.  1-<span style="font-family:宋体;">氨基</span><span style="font-family:Calibri;">-4-</span><span style="font-family:宋体;">苯甲酰氨基蒽醌，译自</span><span style="font-family:Calibri;">FIAT.</span><o:p></o:p> <br /> <p class="MsoNormal"> <span style="font-family:宋体;">在</span>1000 L<span style="font-family:宋体;">带搅拌的陶瓷衬里釜中加入</span><span style="font-family:Calibri;">100 kg 1,4-</span><span style="font-family:宋体;">二氨基蒽醌隐色体，</span><span style="font-family:Calibri;">700 L</span><span style="font-family:宋体;">硝基苯和</span><span style="font-family:Calibri;">1 L</span><span style="font-family:宋体;">哌啶，混合物加热到</span><span style="font-family:Calibri;">150</span>℃<span style="font-family:宋体;">，在此温度下进行搅拌，直至取样在显微镜下检验氧化已经完全。混合物冷却到</span>15℃<span style="font-family:宋体;">，然后加入</span>60 kg <span style="font-family:宋体;">碳酸钠和</span><span style="font-family:Calibri;">2 L</span><span style="font-family:宋体;">水，升温至</span><span style="font-family:Calibri;">50 </span>– 55℃<span style="font-family:宋体;">。另将</span>70 kg <span style="font-family:宋体;">苯甲酰氯和</span><span style="font-family:Calibri;">140 kg</span><span style="font-family:宋体;">硝基苯预先准备成溶液，于</span><span style="font-family:Calibri;">2 </span>– 3<span style="font-family:宋体;">小时内在搅拌下缓缓加入，保持温度在</span><span style="font-family:Calibri;">50 </span>– 55℃<span style="font-family:宋体;">，然后温度缓缓升至</span>60℃<span style="font-family:宋体;">，在</span>60℃<span style="font-family:宋体;">保持</span>1<span style="font-family:宋体;">小时以上。取样溶解于</span><span style="font-family:Calibri;">50 </span><span style="font-family:宋体;">：</span><span style="font-family:Calibri;">50</span><span style="font-family:宋体;">吡啶和乙醇混合物中，在显微镜下检验，与标准品相同。</span><o:p></o:p> <br /> <p class="MsoNormal"> <span style="font-family:宋体;">当反应已经满意后，冷却到</span>25℃<span style="font-family:宋体;">，过滤，滤饼先用</span>250 L<span style="font-family:宋体;">硝基苯洗涤，然后在抽滤器上用</span><span style="font-family:Calibri;">250 L 31% </span><span style="font-family:宋体;">盐酸和</span><span style="font-family:Calibri;">800 L</span><span style="font-family:宋体;">水的溶液打浆，浆液进行过滤，并</span><span style="font-family:Calibri;">4</span><span style="font-family:宋体;">次用</span><span style="font-family:Calibri;">500 L</span><span style="font-family:宋体;">水洗涤，洗涤后，将浆料送入</span><span style="font-family:Calibri;">3</span><span style="font-family:宋体;">立方米耙式干燥器中干燥。</span><o:p></o:p> <br /> <p class="MsoNormal"> <span style="font-family:宋体;">得</span>139 kg 90% 1-<span style="font-family:宋体;">氨基</span><span style="font-family:Calibri;">-4-</span><span style="font-family:宋体;">苯甲酰氨基蒽醌，相当于</span><span style="font-family:Calibri;">125 kg </span><span style="font-family:宋体;">纯品，收率为理论量的</span><span style="font-family:Calibri;">87%</span><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;">唐培堃（天津大学化工系）。《</span>1-<span style="font-family:宋体;">氨基</span><span style="font-family:Calibri;">-4-</span><span style="font-family:宋体;">苯甲酰氨基蒽醌制备方法的探讨》。</span><span style="font-family:Calibri;">[J] </span><span style="font-family:宋体;">染料情报（天津），</span><span style="font-family:Calibri;">1983, 1, 18-20(41).</span><span style="font-family:宋体;">摘录如下：</span><o:p></o:p> <br /> <p class="MsoNormal"> <span style="font-family:宋体;">西德专利</span>2,937,876<span style="font-family:宋体;">（</span><span style="font-family:Calibri;">81, 4, 2</span><span style="font-family:宋体;">）</span><span style="font-family:Calibri;">=(</span><span style="font-family:宋体;">日开特 昭</span><span style="font-family:Calibri;">56-51439) </span><span style="font-family:宋体;">指出，用</span><span style="font-family:Calibri;">1,4-</span><span style="font-family:宋体;">二氨基蒽醌隐色体为原料制备</span><span style="font-family:Calibri;">1-</span><span style="font-family:宋体;">氨基</span><span style="font-family:Calibri;">-4-</span><span style="font-family:宋体;">苯甲酰氨基蒽醌的方法存在很多缺点。并提出了用</span><span style="font-family:Calibri;">1,4-</span><span style="font-family:宋体;">二氨基蒽醌为原料，在少量脂肪酸族叔胺醇或季胺化合物存在下进行单苯甲酰化的方法。</span><o:p></o:p> <br /> <p class="MsoNormal"> DE 2,937,876<span style="font-family:宋体;">的实例</span><span style="font-family:Calibri;">1</span><span style="font-family:宋体;">：在</span><span style="font-family:Calibri;">250 ml</span><span style="font-family:宋体;">硝基苯中加入</span><span style="font-family:Calibri;">30 g 1,4-</span><span style="font-family:宋体;">二氨基蒽醌（纯度</span><span style="font-family:Calibri;">91%</span><span style="font-family:宋体;">），</span><span style="font-family:Calibri;">14 g </span><span style="font-family:宋体;">碳酸钠和</span><span style="font-family:Calibri;">0.2 g </span><span style="font-family:宋体;">三甲基</span><span style="font-family:Calibri;">-</span><span style="font-family:宋体;">乙醇氢氧化铵（</span><span style="font-family:Calibri;">60% </span><span style="font-family:宋体;">水溶液），充分混合后，补加</span><span style="font-family:Calibri;">0.9 ml</span><span style="font-family:宋体;">水，将混合物加热至</span><span style="font-family:Calibri;">35 </span>– 40℃<span style="font-family:宋体;">，用</span>3<span style="font-family:宋体;">小时滴加</span><span style="font-family:Calibri;">16 ml </span><span style="font-family:宋体;">苯甲酰氯，然后在</span><span style="font-family:Calibri;">100</span>℃<span style="font-family:宋体;">保温</span>2 – 3 <span style="font-family:宋体;">小时，再滴加不多于</span><span style="font-family:Calibri;">6 ml</span><span style="font-family:宋体;">的苯甲酰氯。当蒲板色层分析分析指出只有痕迹量的原始反应物（＜</span><span style="font-family:Calibri;">0.5%</span><span style="font-family:宋体;">），并生成微量双苯甲酰化产物（＜</span><span style="font-family:Calibri;">2%</span><span style="font-family:宋体;">）时，即可认为反应已达终点。加入</span><span style="font-family:Calibri;">1 ml</span><span style="font-family:宋体;">水，用减压蒸馏法蒸出硝基苯，得到</span><span style="font-family:Calibri;">65 g</span><span style="font-family:宋体;">产品。产品中含有</span><span style="font-family:Calibri;">58% 1-</span><span style="font-family:宋体;">氨基</span><span style="font-family:Calibri;">-4-</span><span style="font-family:宋体;">苯甲酰氨基蒽醌。</span><span style="font-family:Calibri;">0.4% 1,4-</span><span style="font-family:宋体;">二氨基蒽醌和</span><span style="font-family:Calibri;">1.5% 1,4-</span><span style="font-family:宋体;">双苯甲酰氨基蒽醌。</span><span style="font-family:Calibri;">1-</span><span style="font-family:宋体;">氨基</span><span style="font-family:Calibri;">-4-</span><span style="font-family:宋体;">苯甲酰氨基蒽醌为理论量的</span><span style="font-family:Calibri;">94.%</span><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;">赵维绳</span>  <span style="font-family:宋体;">陈</span> <span style="font-family:宋体;">彬</span>  <span style="font-family:宋体;">汪维凤</span> <span style="font-family:宋体;">编著《还原染料》。化学工业出版社</span> <span style="font-family:宋体;">出版。</span>1993<span style="font-family:宋体;">年。</span>P. 97.  1-<span style="font-family:宋体;">氨基</span><span style="font-family:Calibri;">-4-</span><span style="font-family:宋体;">苯甲酰氨基蒽醌。</span><o:p></o:p> <br /> <p class="MsoNormal"> <span style="font-family:宋体;">为了提高收率，可采用隐色体酰化法，即先将</span>1,4-<span style="font-family:宋体;">二氨基蒽醌还原为隐色体，再于硝基苯和少量哌啶溶液中，加热到</span><span style="font-family:Calibri;">150</span>℃<span style="font-family:宋体;">，使隐色体溶解，冷至</span>15℃<span style="font-family:宋体;">，加入碳酸钠缚酸剂，用苯甲酰氯酰化，过滤，用盐酸洗去为反应的二氨基蒽醌，可得</span>1-<span style="font-family:宋体;">氨基</span><span style="font-family:Calibri;">-4-</span><span style="font-family:宋体;">苯甲酰氨基蒽醌，收率为</span><span style="font-family:Calibri;">90%</span><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</span> <span style="font-family:宋体;">主编《染料品种大全》。沈阳出版社</span> <span style="font-family:宋体;">出版。</span> 2018<span style="font-family:宋体;">年。 </span>P. 2030.  <span style="font-family:宋体;">中文名称：</span><span style="font-family:Calibri;">1-</span><span style="font-family:宋体;">氨基</span><span style="font-family:Calibri;">-4-</span><span style="font-family:宋体;">苯甲酰氨基蒽醌。</span><o:p></o:p> <br /> <p class="MsoNormal"> <span style="font-family:宋体;">【可合成的染料】</span>C.I. <span style="font-family:宋体;">还原橙</span><span style="font-family:Calibri;">17</span><span style="font-family:宋体;">；</span><span style="font-family:Calibri;">C.I. </span><span style="font-family:宋体;">还原红</span><span style="font-family:Calibri;">44</span><span style="font-family:宋体;">；</span><span style="font-family:Calibri;">C.I. </span><span style="font-family:宋体;">还原紫</span><span style="font-family:Calibri;">16</span><span style="font-family:宋体;">；</span><span style="font-family:Calibri;">C.I. </span><span style="font-family:宋体;">还原棕</span><span style="font-family:Calibri;">3</span><span style="font-family:宋体;">：</span><span style="font-family:Calibri;">C.I.</span><span style="font-family:宋体;">可还原棕</span><span style="font-family:Calibri;">3</span><span style="font-family:宋体;">；</span><span style="font-family:Calibri;">C.I. </span><span style="font-family:宋体;">还原棕</span><span style="font-family:Calibri;">25</span><span style="font-family:宋体;">；</span><span style="font-family:Calibri;">C.I. </span><span style="font-family:宋体;">还原棕</span><span style="font-family:Calibri;">84</span><span style="font-family:宋体;">；</span><span style="font-family:Calibri;">C.I. </span><span style="font-family:宋体;">还原黑</span><span style="font-family:Calibri;">27</span><span style="font-family:宋体;">：</span><span style="font-family:Calibri;">C.I. </span><span style="font-family:宋体;">还原黑</span><span style="font-family:Calibri;">29</span><span style="font-family:宋体;">： </span><span style="font-family:Calibri;">C.I. </span><span style="font-family:宋体;">还原黑</span><span style="font-family:Calibri;">30</span><span style="font-family:宋体;">；</span><span style="font-family:Calibri;">C.I. </span><span style="font-family:宋体;">颜料棕</span><span style="font-family:Calibri;">28</span><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;">陈忠源</span> 2020<span style="font-family:宋体;">年。</span><span style="font-family:Calibri;">/ 2021</span><span style="font-family:宋体;">年</span><span style="font-family:Calibri;">6</span><span style="font-family:宋体;">月</span><span style="font-family:Calibri;">9</span><span style="font-family:宋体;">日星期三。<br /> </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=10001586" target="_blank">http://www.陈忠源化学文库.cn/Article.asp?ID=10001586</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。 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