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发 送 文 章     CAS号 [612-45-3] 生产工艺 2-硝基-4-甲基乙酰苯胺 [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>CAS</u></strong></span><strong><u><span style="font-family:宋体;">号</span><span> [612-45-3] </span></u></strong><strong><u><span style="font-family:宋体;">生产工艺</span> </u><span><span>    </span>2-</span></strong><strong><span style="font-family:宋体;">硝基</span><span>-4-</span></strong><strong><span style="font-family:宋体;">甲基乙酰苯胺</span><span></span></strong> <br /> <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>Acetamide, </span></strong><span style="font-size:9pt;">N-(4-methyl-2-nitrophenyl)-</span> <br /> <strong><u><span style="font-size:9pt;font-family:宋体;">发明者：</span></u></strong><strong><span style="font-size:9pt;"><span>   </span>Winther, Laska, Zitscher<span>  </span>1911</span></strong><strong><span style="font-size:9pt;font-family:宋体;">年。</span></strong><strong><span style="font-size:9pt;"></span></strong> <br /> <strong><u><span style="font-size:9pt;font-family:宋体;">用途：</span></u></strong><span style="font-size:9pt;"><span>  </span></span><span style="font-size:9pt;font-family:宋体;">合成</span><span style="font-size:9pt;">2-</span><span style="font-size:9pt;font-family:宋体;">硝基</span><span style="font-size:9pt;">-4-</span><span style="font-size:9pt;font-family:宋体;">甲基苯胺。</span><span style="font-size:9pt;">[89-62-3]</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><u><span style="font-size:9pt;"></span></u></strong> <br /> <p class="MsoNormal"> <strong><u><span style="font-size:9pt;"><span style="text-decoration:none;"> </span></span></u></strong> <br /> <p class="MsoNormal"> <strong><u><span style="font-size:9pt;">FIAT 1313,II, 206.<span>  </span></span></u></strong><u><span style="font-size:9pt;font-family:宋体;">书本</span></u><u><span style="font-size:9pt;"> (= </span></u><u><span style="font-size:9pt;font-family:宋体;">缩微胶卷</span></u><u><span style="font-size:9pt;"> PB 85172,II, 206)<span>   </span>G. Siegle & Co.<span>                  </span><span>  </span></span></u><u><span style="font-size:9pt;font-family:宋体;">抄录如下。</span></u><u><span style="font-size:9pt;"></span></u> <br /> <p class="MsoNormal"> <u><span style="font-size:9pt;font-family:宋体;">反应式：</span></u><span style="font-size:9pt;"><span>  </span></span><span style="font-size:9pt;font-family:宋体;">本人加注。</span><span style="font-size:9pt;"></span> <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_01062016_095100.png" width="313" height="88" /></span><span style="font-size:9pt;"></span> <br /> <p class="MsoNormal"> <u><span style="font-size:9pt;">Nitration:</span></u> <br /> <p class="MsoNormal" style="text-indent:18pt;"> <strong><span style="font-size:9pt;">100 kg </span></strong><span style="font-size:9pt;">of <strong>acetyl para toluidine </strong>are added to the nitration vessel containing a mixture of <strong>198 kg nitric acid 65%</strong> and <strong>145 kg sulfuric acid 96%.</strong> The material is nitrated at <strong>28-30<sup>0</sup>C</strong> for about <strong>2 hours,</strong> after which the nitrated material is run under agitation into a vat containing <strong>600 l. water.</strong> The material is then filtered.</span> <br /> <p class="MsoNormal" style="text-indent:18pt;"> <span style="font-size:9pt;font-family:宋体;">以上是美国人译自德文的生产工艺，但未说明资料来源。其中译文，见：</span><span style="font-size:9pt;"></span> <br /> <p class="MsoNormal"> <span style="font-size:9pt;font-family:宋体;">张澍声</span><span style="font-size:9pt;"><span>  </span></span><span style="font-size:9pt;font-family:宋体;">精细化工中间体工业生产技术</span><span style="font-size:9pt;"> <span>– BIOS<span>  </span>FIAT<span>  </span>PB REPORTER<span>  </span>1964</span></span><span style="font-size:9pt;font-family:宋体;">年</span><span style="font-size:9pt;">4</span><span style="font-size:9pt;font-family:宋体;">月</span><span style="font-size:9pt;"><span>  </span></span><span style="font-size:9pt;font-family:宋体;">第</span><span style="font-size:9pt;">157</span><span style="font-size:9pt;font-family:宋体;">页。</span><span style="font-size:9pt;"></span> <br /> <p class="MsoNormal"> <span style="font-size:9pt;"> </span> <br /> <p class="MsoNormal"> <strong><u><span style="font-size:9pt;">PB 74026, 2334-2335.<span>  </span></span></u></strong><u><span style="font-size:9pt;font-family:宋体;">缩微胶卷。</span></u><u><span style="font-size:9pt;"><span>  </span>I. G. Levekusen.<span>   </span></span></u><u><span style="font-size:9pt;font-family:宋体;">是生产工艺原件。</span></u><u><span style="font-size:9pt;"><span>     </span><span>  </span></span></u><u><span style="font-size:9pt;font-family:宋体;">抄录如下。</span></u><u><span style="font-size:9pt;"> <span></span></span></u><br /> <strong><u><span style="font-size:9pt;">Hergang:</span></u></strong><span style="font-size:9pt;"><span>  </span>4-Acetyltoluidin wird in Schwefelsaeure mit Salpetersaeure in <strong>3</strong>-<strong>Stellung nitriert.</strong></span> <p class="MsoNormal"> <strong><u><span style="font-size:9pt;">Apparatur:</span></u></strong> <br /> <p class="MsoNormal"> <span style="font-size:9pt;">1)<span>  </span>2 ca. 2900 Liter gus</span><span style="font-size:9pt;">seisern Nitrierkessel mit Bleischlangen und Kuehlmantel fur Sole.<span>  </span>Dazu gehoeren:</span> <br /> <p class="MsoNormal" style="margin-left:18pt;text-indent:-18pt;"> <span style="font-size:9pt;"><span>    </span>Je 1 Schraubenruehrer mit 2 Fluegel und einem kleinem Mitnehmer an der Achse, um die einfliessende Salpetersaeure sofort gut unterzumischen (110 Touren) und fuer jeder Kessel ein Salpetersaeuremessgefass aus V<sub>2</sub>A-Metal.</span> <br /> <p class="MsoNormal" style="margin-left:18pt;text-indent:-18pt;"> <span style="font-size:9pt;">2)<span>  </span>2 eiserne 10000 Liter-Buetten, gummiert, ausgemauert und mit Asplittkaett gefugt, Holzruehrer und Bleischlangen fuer Wasserkuehlung.</span> <br /> <p class="MsoNormal" style="margin-left:18pt;text-indent:-18pt;"> <span style="font-size:9pt;">3)<span>  </span>2 eiserne Kastennutschen mit je ca. 5 cbm Inhalt, gummiert und saeurefest ausgemauert wie 2), Holzroste mitJuteleinenbespannung.</span> <br /> <p class="MsoNormal" style="margin-left:18.05pt;text-indent:-18.05pt;"> <strong><u><span style="font-size:9pt;">Einsatz:</span></u></strong><span style="font-size:9pt;"><span>  </span>je Nitrierkessel:<span>                         </span>500 kg Aceparatoluidin 100%ig Mol 149 (231.5 kg Nitrit)</span> <br /> <p class="MsoNormal" style="margin-left:18pt;text-indent:-18pt;"> <span style="font-size:9pt;"><span>    </span>1700 kg Schwefelsaeure 62.5 <sup>0</sup>Be“ = 82-83%ig.<span>     </span>312 kg Salpetersaeure 45.5<sup>0</sup>Be‘ = 80%ig</span> <br /> <p class="MsoNormal" style="margin-left:18.05pt;text-indent:-18.05pt;"> <strong><u><span style="font-size:9pt;">Verfahren:</span></u></strong><strong><span style="font-size:9pt;"><span>  </span></span></strong><u><span style="font-size:9pt;">Nitrierung:</span></u> <br /> <p class="MsoNormal" style="margin-left:18pt;text-indent:-18pt;"> <span style="font-size:9pt;"><span>    </span>Es werden in einem Nitrierkessel <strong>1700 kg Schwefelsaeure 62.5<sup>0</sup>Be‘</strong> eingefuellt, das is <strong>H<sub>2</sub>SO<sub>4</sub> =82%.<span>  </span></strong>Starkere </span><br /> <p class="MsoNormal" style="margin-left:18pt;text-indent:-18pt;"> <span style="font-size:9pt;">Saeure bewirkt die Bildung des <strong>Isomeren 1,2-Nitro-4-acettoluidde,<span>  </span>schwaechere Saeure</strong> bedingt<span>  </span>starkere </span><br /> <p class="MsoNormal" style="margin-left:18pt;text-indent:-18pt;"> <span style="font-size:9pt;">Zersetzung. Nun tragt man in etwa <strong><sup>1</sup>/<sub>2</sub> – 1 Std. 500 kg Acetparatoluidin </strong>100%ig Mol 149 (=231.5 kg Nitrit) d.i. <strong>510</strong></span> <br /> <p class="MsoNormal" style="margin-left:18.05pt;text-indent:-18.05pt;"> <strong><span style="font-size:9pt;">Kg </span></strong><span style="font-size:9pt;">98%ige Ware, bei <strong>25<sup>0</sup></strong> ein. Anfangs <strong>dunnfluessig,</strong> wird die Mischung nach ca. <strong>2 Stunden </strong>breiig <strong>dick</strong>, es<span>  </span>bildet</span> <br /> <p class="MsoNormal" style="margin-left:18pt;text-indent:-18pt;"> <span style="font-size:9pt;">sich das <strong>Sulfat</strong> des Acettoluide, es wird dann mit <strong>Sole</strong> auf <strong>20<sup>0</sup></strong> Heruehtgekuehlt. (</span><span style="font-size:9pt;font-family:宋体;">原文不清，可能有错</span><span style="font-size:9pt;">)</span><span style="font-size:9pt;font-family:宋体;">。</span><span style="font-size:9pt;"></span> <br /> <p class="MsoNormal" style="margin-left:18pt;text-indent:-18pt;"> <span style="font-size:9pt;"><span>    </span>Aus einem Messgefess, in weichem sich <span> </span><strong>312 kg Salpetersaeure 80%ig </strong>(45.5<sup>0</sup>Be‘) befinden, fliessen dann </span><br /> <p class="MsoNormal" style="margin-left:18pt;text-indent:-18pt;"> <span style="font-size:9pt;">unter dauernder Solekuhlung ..-achen <strong>18 </strong>und <strong>21<sup>0</sup></strong> die Haelfte der Salpetersaeure zu. (Dauer <strong>1 Std.</strong>) Hiernach wird </span><br /> <p class="MsoNormal" style="margin-left:18pt;text-indent:-18pt;"> <span style="font-size:9pt;">staerker gekuehlt, sodass waehrend der 2. Haelfte der nitrierung die <strong>Temperatur </strong>von <strong>20<sup>0 </sup></strong>nicht uberschriften wird.</span> <br /> <p class="MsoNormal" style="margin-left:18pt;text-indent:-18pt;"> <span style="font-size:9pt;">Dauer ca. <strong>1-2 Std. </strong>Wahrend des <strong>Nitrieren </strong>geht das <strong>Acettoluidinsulfat</strong> in Loesung, sodass gegen Ende ...</span> <br /> <p class="MsoNormal" style="margin-left:18.05pt;text-indent:-18.05pt;"> <strong><span style="font-size:9pt;">Gelbbraune </span></strong><span style="font-size:9pt;">klare Flusigkeit vorhanden ist. Unterhalb <strong>16<sup>0</sup></strong> tritt <strong>keine Nitrierung </strong>ein und bei zu <strong>hoher Nitrierungs-</strong></span> <br /> <p class="MsoNormal" style="margin-left:18.05pt;text-indent:-18.05pt;"> <strong><span style="font-size:9pt;">Temperatur </span></strong><span style="font-size:9pt;">(besonders am Schluss) fangt die Masse an zu Schaumen (<strong>Zersetzung</strong>)</span> <br /> <p class="MsoNormal" style="margin-left:18.05pt;text-indent:-18.05pt;"> <strong><span style="font-size:9pt;"><span>    </span></span></strong><span style="font-size:9pt;">Es wird nach <strong>2 Stunden </strong>bei <strong>18-20<sup>0 </sup></strong>nachgeruehrt.</span> <br /> <p class="MsoNormal" style="margin-left:18.05pt;text-indent:-18.05pt;"> <strong><u><span style="font-size:9pt;">Probe:</span></u></strong><span style="font-size:9pt;"><span>  </span>100 g Nitrierung werden im <strong>Labor</strong> auf in <sup>1</sup>/<sub>2</sub> Liter Eisswasser gegossen, abgenutscht, gewaschen, mit</span> <br /> <p class="MsoNormal" style="margin-left:18pt;text-indent:-18pt;"> <span style="font-size:9pt;">Sodaloesung uberdenkt, wieder gewaschen und trocken gesaugt.</span> <br /> <p class="MsoNormal" style="margin-left:18pt;text-indent:-18pt;"> <span style="font-size:9pt;"><span>    </span>Das erhaltene Nitroacettoluid wird in 100 ccm Eisessig geloest, in 1 Liter kaltes Wasser gegossen und einige </span><br /> <p class="MsoNormal" style="margin-left:18pt;text-indent:-18pt;"> <span style="font-size:9pt;">Stunden mit Zinkstaub reduziert, Salzsaeure zugegeben. Sodass stak kongosauer, filtriert und Filtrat diazotiert.</span> <br /> <p class="MsoNormal" style="margin-left:18pt;text-indent:-18pt;"> <span style="font-size:9pt;"><span>    </span><strong><u>Ergit:</u></strong> 6.8 g Nitrit d.i. 135 g Nitrit = <strong>80% Ausbeute.</strong></span> <br /> <p class="MsoNormal" style="margin-left:18pt;text-indent:-18pt;"> <span style="font-size:9pt;"><span>    </span>Die Nitrierung wird jetzt auf <strong>10<sup>0</sup></strong> abgekuehlt und in eine Buette in ca. <strong>7000 Liter</strong> kaltes <strong>Wasser</strong>(<strong>15<sup>0</sup></strong>)gedrueckt.</span> <br /> <p class="MsoNormal" style="margin-left:18pt;text-indent:-18pt;"> <span style="font-size:9pt;">Und dabei gekuehlt, sodass die Temperatur <strong>25<sup>0</sup></strong> nicht ubersteigt. Das Nitroacettoluidin faellt in keinen <strong>gelben </strong></span><br /> <p class="MsoNormal" style="margin-left:18.05pt;text-indent:-18.05pt;"> <strong><span style="font-size:9pt;">Koernern </span></strong><span style="font-size:9pt;">aus. Es wird auf eine Nutsche abgelassen (Ohne Vakuum) und mit Wasser (ca. <strong>2000 Liter</strong>) moegliechst</span> <br /> <p class="MsoNormal" style="margin-left:18pt;text-indent:-18pt;"> <span style="font-size:9pt;">Neutral gewaschen. Dann wird ueber das Nutschgut noch ca. <strong>3000 Liter</strong> Sodaloesung gegeben, welche is der </span><br /> <p class="MsoNormal" style="margin-left:18pt;text-indent:-18pt;"> <span style="font-size:9pt;">Buette aus <strong>50 kg Soda </strong>bereitet ist. Die Ablaufbruehe, die sauer <strong>hellgelb</strong> und klar ist, wird jetzt trueb und zuletzt</span> <br /> <p class="MsoNormal" style="margin-left:18.05pt;text-indent:-18.05pt;"> <strong><span style="font-size:9pt;">dunkelbraun</span></strong><span style="font-size:9pt;"> aber wieder klar. Es werden dann nochmals <strong>2000 Liter Wasser</strong> ueber die Nutsche gegeben, sodass</span> <br /> <p class="MsoNormal" style="margin-left:18pt;text-indent:-18pt;"> <span style="font-size:9pt;">der Ablauf zum Schluss neutral <strong>gelb</strong> und klar bleibt. Es wird dann moeglichst trocken genutscht.</span> <br /> <p class="MsoNormal" style="margin-left:18pt;text-indent:-18pt;"> <span style="font-size:9pt;"><span>    </span><strong><u>Ausbeute:</u></strong> ca. <strong>1300 kg </strong>feuchte Koerner.</span> <br /> <p class="MsoNormal" style="margin-left:18pt;text-indent:-18pt;"> <span style="font-size:9pt;"> </span> <br /> <p class="MsoNormal" style="margin-left:18pt;text-indent:-18pt;"> <span style="font-size:9pt;"><span>    </span></span><span style="font-size:9pt;font-family:宋体;">以上资料未见有英译文。这一资料的特点是说明硝化会有</span><span style="font-size:9pt;">2-</span><span style="font-size:9pt;font-family:宋体;">位体和</span><span style="font-size:9pt;">3-</span><span style="font-size:9pt;font-family:宋体;">位体。强酸会生成</span><span style="font-size:9pt;">2-</span><span style="font-size:9pt;font-family:宋体;">位体，弱酸</span><span style="font-size:9pt;"></span> <br /> <p class="MsoNormal" style="margin-left:18pt;text-indent:-18pt;"> <span style="font-size:9pt;font-family:宋体;">会引起乙酰基的水解等。另有硝化终点的控制。</span><span style="font-size:9pt;"></span> <br /> <p class="MsoNormal" style="margin-left:18pt;text-indent:-18pt;"> <span style="font-size:9pt;"> </span> <br /> <p class="MsoNormal" style="margin-left:18.05pt;text-indent:-18.05pt;"> <strong><u><span style="font-size:9pt;font-family:宋体;">加注：</span></u></strong><span style="font-size:9pt;"></span> <br /> <p class="MsoNormal" style="margin-left:18pt;text-indent:-18pt;"> <span style="font-size:9pt;"><span>    </span></span><span style="font-size:9pt;font-family:宋体;">据我所知，国内外科技人员，一般只知道英文资料</span><span style="font-size:9pt;">BIOS</span><span style="font-size:9pt;font-family:宋体;">和</span><span style="font-size:9pt;">FIAT</span><span style="font-size:9pt;font-family:宋体;">，因为它是书本，容易看。一些出版物</span><span style="font-size:9pt;"></span> <br /> <p class="MsoNormal" style="margin-left:18pt;text-indent:-18pt;"> <span style="font-size:9pt;font-family:宋体;">是利用它出版所谓新书。而</span><span style="font-size:9pt;">PB</span><span style="font-size:9pt;font-family:宋体;">报告是缩微胶卷，是德文，又没有目录可检索。前面我已提到</span><span style="font-size:9pt;">BIOS</span><span style="font-size:9pt;font-family:宋体;">和</span><span style="font-size:9pt;">FIAT</span> <br /> <p class="MsoNormal" style="margin-left:18pt;text-indent:-18pt;"> <span style="font-size:9pt;font-family:宋体;">是二手资料，译文不完全，有的还有错。现在提倡创新，了解一些产品历史，对研究以及开发应是可以的。</span><span style="font-size:9pt;"></span> <br /> <p class="MsoNormal" style="margin-left:18pt;text-indent:-18pt;"> <span style="font-size:9pt;"><span>    </span></span><span style="font-size:9pt;font-family:宋体;">以上供参考。</span><span style="font-size:9pt;"></span> <br /> <p class="MsoNormal" style="margin-left:18pt;text-indent:-18pt;"> <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;">5</span><span style="font-size:9pt;font-family:宋体;">月</span><span style="font-size:9pt;">31</span><span style="font-size:9pt;font-family:宋体;">日</span><span style="font-size:9pt;"><span>             </span></span><span style="font-size:9pt;font-family:宋体;">于</span><span style="font-size:9pt;"> </span><span style="font-size:9pt;font-family:宋体;">无锡</span><span style="font-size:9pt;"><span>  </span></span><span style="font-size:9pt;font-family:宋体;">明辉国际。</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=10000144" target="_blank">http://www.陈忠源化学文库.cn/Article.asp?ID=10000144</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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