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发 送 文 章     CAS号 [95-74-9] 生产工艺，3-氯-4-甲基苯胺 [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" align="center" style="font-size:medium;white-space:normal;text-align:center;"> <span lang="EN-US" style="font-size:16pt;">CAS</span><span style="font-size:16pt;font-family:宋体;">号</span><span lang="EN-US" style="font-size:16pt;"> [95-74-9] </span><span style="font-size:16pt;font-family:宋体;">生产工艺，</span><span lang="EN-US" style="font-size:16pt;">3-</span><span style="font-size:16pt;font-family:宋体;">氯</span><span lang="EN-US" style="font-size:16pt;">-4-</span><span style="font-size:16pt;font-family:宋体;">甲基苯胺</span><span lang="EN-US" style="font-size:16pt;"><o:p></o:p></span> <br /> <p class="MsoNormal" style="font-size:medium;white-space:normal;"> <span lang="EN-US" style="font-size:12pt;"> </span> <br /> <p class="MsoNormal" style="font-size:medium;white-space:normal;"> <span lang="EN-US" style="font-size:12pt;">CAS</span><span style="font-size:12pt;font-family:宋体;">名：</span><span lang="EN-US" style="font-size:12pt;">Benzenamine, 3-chloro-4-methyl      Beil. 12, 988<o:p></o:p></span> <br /> <p class="MsoNormal" style="font-size:medium;white-space:normal;"> <span style="font-size:12pt;font-family:宋体;">用途：染料中间体：</span><span lang="EN-US" style="font-size:12pt;">2B</span><span style="font-size:12pt;font-family:宋体;">酸</span><span lang="EN-US" style="font-size:12pt;"> [88-51-7]</span><span style="font-size:12pt;font-family:宋体;">；农药中间体：绿麦隆</span><span lang="EN-US" style="font-size:12pt;"> [15545-48-9]</span><span style="font-size:12pt;font-family:宋体;">等。</span><span lang="EN-US" style="font-size:12pt;"><o:p></o:p></span> <br /> <p class="MsoNormal" style="font-size:medium;white-space:normal;"> <span style="font-size:12pt;font-family:宋体;">生产工艺，生产过程：</span><span lang="EN-US" style="font-size:12pt;">3-</span><span style="font-size:12pt;font-family:宋体;">氯</span><span lang="EN-US" style="font-size:12pt;">-4-</span><span style="font-size:12pt;font-family:宋体;">甲基硝基苯用铁粉或硫化钠还原，或者是加氢还原。</span><span lang="EN-US" style="font-size:12pt;"><o:p></o:p></span> <br /> <p class="MsoNormal" style="font-size:medium;white-space:normal;"> <span lang="EN-US" style="font-size:12pt;">PB 25602. Manufacturing methods of“Basefabrik”and other manufacturing methods. Apr. 1946，</span><span style="font-size:12pt;font-family:宋体;">共</span><span lang="EN-US" style="font-size:12pt;">1430</span><span style="font-size:12pt;font-family:宋体;">页（沈阳院有此胶卷）。</span><span lang="EN-US" style="font-size:12pt;"><o:p></o:p></span> <br /> <p class="MsoNormal" style="font-size:medium;white-space:normal;"> <span lang="EN-US" style="font-size:12pt;">PB 25602, P.891-892, 2-Chloro-p-toluidine, crude.  </span><span style="font-size:12pt;font-family:宋体;">美国人介绍：资料是采用铁粉还原法，本人未抄录。</span><span lang="EN-US" style="font-size:12pt;"><o:p></o:p></span> <br /> <p class="MsoNormal" style="font-size:medium;white-space:normal;"> <span lang="EN-US" style="font-size:12pt;"> </span> <br /> <p class="MsoNormal" style="font-size:medium;white-space:normal;"> <span style="font-size:12pt;font-family:宋体;">候乐山</span><span style="font-size:12pt;"> </span><span style="font-size:12pt;font-family:宋体;">主编《中国精细化工产品集</span><span style="font-size:12pt;"> <span lang="EN-US">– </span></span><span style="font-size:12pt;font-family:宋体;">原料及中间体</span><span lang="EN-US" style="font-size:12pt;">10396</span><span style="font-size:12pt;font-family:宋体;">种》。中国化工信息中心</span><span style="font-size:12pt;"> </span><span style="font-size:12pt;font-family:宋体;">出版。</span><span lang="EN-US" style="font-size:12pt;">2006</span><span style="font-size:12pt;font-family:宋体;">年，</span><span lang="EN-US" style="font-size:12pt;">3-</span><span style="font-size:12pt;font-family:宋体;">氯对甲苯胺，摘录</span><span lang="EN-US" style="font-size:12pt;"><o:p></o:p></span> <br /> <p class="MsoNormal" style="font-size:medium;white-space:normal;"> <span lang="EN-US" style="font-size:12pt;">P. 862</span><span style="font-size:12pt;font-family:宋体;">【生产方法】</span><span lang="EN-US" style="font-size:12pt;">1. </span><span style="font-size:12pt;font-family:宋体;">氯化</span><span lang="EN-US" style="font-size:12pt;"> [121-86-8] </span><span style="font-size:12pt;font-family:宋体;">（</span><span style="font-size:12pt;font-family:宋体;">已在</span><span lang="EN-US" style="font-size:12pt;">2016</span><span style="font-size:12pt;font-family:宋体;">年</span><span lang="EN-US" style="font-size:12pt;">12</span><span style="font-size:12pt;font-family:宋体;">月</span><span lang="EN-US" style="font-size:12pt;">5</span><span style="font-size:12pt;font-family:宋体;">日上传发布。）</span><span lang="EN-US" style="font-size:12pt;"><o:p></o:p></span> <br /> <p class="MsoNormal" style="font-size:medium;white-space:normal;"> <span lang="EN-US" style="font-size:12pt;">2. </span><span style="font-size:12pt;font-family:宋体;">还原：将配好的硫化钠溶液加入反应锅内，在</span><span lang="EN-US" style="font-size:12pt;">70 – 80</span><span style="font-size:12pt;font-family:宋体;">℃</span><span style="font-size:12pt;font-family:宋体;">加入上述</span><span lang="EN-US" style="font-size:12pt;">2-</span><span style="font-size:12pt;font-family:宋体;">氯</span><span lang="EN-US" style="font-size:12pt;">-4-</span><span style="font-size:12pt;font-family:宋体;">硝基甲苯，回流</span><span lang="EN-US" style="font-size:12pt;">4 h</span><span style="font-size:12pt;font-family:宋体;">，温度为</span><span lang="EN-US" style="font-size:12pt;">110±5</span><span style="font-size:12pt;font-family:宋体;">℃</span><span style="font-size:12pt;font-family:宋体;">，胺油纯度＞</span><span lang="EN-US" style="font-size:12pt;">98.5%</span><span style="font-size:12pt;font-family:宋体;">，熔点＞</span><span lang="EN-US" style="font-size:12pt;">19</span><span style="font-size:12pt;font-family:宋体;">℃</span><span style="font-size:12pt;font-family:宋体;">时，蒸馏，得成品，收率</span><span lang="EN-US" style="font-size:12pt;">90%</span><span style="font-size:12pt;font-family:宋体;">。</span><span lang="EN-US" style="font-size:12pt;"><o:p></o:p></span> <br /> <p class="MsoNormal" style="font-size:medium;white-space:normal;"> <span style="font-size:12pt;font-family:宋体;">如果采用铁粉还原，反应温度</span><span lang="EN-US" style="font-size:12pt;">100</span><span style="font-size:12pt;font-family:宋体;">℃</span><span style="font-size:12pt;font-family:宋体;">左右，反应物用甲苯萃取。收率</span><span lang="EN-US" style="font-size:12pt;">95%</span><span style="font-size:12pt;font-family:宋体;">。</span><span lang="EN-US" style="font-size:12pt;"><o:p></o:p></span> <br /> <p class="MsoNormal" style="font-size:medium;white-space:normal;"> <span lang="EN-US" style="font-size:12pt;"> </span> <br /> <p class="MsoNormal" style="font-size:medium;white-space:normal;"> <span lang="EN-US" style="font-size:12pt;">P. 837 </span><span style="font-size:12pt;font-family:宋体;">绿麦隆。其中【生产方法】</span><span lang="EN-US" style="font-size:12pt;"><o:p></o:p></span> <br /> <p class="MsoNormal" style="font-size:medium;white-space:normal;"> <span lang="EN-US" style="font-size:12pt;">1. </span><span style="font-size:12pt;font-family:宋体;">氯化：将对硝基甲苯在三氯化铁与碘下与氯反应。</span><span lang="EN-US" style="font-size:12pt;"><o:p></o:p></span> <br /> <p class="MsoNormal" style="font-size:medium;white-space:normal;"> <span lang="EN-US" style="font-size:12pt;">2. </span><span style="font-size:12pt;font-family:宋体;">还原：</span><span lang="EN-US" style="font-size:12pt;">3-</span><span style="font-size:12pt;font-family:宋体;">氯</span><span lang="EN-US" style="font-size:12pt;">-4-</span><span style="font-size:12pt;font-family:宋体;">甲苯硝基苯以雷尼镍作催化剂，通氢气进行催化加氢反应得。</span><span lang="EN-US" style="font-size:12pt;"><o:p></o:p></span> <br /> <p class="MsoNormal" style="font-size:medium;white-space:normal;"> <span lang="EN-US" style="font-size:12pt;"> </span> <br /> <p class="MsoNormal" style="font-size:medium;white-space:normal;"> <span lang="EN-US" style="font-size:12pt;">P. 877</span><span style="font-size:12pt;font-family:宋体;">，</span><span lang="EN-US" style="font-size:12pt;">3-</span><span style="font-size:12pt;font-family:宋体;">氯</span><span lang="EN-US" style="font-size:12pt;">-4-</span><span style="font-size:12pt;font-family:宋体;">甲基苯胺。资料中无生产方法。</span><span lang="EN-US" style="font-size:12pt;"><o:p></o:p></span> <br /> <p class="MsoNormal" style="font-size:medium;white-space:normal;"> <span lang="EN-US" style="font-size:12pt;"> </span> <br /> <p class="MsoNormal" style="font-size:medium;white-space:normal;"> <span style="font-size:12pt;font-family:宋体;">许丹倩</span><span lang="EN-US" style="font-size:12pt;">  </span><span style="font-size:12pt;font-family:宋体;">严新焕</span><span lang="EN-US" style="font-size:12pt;">  </span><span style="font-size:12pt;font-family:宋体;">徐振元（浙江工业大学）。《低压液相催化加氢合成</span><span lang="EN-US" style="font-size:12pt;">3-</span><span style="font-size:12pt;font-family:宋体;">氯</span><span lang="EN-US" style="font-size:12pt;">-4-</span><span style="font-size:12pt;font-family:宋体;">甲苯胺研究》。</span><span lang="EN-US" style="font-size:12pt;">[J] </span><span style="font-size:12pt;font-family:宋体;">染料工业，</span><span lang="EN-US" style="font-size:12pt;">2001, 1, P.16-18</span><span style="font-size:12pt;font-family:宋体;">。</span><span lang="EN-US" style="font-size:12pt;"><o:p></o:p></span> <br /> <p class="MsoNormal" style="font-size:medium;white-space:normal;"> <span style="font-size:12pt;font-family:宋体;">反应过程：</span><span lang="EN-US" style="font-size:12pt;">3-</span><span style="font-size:12pt;font-family:宋体;">氯</span><span lang="EN-US" style="font-size:12pt;">-4-</span><span style="font-size:12pt;font-family:宋体;">甲基硝基苯，采用骨架镍（抄注：</span><span lang="EN-US" style="font-size:12pt;">CAS</span><span style="font-size:12pt;font-family:宋体;">号</span><span lang="EN-US" style="font-size:12pt;">[7440-02-0]</span><span style="font-size:12pt;font-family:宋体;">，分子量</span><span lang="EN-US" style="font-size:12pt;">58.69</span><span style="font-size:12pt;font-family:宋体;">）为催化剂进行加氢还原。摘录如下：</span><span lang="EN-US" style="font-size:12pt;"><o:p></o:p></span> <br /> <p class="MsoNormal" style="font-size:medium;white-space:normal;"> <span lang="EN-US" style="font-size:12pt;">2  </span><span style="font-size:12pt;font-family:宋体;">实验部分</span><span lang="EN-US" style="font-size:12pt;"><o:p></o:p></span> <br /> <p class="MsoNormal" style="font-size:medium;white-space:normal;"> <span lang="EN-US" style="font-size:12pt;">2.2  </span><span style="font-size:12pt;font-family:宋体;">催化加氢还原</span><span lang="EN-US" style="font-size:12pt;"><o:p></o:p></span> <br /> <p class="MsoNormal" style="font-size:medium;white-space:normal;"> <span style="font-size:12pt;font-family:宋体;">在高压釜中依次加入</span><span lang="EN-US" style="font-size:12pt;">100 g 3-<span style="font-family:宋体;">氯</span></span><span lang="EN-US" style="font-size:12pt;">-4-</span><span style="font-size:12pt;font-family:宋体;">甲基硝基苯</span><span lang="EN-US" style="font-size:12pt;">, </span><span style="font-size:12pt;font-family:宋体;">催化剂</span><span lang="EN-US" style="font-size:12pt;">, </span><span style="font-size:12pt;font-family:宋体;">助剂</span><span lang="EN-US" style="font-size:12pt;">, </span><span style="font-size:12pt;font-family:宋体;">和溶剂甲醇，分别用氮气和氢气置换出釜内空气后，通入氢气至一定压力，开动搅拌，升温至规定温度，反应至不吸氢为止。降温，出料，过滤，滤液进行</span><span lang="EN-US" style="font-size:12pt;">GC</span><span style="font-size:12pt;font-family:宋体;">和</span><span lang="EN-US" style="font-size:12pt;">GC/MS</span><span style="font-size:12pt;font-family:宋体;">分析。</span><span lang="EN-US" style="font-size:12pt;"><o:p></o:p></span> <br /> <p class="MsoNormal" style="font-size:medium;white-space:normal;"> <span lang="EN-US" style="font-size:12pt;">3.  </span><span style="font-size:12pt;font-family:宋体;">结果与讨论。略！</span><span lang="EN-US" style="font-size:12pt;"><o:p></o:p></span> <br /> <p class="MsoNormal" style="font-size:medium;white-space:normal;"> <span lang="EN-US" style="font-size:12pt;">4.  </span><span style="font-size:12pt;font-family:宋体;">结论。摘录</span><span lang="EN-US" style="font-size:12pt;"><o:p></o:p></span> <br /> <p class="MsoNormal" style="font-size:medium;white-space:normal;"> <span style="font-size:12pt;font-family:宋体;">根据试验结果，该加氢反应的较佳条件为：</span><span lang="EN-US" style="font-size:12pt;">Raney </span><span style="font-size:12pt;font-family:宋体;">催化剂（抄注：</span><span lang="EN-US" style="font-size:12pt;">Raney nickel catalyst</span><span style="font-size:12pt;font-family:宋体;">，其</span><span lang="EN-US" style="font-size:12pt;">CAS</span><span style="font-size:12pt;font-family:宋体;">号</span><span lang="EN-US" style="font-size:12pt;"> [7440-02-2]</span><span style="font-size:12pt;font-family:宋体;">）和助剂用量分别选硝基物质量的</span><span lang="EN-US" style="font-size:12pt;">3% </span><span style="font-size:12pt;font-family:宋体;">和</span><span lang="EN-US" style="font-size:12pt;">1%</span><span style="font-size:12pt;font-family:宋体;">，反应温度</span><span lang="EN-US" style="font-size:12pt;">80 – 90</span><span style="font-size:12pt;font-family:宋体;">℃</span><span style="font-size:12pt;font-family:宋体;">，每克硝基物用溶剂甲醇</span><span lang="EN-US" style="font-size:12pt;">1.3 – 6 ml</span><span style="font-size:12pt;font-family:宋体;">，氢压</span><span lang="EN-US" style="font-size:12pt;">1.0 MPa.<o:p></o:p></span> <br /> <p class="MsoNormal" style="font-size:medium;white-space:normal;"> <span style="font-size:12pt;font-family:宋体;">【参考文献】</span><span lang="EN-US" style="font-size:12pt;">5</span><span style="font-size:12pt;font-family:宋体;">篇</span><span lang="EN-US" style="font-size:12pt;"><o:p></o:p></span> <br /> <p class="MsoNormal" style="font-size:medium;white-space:normal;"> <span lang="EN-US" style="font-size:12pt;"> </span> <br /> <p class="MsoNormal" style="font-size:medium;white-space:normal;"> <span style="font-size:12pt;font-family:宋体;">何岩彬</span><span style="font-size:12pt;"> </span><span style="font-size:12pt;font-family:宋体;">主编</span><span style="font-size:12pt;"> </span><span style="font-size:12pt;font-family:宋体;">《染料品种大全》。沈阳出版社</span><span style="font-size:12pt;"> </span><span style="font-size:12pt;font-family:宋体;">出版。</span><span lang="EN-US" style="font-size:12pt;">2018</span><span style="font-size:12pt;font-family:宋体;">年。</span><span lang="EN-US" style="font-size:12pt;">P. 1885. </span><span style="font-size:12pt;font-family:宋体;">未列，可增补！</span><span style="font-size:12pt;"> </span><span style="font-size:12pt;font-family:宋体;">中文名称：</span><span lang="EN-US" style="font-size:12pt;">3-</span><span style="font-size:12pt;font-family:宋体;">氯</span><span lang="EN-US" style="font-size:12pt;">-4-</span><span style="font-size:12pt;font-family:宋体;">甲基苯胺。</span><span lang="EN-US" style="font-size:12pt;"><o:p></o:p></span> <br /> <p class="MsoNormal" style="font-size:medium;white-space:normal;"> <span style="font-size:12pt;font-family:宋体;">用途：合成</span><span lang="EN-US" style="font-size:12pt;">2 B</span><span style="font-size:12pt;font-family:宋体;">酸，见</span><span lang="EN-US" style="font-size:12pt;">p. 1886</span><span style="font-size:12pt;font-family:宋体;">，</span><span style="font-size:12pt;font-family:宋体;">中文名称：</span><span lang="EN-US" style="font-size:12pt;">2-</span><span style="font-size:12pt;font-family:宋体;">氨基</span><span lang="EN-US" style="font-size:12pt;">-4-</span><span style="font-size:12pt;font-family:宋体;">氯</span><span lang="EN-US" style="font-size:12pt;">-5-</span><span style="font-size:12pt;font-family:宋体;">甲基苯磺酸。别名：</span><span lang="EN-US" style="font-size:12pt;">2 B</span><span style="font-size:12pt;font-family:宋体;">酸。</span><span lang="EN-US" style="font-size:12pt;"><o:p></o:p></span> <br /> <p class="MsoNormal" style="font-size:medium;white-space:normal;"> <span style="font-size:12pt;font-family:宋体;">【可合成的染料】</span><span lang="EN-US" style="font-size:12pt;">C.I. </span><span style="font-size:12pt;font-family:宋体;">颜料黄</span><span lang="EN-US" style="font-size:12pt;">85, 86, 191, 191:1</span><span style="font-size:12pt;font-family:宋体;">。</span><span lang="EN-US" style="font-size:12pt;">C.I. </span><span style="font-size:12pt;font-family:宋体;">颜料红</span><span lang="EN-US" style="font-size:12pt;">48, 48:1, 48:2, 48:3, 48:4, 48:5, 48:6, 69, 211, 243, 243:1</span><span style="font-size:12pt;font-family:宋体;">。</span><span lang="EN-US" style="font-size:12pt;"><o:p></o:p></span> <br /> <p class="MsoNormal" style="font-size:medium;white-space:normal;"> <span lang="EN-US" style="font-size:12pt;"> </span> <br /> <p class="MsoNormal" style="font-size:medium;white-space:normal;"> <span style="font-size:12pt;font-family:宋体;">抄注：换了新的图标，本人已不会用了，所以从今以后不再画结构式，改用反应过程说明，对不起</span><span lang="EN-US" style="font-size:12pt;">!<o:p></o:p></span> <br /> <p class="MsoNormal" style="font-size:medium;white-space:normal;"> <span lang="EN-US" style="font-size:12pt;"> </span> <br /> <p class="MsoNormal" style="font-size:medium;white-space:normal;"> <span style="font-size:12pt;font-family:宋体;">陈忠源，首次</span><span style="font-size:12pt;font-family:宋体;">上传于</span><span lang="EN-US" style="font-size:12pt;">2021</span><span style="font-size:12pt;font-family:宋体;">年</span><span lang="EN-US" style="font-size:12pt;">2</span><span style="font-size:12pt;font-family:宋体;">月</span><span lang="EN-US" style="font-size:12pt;">20</span><span style="font-size:12pt;font-family:宋体;">日星期六</span><span lang="EN-US" style="font-size:12pt;">/ </span><span style="font-size:12pt;font-family:宋体;">修改、增补于</span><span lang="EN-US" style="font-size:12pt;">2021</span><span style="font-size:12pt;font-family:宋体;">年</span><span lang="EN-US" style="font-size:12pt;">7</span><span style="font-size:12pt;font-family:宋体;">月</span><span lang="EN-US" style="font-size:12pt;">1</span><span style="font-size:12pt;font-family:宋体;">日星期四</span><span lang="EN-US" style="font-size:12pt;"><o:p></o:p></span> <br /><br /><br />本文地址：<a href="http://www.陈忠源化学文库.cn/Article.asp?ID=10001596" target="_blank">http://www.陈忠源化学文库.cn/Article.asp?ID=10001596</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。 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