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原位在线拉曼光谱分析仪在微通道反应器上的应用

来源：耶拿分析仪器（北京）有限公司分类：动态 2023-11-15 10:37:41 13阅读次数

1

引言

化工及制药过程涉及到很多的有机合成过程，这些过程的主反应大多条件苛刻、机理复杂且危险性大。如常见的硝化反应、格氏反应、氢化等过程。控制不当，有可能会发生爆炸、火灾等事故。因此，在实际的实验室工艺开发、中试及生产过程需要通过改进设备来改善整个过程传质及传热的局限性，同时需要采用先进的在线监测手段去实时监测进程，实现数据监测和控制的同步。

连续流反应设备—微通道反应器和原位在线拉曼光谱仪的结合正好可以满足有机合成过程的需求。本文将介绍原位在线拉曼光谱和微通道反应器结合的应用。

2

实验

微通道反应器本质上讲是一种连续流动的管道式反应器。它包括化工单元所需要的混合器、换热器、反应器控制器等。传统的釜式设备在传质和传热方面都具有局限性，而连续流微通道反应器具有持液量小、高效传质、传热，是应对高危有机合成过程的有效方案。

作为有机合成过程或制药中的PAT，拉曼光谱分析仪实时提供多个反应过程参数的原位测量，和微通道反应器结合使用，可以实现过程数据的快速获取，并为过程决策提供数据支撑。避免常规检测的滞后性造成反应的失控。

用于过程分析的原位在线拉曼光谱仪

在本文所描述的研究中，耶拿的Rxn系列拉曼分析仪用于在实验室/工艺开发（左）或生产（右）环境中在微通道反应器上实现的有机合成过程收集拉曼光谱。

探头种类多样、探头插入方式灵活多样

有机合成过程

反应原理

放热氧化硝化过程，传质传热不理想，监控数据滞后，会导致反应失控。

在线拉曼采样探头和反应器的结合

原位在线拉曼光谱仪和微通道反应器的结合

原位在线拉曼光谱仪监测微通道反应过程

微通道反应器的使用，在放热氧化硝化步骤中具有出色的传热、混合和停留时间控制；

通过原位在线拉曼光谱监测，在工艺开发早期可进行动力学、机理等分析，同时可在微通道反应器各模块类型、组合方式等筛选过程及后期的反应控制中发挥作用。

。

3

结论

1.原位在线拉曼光谱分析仪在化工和制药的工艺开发及放大生产过程中都表现出高度的功能和灵活性。

2.原位在线拉曼光谱分析仪和微通道反应器等连续流设备的结合，可高效、快速、稳定的提供实时监测数据，无论是在连续流反应工艺开发过程，更或者是在实际的生产过程，都可以发挥积极的作用。

3.在微通道及其他连续流反应器实施的化工及制药工艺中，原位在线拉曼光谱可以为动力学研究、机理剖析、过程实时监控等提供数据保证，是数据驱动控制的基础和保障。?

参考文献

David Ford, “Development of a continuous oxidative nitration reaction of a nitroalkane”, Kaiser Webinar.

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[8]未定义数组索引: page
[8]未定义数组下标: 0
[2]Declaration of app\common\model\News::getAllList($filter = Array, $limit = 16, $order = Array, $with = Array) should be compatible with app\common\model\BaseModel::getAllList($filter = Array, $with = Array, $limit = 0, $sort = Array, $field = 'a.*', $join = Array)
[2]Declaration of app\common\model\Company::getAllList($filter = Array, $limit = 20) should be compatible with app\common\model\BaseModel::getAllList($filter = Array, $with = Array, $limit = 0, $sort = Array, $field = 'a.*', $join = Array)
[8]未定义数组索引: center
[8]Only variables should be passed by reference
[2]Declaration of app\common\model\NewsComment::getAllList($filter = Array, $limit = 16) should be compatible with app\common\model\BaseModel::getAllList($filter = Array, $with = Array, $limit = 0, $sort = Array, $field = 'a.*', $join = Array)
[8192]Function create_function() is deprecated
[8192]Function create_function() is deprecated
[8]未定义数组索引: area
[8]未定义数组索引: st
[2]Declaration of app\common\model\Topic::getList($filter = Array) should be compatible with app\common\model\BaseModel::getList($filter = Array, $sort = Array)
[2]Declaration of app\common\model\Topic::getAllList($filter = Array, $field = 'id,md5,tit...', $limit = 0) should be compatible with app\common\model\BaseModel::getAllList($filter = Array, $with = Array, $limit = 0, $sort = Array, $field = 'a.*', $join = Array)
[2]Declaration of app\common\model\TopicInfoList::getAllList($filter = Array, $limit = 8) should be compatible with app\common\model\BaseModel::getAllList($filter = Array, $with = Array, $limit = 0, $sort = Array, $field = 'a.*', $join = Array)
[8]未定义数组索引: center
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[8]未定义数组索引: goods_list
[8]未定义数组下标: 0
[8]未定义数组索引: center
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[8]未定义数组索引: wtt_list

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[ SQL ] SELECT * FROM `news_category` WHERE `id` IN (7) [ RunTime:0.000181s ]
[ SQL ] SHOW COLUMNS FROM `user_follow` [ RunTime:0.000874s ]
[ SQL ] SELECT `id` FROM `user_follow` WHERE `user_id` IS NULL AND `follow_user_id` = 189 LIMIT 1 [ RunTime:0.000198s ]
[ SQL ] SHOW COLUMNS FROM `news_comment` [ RunTime:0.000822s ]
[ SQL ] SELECT * FROM `news_comment` WHERE `news_id` = 2420 AND `parent_id` = 0 ORDER BY `id` DESC [ RunTime:0.000227s ]
[ SQL ] SELECT COUNT(*) AS tp_count FROM `news_comment` WHERE `news_id` = 2420 LIMIT 1 [ RunTime:0.000159s ]
[ SQL ] SELECT * FROM `news` WHERE `is_show` = 1 AND `review_status` = 1 AND `id` IN (2420,1930,1246,4559,4059,3322,3306,7268,2598,5902) ORDER BY field(id,2420,1930,1246,4559,4059,3322,3306,7268,2598,5902) [ RunTime:0.000429s ]
[ SQL ] SELECT * FROM `user_info` WHERE `user_id` IN (189,309,777,785,333,226) [ RunTime:0.000693s ]
[ SQL ] SHOW COLUMNS FROM `topic` [ RunTime:0.000977s ]
[ SQL ] SELECT `id`,`md5`,`title`,`created_time` FROM `topic` WHERE `review_status` = 1 ORDER BY `id` DESC LIMIT 4 [ RunTime:0.000168s ]
[ SQL ] SHOW COLUMNS FROM `topic_info_list` [ RunTime:0.000793s ]
[ SQL ] SELECT * FROM `topic_info_list` WHERE `topic_id` = 1 ORDER BY `id` DESC LIMIT 2 [ RunTime:0.000178s ]
[ SQL ] SELECT * FROM `news` WHERE `id` IN (864,849) [ RunTime:0.000212s ]
[ SQL ] SELECT `id`,`md5`,`title`,`created_time` FROM `news` WHERE `review_status` = 1 AND `is_show` = 1 ORDER BY `id` DESC LIMIT 10 [ RunTime:0.000163s ]
[ SQL ] SHOW COLUMNS FROM `user` [ RunTime:0.000781s ]
[ SQL ] SELECT `a`.* FROM `user` `a` INNER JOIN `news` `b` ON `a`.`id`=`b`.`user_id` GROUP BY `a`.`id` ORDER BY `b`.`id` DESC LIMIT 10 [ RunTime:0.009499s ]
[ SQL ] SELECT * FROM `user_info` WHERE `user_id` IN (351,466,458,209,372,521,819,385,657,412) [ RunTime:0.000703s ]
[ SQL ] SHOW COLUMNS FROM `seo` [ RunTime:0.000826s ]
[ SQL ] SELECT * FROM `seo` WHERE `column_type` = '02' AND `page_type` = 'news' AND `info_id` = 2420 LIMIT 1 [ RunTime:0.000171s ]
[ SQL ] SELECT * FROM `news_belong_category` WHERE `news_id` = 2420 [ RunTime:0.001750s ]
[ SQL ] SELECT * FROM `news_belong_category` WHERE `news_id` = 1930 [ RunTime:0.001772s ]
[ SQL ] SELECT * FROM `news_belong_category` WHERE `news_id` = 1246 [ RunTime:0.001679s ]
[ SQL ] SELECT * FROM `news_belong_category` WHERE `news_id` = 4559 [ RunTime:0.001871s ]
[ SQL ] SELECT * FROM `news_belong_category` WHERE `news_id` = 4059 [ RunTime:0.001976s ]
[ SQL ] SELECT * FROM `news_belong_category` WHERE `news_id` = 3322 [ RunTime:0.001771s ]
[ SQL ] SELECT * FROM `news_belong_category` WHERE `news_id` = 3306 [ RunTime:0.002150s ]
[ SQL ] SELECT * FROM `news_belong_category` WHERE `news_id` = 7268 [ RunTime:0.001882s ]
[ SQL ] SELECT * FROM `news_belong_category` WHERE `news_id` = 2598 [ RunTime:0.001627s ]
[ SQL ] SELECT * FROM `news_belong_category` WHERE `news_id` = 5902 [ RunTime:0.001648s ]
[ SQL ] SELECT * FROM `user` WHERE `id` = 189 LIMIT 1 [ RunTime:0.000165s ]
[ SQL ] SELECT COUNT(*) AS tp_count FROM `user_follow` WHERE `follow_user_id` = 351 LIMIT 1 [ RunTime:0.000263s ]
[ SQL ] SELECT COUNT(*) AS tp_count FROM `user_follow` WHERE `user_id` = 351 LIMIT 1 [ RunTime:0.000143s ]
[ SQL ] SELECT COUNT(*) AS tp_count FROM `user_follow` WHERE `follow_user_id` = 466 LIMIT 1 [ RunTime:0.000149s ]
[ SQL ] SELECT COUNT(*) AS tp_count FROM `user_follow` WHERE `user_id` = 466 LIMIT 1 [ RunTime:0.000153s ]
[ SQL ] SELECT COUNT(*) AS tp_count FROM `user_follow` WHERE `follow_user_id` = 458 LIMIT 1 [ RunTime:0.000172s ]
[ SQL ] SELECT COUNT(*) AS tp_count FROM `user_follow` WHERE `user_id` = 458 LIMIT 1 [ RunTime:0.000144s ]
[ SQL ] SELECT COUNT(*) AS tp_count FROM `user_follow` WHERE `follow_user_id` = 209 LIMIT 1 [ RunTime:0.000165s ]
[ SQL ] SELECT COUNT(*) AS tp_count FROM `user_follow` WHERE `user_id` = 209 LIMIT 1 [ RunTime:0.000135s ]
[ SQL ] SELECT COUNT(*) AS tp_count FROM `user_follow` WHERE `follow_user_id` = 372 LIMIT 1 [ RunTime:0.000169s ]
[ SQL ] SELECT COUNT(*) AS tp_count FROM `user_follow` WHERE `user_id` = 372 LIMIT 1 [ RunTime:0.000137s ]
[ SQL ] SELECT COUNT(*) AS tp_count FROM `user_follow` WHERE `follow_user_id` = 521 LIMIT 1 [ RunTime:0.000137s ]
[ SQL ] SELECT COUNT(*) AS tp_count FROM `user_follow` WHERE `user_id` = 521 LIMIT 1 [ RunTime:0.000153s ]
[ SQL ] SELECT COUNT(*) AS tp_count FROM `user_follow` WHERE `follow_user_id` = 819 LIMIT 1 [ RunTime:0.000131s ]
[ SQL ] SELECT COUNT(*) AS tp_count FROM `user_follow` WHERE `user_id` = 819 LIMIT 1 [ RunTime:0.000152s ]
[ SQL ] SELECT COUNT(*) AS tp_count FROM `user_follow` WHERE `follow_user_id` = 385 LIMIT 1 [ RunTime:0.000150s ]
[ SQL ] SELECT COUNT(*) AS tp_count FROM `user_follow` WHERE `user_id` = 385 LIMIT 1 [ RunTime:0.000138s ]
[ SQL ] SELECT COUNT(*) AS tp_count FROM `user_follow` WHERE `follow_user_id` = 657 LIMIT 1 [ RunTime:0.000137s ]
[ SQL ] SELECT COUNT(*) AS tp_count FROM `user_follow` WHERE `user_id` = 657 LIMIT 1 [ RunTime:0.000126s ]
[ SQL ] SELECT COUNT(*) AS tp_count FROM `user_follow` WHERE `follow_user_id` = 412 LIMIT 1 [ RunTime:0.000205s ]
[ SQL ] SELECT COUNT(*) AS tp_count FROM `user_follow` WHERE `user_id` = 412 LIMIT 1 [ RunTime:0.000150s ]

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