| 第 52 卷第 3 期 |  | Vol. 52 No. 3 | | 2022 年 6 月 | Jun 2022 |
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所屬欄目：農藥及中間體
微通道反應器在唑草酮硝化反應中的應用 |
| 李金平，丁小兵
（江蘇蘇化集團技術(shù)中心，江蘇 蘇州 215007） |
| 摘 要：應用微通道反應器對唑草酮中間體連續硝化工藝進(jìn)行研究，包括反應器的選型、空速比、硝酸與底物1-（4-氯-2-氟苯基）-3-甲基-4-二氟甲基-1H-1，2，4-三唑啉-5-酮的配比、硫酸的濃度與套用、反應溫度梯度控制等工藝條件的優(yōu)化。結果表明，使用特種合金微反應器，在n（底物）∶n（硝酸）∶n（85%硫酸）=1.0∶1.1∶6.6、空速比為60 h-1、一級反應器控溫（35±2） ℃、二級反應器控溫（45±2） ℃條件下，底物硝化轉化率≥99%，產(chǎn)品收率≥95%，并實(shí)現了工藝連續化。相對于釜式間歇反應，具有收率高、反應通量大、更安全高效的特點(diǎn)。 |
| 關(guān)鍵詞：微通道反應器；唑草酮；硝化反應；空速比 |
| 中圖分類(lèi)號：TQ457 文獻標識碼：A 文章編號：1009-9212（2022）03-0016-04 |
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| Application of Microchannel Reactor in the Nitration Reaction of Carfentrazone-ethyl Intermediate |
| LI Jin-ping, DING Xiao-bing
(Jiangsu Chemical Group Technology Center, Suzhou 215007, China) |
| Abstract：A process for continuous nitration of Carfentrazone-ethyl intermediate using microchannel reactors was systematically studied. Factors including type of microchannel reactors, space velocity ratio, molar ratio of nitric acid and substrates [1-(4-chloro-2-fluorophenyl)-3-methyl-4-(difluoromethyl)-1H-1,2,4-triazol-5-one], concentration and recycle of sulfuric acid, reaction temperature gradient control and other process were evaluated; The optimal condition were as followings: n(substrate)∶n(nitric acid)∶n(85% sulfuric acid)=1.0∶1.1∶6.6; the space velocity ratio was 60ｈ-1 using microreactors (special alloy); the control temperature of the first reactor was of (35±2) ℃; and the temperature of the second reactor was of (45±2) ℃; Under optimal conditions, the nitration conversion rate of the substrate was ≥99%; a total yield was of ≥95%. Compared with the batch reaction, it has the advantages including higher yield, higher reaction throughput, safer and faster. |
| Key words：microchannel reactor; Carfentrazone-ethyl; nitration reaction; space velocity ratio |
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作者簡(jiǎn)介：李金平（1968－），男，江西新余人，高級工程師，研究方向：農藥、有機合成、微反應器化學(xué)應用研究（E-mail：ljp@jsgc.com）。
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收稿日期：2021-12-10
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