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        對稱性硫脲的綠色合成工藝
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        1. 河南省非輪胎類橡膠助劑工程技術研究中心,河南 鶴壁 458030;2. 河南易交聯新材料研究院有限公司,河南 鶴壁 458030

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        Green synthesis of symmetric thiourea compounds
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        1. Henan Engineering and Technology Research Center of Non-tire Rubber Auxiliaries, Hebi 458030, Henan, China;2. Henan Yijiaolian New Material Research Institute Co., Ltd., Hebi 458030, Henan, China

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          摘要:

          以乙二胺、CS 2 為原料、水為溶劑,一鍋合成了亞乙基硫脲(ETU),收率和 HPLC 純度均達到 99%以上。 利用 NMR、FTIR 對產物結構進行了確證??疾炝?CS 2 滴加溫度、乙二胺與 CS 2 物質的量比、回流反應溫度、 回流反應升溫速率及 NaOH 反應段 NaOH 用量對 ETU 收率、HPLC 純度的影響。結果表明,ETU 的最佳合成工 藝條件為 CS 2 滴加溫度 25~30 ℃、n(乙二胺)∶n(CS 2 )=1∶1.20、回流反應溫度 65~70 ℃、回流反應升溫速率 0.17 ℃/min、NaOH 反應段 NaOH 用量為乙二胺質量的 3.0%。以此工藝為模板,合成了 1,3-二乙基硫脲(DETU)和 四氫-2(1H)-嘧啶硫酮(PUR)。中試實驗表明,該工藝穩定可靠,產品收率、HPLC 純度均達到 99%以上,母液 可循環套用。

          Abstract:

          Ethylene thiourea (ETU), with both yield and HPLC purity over 99%, was synthesized with ethylenediamine and CS 2 as raw materials and water as solvent in one pot, and characterized by NMR and FTIR. The effects of CS 2 dropping temperature, molar ratio of ethylenediamine to CS 2 , reflux reaction temperature, reflux heating rate, and NaOH dosage in NaOH reaction section on the yield and purity of ETU were then investigated. The results showed that the optimum synthesis conditions were as follows: CS 2 dropping temperature of 25~30 ℃, n(ethylenediamine)∶n(CS 2 )=1∶1.20, reflux reaction temperature of 65~70 ℃, reflux heating rate of 0.17 ℃/min, and NaOH dosage in NaOH reaction section being 3.0% of the mass of ethylenediamine. 1,3-diethylthiourea (DETU) and tetrahydro-2(1H)-pyrimidine thioketone (PUR) were then synthesized under the optimized process conditions, and the pilot test indicated that the process was stable and reliable with the yield and HPLC purity of products obtained >99%, and the mother liquor could be recycled.

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        李合平,常帥軍,宋士杰,劉俊勇,蘇瓊.對稱性硫脲的綠色合成工藝[J].精細化工,2023,40(6):

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        • 收稿日期:2022-09-06
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        • 在線發布日期: 2023-06-28
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