第 51 卷第 5 期 |  | Vol. 51 No. 5 | 2021 年 10 月 | Oct 2021 |
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所屬欄目:功能材料
1,3-雙(2-噁唑啉基)苯的合成工藝優(yōu)化 |
張 浩,曾桂鈺,陶錫祺
(江西仰立新材料有限公司,江西 吉安 343000) |
摘 要:以間苯二甲腈、乙醇胺為原料,無(wú)水醋酸鋅或氯化鋅為催化劑,合成了1,3-雙(2-噁唑啉基)苯,優(yōu)化了工藝條件。優(yōu)化條件為:n(間苯二甲腈)∶n(乙醇胺)∶n(催化劑)=1.00∶4.00∶0.04,反應5 h,溫度120~125 ℃。優(yōu)化條件下,產(chǎn)品含量99.2%,反應收率94.7%,產(chǎn)品結構經(jīng)核磁、紅外和質(zhì)譜確證。該工藝還提出了乙醇胺的回收方法,具有收率高、成本低、三廢排放少等優(yōu)勢,宜于工業(yè)化生產(chǎn)。 |
關(guān)鍵詞:噁唑啉;間苯二甲腈;乙醇胺 |
中圖分類(lèi)號:TQ25 文獻標識碼:A 文章編號:1009-9212(2021)05-0078-03 |
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Process Optimization for the Preparation of 2,2'-(1,3-Phenylene) Bis-(2-oxazoline) |
ZHANG Hao, ZENG Gui-yu, TAO Xi-qi
(Jiangxi Univate New Material Co.,Ltd., Ji'an 343000, China) |
Abstract:2,2'-(1,3-Phenylene)bis-(2-oxazoline) was prepared from 1,3-dicyanobenzene and ethanolamine using Zn(OAc)2 or ZnCl2 as catalyst. Process conditions were optimized and obtained as followings: the ratio of n(1,3-Dicyanobenzene)∶n(ethanolamine)∶n(catalyst) was of 1.00∶4.00∶0.04; reacting time was of 5 h; the reaction temperature was at a range from 120 ℃ to 125 ℃. The yield and purity of the product were reached up to 94.7% and 99.2%, respectively. The objective product was confirmed by 1H NMR, 13C NMR, IR and MS. The recovery of ethanolamine was also presented. This process has the advantages including high yield, low cost, less waste water and facile industrialization. |
Key words:oxazoline; 1,3-dicyanobenzene; ethanolamine |
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作者簡(jiǎn)介:張 浩(1989—),男,安徽臨泉人,工程師,博士,主要從事精細化工的工藝研發(fā)工作(E-mail:hao_zhang@cacch.com)。
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收稿日期:2021-08-03
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