| 3-硝基-4-羟基苯甲酸的制备研究 |
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| 引用本文： | 全保学,蒋文伟,杨琴. 3-硝基-4-羟基苯甲酸的制备研究[J]. 陕西化工, 2014, 0(2): 332-334 |
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| 作者姓名： | 全保学 蒋文伟 杨琴 |
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| 作者单位： | [1]四川大学化学工程学院,四川成都610065 [2]成都惠恩精细化工有限责任公司,四川成都610065 |
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| 摘 要： | 以3-硝基-4-氯苯甲酸为原料,经水解反应得到产品,最佳水解条件为：氢氧化钠/3-硝基-4-氯苯甲酸摩尔比为4.5,碱液质量分数为15％,水解温度为95℃,反应时间为10 h.在最佳水解条件基础上,考察了碱液的循环利用,提高了氢氧化钠的利用率.总收率大于91％,纯度大于99％ （HPLC）,经FTIR、1H NMR、13C NMR和MS分析,证实产品为3-硝基-4-羟基苯甲酸.
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| 关 键 词： | 3-硝基-4-羟基苯甲酸 3-硝基4-氯苯甲酸 水解 循环 |
Study on preparation of 3-nitro-4-hydroxyl benzoic acid |
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| QUAN Bao-xue,JIANG Wen-wei,YANG Qin. Study on preparation of 3-nitro-4-hydroxyl benzoic acid[J]. Applied Chemical Industry, 2014, 0(2): 332-334 |
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| Authors: | QUAN Bao-xue JIANG Wen-wei YANG Qin |
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| Affiliation: | 1. College of Chemical Engineering, Sichuan University, Chengdu 610065, China; 2. Chengdu Huien Fine Chemical Co. ,Ltd. ,Chengdu 610065 ,China) |
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| Abstract: | 3-Nitro-4-hydroxybenzoic acid was synthesized from 3-nitro-4-chlorobenzoic acid through hydro- lyzation in sodium hydroxide solution. Best result was obtained under conditions of reaction temperature of 95 ℃, molar ratio of sodium hydroxide to 3-nitro-4-chlorobenzoic acid of 4.5, mass concentration of sodium hydroxide of 15% ,reaction time of 10 h. Based on the optimized process, the recycle of sodium hydroxide was studied. High yield （ 〉 91% ） ,high purity （ 〉 99% HPLC was achieved. The structure of the title compound was confirmed by 1H NMR,13C NMR,FTIR and MS. |
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| Keywords: | 3-nitro-4-hydroxyl benzoic acid 3-nitro-4-chloro benzoic acid hydrolyzation recycle |
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