丁基黄原酸丙腈脂分子结构的研究

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我所近年来研究的一种新型捕收剂,S—氰乙基O—丁基黄原酸酯,又称丁基黄原酸丙腈酯或OSN—43。由于作为硫化矿捕收剂有用量少,成本低,选择性不浮硫或少浮硫等优点,在国内已推广使用。虽然,七十年代国外曾有对黄原酸烷基酯(08—系列)的气相,液相色谱分析报告,但对黄原酸丙腈酯的物理性质,化学结构以及分析方法的研究介绍甚我所近年来研究的一种新型捕收剂,S—氰乙基O—丁基黄原酸酯,又称丁基黄原酸丙腈酯或OSN—43。由于作为硫化矿捕收剂有用量少,成本低,选择性不浮硫或少浮硫等优点,在国内已推广使用。虽然,七十年代国外曾有对黄原酸烷基酯(08—系列)的气相,液相色谱分析报告,但对黄原酸丙腈酯的物理性质,化学结构以及分析方法的研究介绍甚少。红外、紫外,核磁共振光谱标准及商业图谱至今尚未见到。为了进一步弄清其结构与性质的关系,我们对不同方法制得的产品进行了研究,作了红外光谱、紫外光谱、核磁共振光谱分析。本文着重介绍对该药剂分子结构的解析鉴定工作。一、丁基黄原酸丙腈酯分子结构的研究 <1>二步法合成工艺的简述: (a)丁基黄药的制备: 醇:氢氧化钠和二硫化碳三者发生化学作用,生成黄药。反应可示如下: 反应属于放热反应,通常要在冷却下进行,产品为浅黄色粉状物,合成产品的品位在83%~85%之间,实收率为95.5%。 (b)丁基黄原酸丙腈酯的制备: 丁黄原酸丙腈酯,是通过丁基黄药与丙烯腈或β—卤代丙腈反应制得的,反应如下: NaOH+HCl→NaCl+H_2O 反应温度为35℃~40℃,反应可在水相或有机相中进行。为了促进反应进行,可加入适量的盐酸,中和反应中生成的NaOH,以使反应向生成物方向进行。粗产物为黄色 In recent years I studied a new collector, S-cyanoethyl O-butyl xanthate, also known as butyl xanthogenate or OSN-43. As sulfide ore collector less useful, low cost, selective non-sulfur or less floating sulfur, etc., has been promoted in China. Although gas and liquid chromatographic analysis of alkyl xanthogenate (08-series) has been reported abroad in the 1970s, the study on the physical properties, chemical structures and analytical methods of xanthogen propionate In recent years I studied a new collector, S-cyanoethyl O-butyl xanthate, also known as butyl xanthogenate or OSN-43. As sulfide ore collector less useful, low cost, selective non-sulfur or less floating sulfur, etc., has been promoted in China. Although gas and liquid chromatographic analysis of alkyl xanthogenate (08-series) has been reported abroad in the 1970s, the study on the physical properties, chemical structures and analytical methods of xanthogen propionate less. Infrared, ultraviolet, nuclear magnetic resonance spectroscopy standards and commercial maps have not yet been seen. In order to further clarify the relationship between its structure and properties, we have studied the products made by different methods and made infrared spectroscopy, ultraviolet spectroscopy and nuclear magnetic resonance spectroscopy. This article focuses on the analytical identification of the molecular structure of the drug. A, butyl xanthogen propionitrile molecular structure of <1> two-step synthesis of a brief description: (a) butyl xanthate preparation: alcohol: sodium hydroxide and carbon disulfide three chemical interaction occurs Xanthate. The reaction can be shown as follows: The reaction is an exothermic reaction, usually carried out under cooling, the product is a light yellow powder, the grade of the synthetic product is between 83% and 85%, and the actual yield is 95.5%. (b) Preparation of Butylxanthogen Propionitrile: Butyroline propionate is prepared by the reaction of Butyl xanthate with acrylonitrile or β-halopropionitrile as follows: NaOH + HCl → NaCl + H_2O reaction temperature of 35 ℃ ~ 40 ℃, the reaction can be carried out in the aqueous or organic phase. In order to promote the progress of the reaction, an appropriate amount of hydrochloric acid may be added to neutralize the NaOH generated during the reaction so that the reaction proceeds toward the product. The crude product is yellow
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