烷基黄原酸酯系列药剂的合成与应用

【作者】 周继亮；

【导师】 钟宏；

【作者基本信息】 中南大学 ， 化学工艺， 2003， 硕士

【摘要】 传统硫化矿捕收剂黄药的捕收能力虽然较强，但是其选择性较低。因此有必要对其进行改性，研制出新型高效硫化矿捕收剂。 本文通过酯化反应对黄药进行了改性：选择能与黄原酸基团形成大共轭体系的氯代烃(氯甲酸乙酯、烯丙基氯、苄基氯)与烷基黄药在水溶液中反应，相应地合成了烷基黄原酸甲酸乙酯、烷基黄原酸烯丙酯及烷基黄原酸苄基酯三系列药剂。通过试验考察了反应温度、反应时间及物料摩尔比对烷基黄原酸酯产率的影响，优化了其合成工艺参数。试验结果表明异丙基黄原酸甲酸乙酯合成的最优工艺参数为反应温度25℃、反应时间4.0小时、物料摩尔比(异丙基黄药：氯甲酸乙酯)1.05：1.00；异丙基黄原酸烯丙酯合成的最优工艺参数为反应温度45℃、反应时间4.0小时、物料摩尔比(异丙基黄药：氯甲酸乙酯)1.05：1.00；而合成异丙基黄原酸苄基酯的最优工艺参数为反应温度55℃、反应时间6.0小时、物料摩尔比(异丙基黄药：氯甲酸乙酯)1.10：1.00。在最佳工艺条件下，异丙基黄原酸甲酸乙酯产率达到93.76％，异丙基黄原酸烯丙酯为85.51％，而异丙基黄原酸苄基酯产率达到91.86％。然后对合成产品进行了折光率、紫外光谱及红外光谱等物性分析，鉴定了其化学结构，表明所合成产物为目标产物。 通过对德兴硫化铜矿的浮选试验，研究了合成产品烷基黄原酸酯药剂的浮选性能。试验结果表明三系列烷基黄原酸酯产品浮选硫化铜矿石时，均表现出较强的捕收能力和优于丁基黄药的选择性能；在三系列烷基黄原酸酯药剂中又以烷基黄原酸苄基酯的选择性最好。当用丁基黄原酸苄基酯闭路浮选德兴铜矿硫化铜矿时，铜品位为6.95％，铜回收率为91.44％；与丁基黄药相比，其铜品位提高近2％，回收率提高将近1％，其浮选指标明显优于丁基黄药。作为一种新型高效硫化矿捕收剂，本论文所研制的烷基黄原酸苄基酯药剂具有工业应用前景。更多还原

【Abstract】 Though xanthate, the traditional sulfide ores collector, is effective in collecting ability, its selectivity is not good. Hence it is necessary to improve the structure of xanthate and develop new type of sulfide ores collectors of high flotation properties.In this paper the chlorinated hydrocarbon (ethyl chloroformate, allyl chloride, benzyl chloride) were chosen as raw materials to react with alkyl xanthate in the aqueous solution. Three series of alkyl xanthic esters (alkyl xanthogen ethyl formate, allyl esters of alkyl xanthate, benzyl esters of alkyl xanthate) were prepared. The effects of reaction temperature, reaction time and molar ratio of reactants on yield were studied. The experiment results showed that the optimum technical parameters for the synthesis of alkyl xanthogen ethyl formate are 25 ℃ (reaction temperature)., 4.0hr(reaction time) and 1.05:1.00(molar ratio of xanthate to ethyl chloroformate). The optimum technical parameters for the synthesis of allyl esters of alkyl xanthate are 45 ℃ (reaction temperature),4.0hr (reaction time) and 1.05:1.00 (molar ratio of xanthate to allyl chloride). And for the synthesis of benzyl esters of alkyl xanthate, the optimum technical parameters are 55 ℃ (reaction temperature. 6hr(reaction time) and 1.10:1.00(molar ratio of xanthate to benzyl chloride). In the optimum technical conditions, the yield of isopropyl xanthogen ethyl formate is 93.76 %. The yield of allyl esters of isopropyl xanthate in the optimum technical conditions is 85.51 %. And the yield of the benzyl esters of isopropyl xanthate in the optimum technical conditions is 91.86%. The analysis has been done of the products using some physical measures such as the refraction index, ultraviolet spectrum, infrared spectrum. The results showed that the synthesized products are the aimed products.Then the copper sulfides of Dexing were adopted for investigating the flotation properties of the synthesized products. The results showed that all the synthesized products have good collecting ability. And threeseries of alkyl xanthic esters, especially the series of benzyl esters of alkyl xanthate, are superior to butyl xanthate in selectivity. Using benzyl ester of butyl xanthate as collector in the closed flotation circuit of Dexing copper sulfides, We have acquired the ideal separation indexes which are superior to that of the butyl xanthate. The copper concentrate grade of the product is 6.95% (about two percent higher than that of the butyl xanthate) and the copper recovery of the product is 91.44% (about one percent higher than that of the butyl xanthate). As a new type of sulfide ores collectors of high flotation properties, the benzyl esters of alkyl xanthate are likely to be used successfully in the flotation industry.更多还原