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作 者:李欣阳 王海增[1] LI Xin-yang;WANG Hai-zeng(College of Chemistry and Chemical Engineering,Ocean University of China,Qingdao 266100,China)
机构地区:[1]中国海洋大学化学化工学院,山东青岛266100
出 处:《现代化工》2024年第2期184-190,共7页Modern Chemical Industry
基 金:中央高校基本科研业务费专项(201964021);山东省海洋精细化工重点实验室开放基金项目(2020301)。
摘 要:为了开拓镁资源高值化开发的新路径,以六水氯化镁为镁源,分别与D,L-酒石酸、D-酒石酸、L-酒石酸反应,在温和的条件下一步合成了3种酒石酸镁[Mg(D,L-tart)(H_(2)O)_(2)·3H_(2)O(Ⅰ)、Mg(D-tart)(H_(2)O)·1.5H_(2)O(Ⅱ)、Mg(D-tart)(Ⅲ)]。结果表明,在常温水溶液体系中合成了产品Mg(D,L-tart)(H_(2)O)_(2)·3H_(2)O(Ⅰ),最佳合成条件为反应温度-5℃、pH 8.00且体系中乙醇体积分数达到0.36时反应1 h;通过水-乙醇混合溶剂合成了产品Mg(D-tart)(H_(2)O)·1.5H_(2)O(Ⅱ),最佳反应条件为反应温度60℃、pH为6.00~7.00且体系内乙醇体积分数达到0.46时反应24 h;分别在温和的水热条件下或水-DMAC混合溶剂体系中合成无结晶水的产品Mg(D-tart)(Ⅲ),当DMAC体积分数达到0.55时产物Mg(D-tart)(Ⅲ)达到最佳产率超过94%。同时考察了合成条件对产物晶体形貌及收率的影响。Focusing on the high-value development of magnesium resources,magnesium chloride hexahydrate is used as magnesium source to react with D,L-tartaric acid,D-tartaric acid,and L-tartaric acid,respectively,to synthesize Mg(D,L-tart)(H_(2)O)_(2)·3H_(2)O(Product I),Mg(D-tart)(H_(2)O)·1.5H_(2)O(ProductⅡ),and Mg(D-tart)(ProductⅢ)under mild conditions.In the normal temperature aqueous solution system,the product I is synthesized,and the best synthesis conditions for Product I are as follows:reaction temperature is-5℃,pH=8.00,the ethanol volume fraction in the system reaches 0.36,and the reaction lasts for 1 h.ProductⅡis obtained by using water-ethanol mixing as solvent,and the best reaction conditions are as follows:reaction temperature is 60℃,pH=6.00-7.00,the ethanol volume fraction in the system is 0.46,and the reaction lasts for 24 hours.ProductⅢcan be prepared under mild hydrothermal conditions or water-DMAC mixed solvent system.The best yield of ProductⅢreaches over 94%when the volume concentration of DMAC is 0.55.The influences of the synthesis conditions on the crystal morphology and yield of the products are also investigated.
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