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低热固相合成手性及非手性碱金属磷酸锌盐及其催化性能的研究

Synthesis of Chiral and Achiral Alkali Zincophosphate Salts by Solid Phase Reaction at Low-Heating Temperature and Study of Its Catalysis

【作者】 孙雅博

【导师】 廖森;

【作者基本信息】 广西大学 , 应用化学, 2006, 硕士

【摘要】 第一章:以七水合硫酸锌与十二水合磷酸钠为原料,聚乙二醇-400为模板剂,首次用低热固相反应合成得到了手性磷酸锌钠晶体。实验结果表明:(1)以七水硫酸锌和十二水合磷酸钠为原料,PEG-400为模板剂,用室温固相反应法合成首次得到手性磷酸锌钠晶体。(2)本法合成手性磷酸锌钠晶体,在研磨20min,60℃保温后就能得到比较完好的晶体,如果静置时间过长反而会增加杂质的生成。(3)用不同的锌盐和钠盐反应得到不同的产物,经分析得知是混合物的酸碱性不同所致,所以混合物的pH值是影响产物的重要因素。(4)在反应物中加入甘氨酸、L—谷氨酸、L—精氨酸,氨基酸结构不同影响产物的结构。(5)温度对手性结构的形成起着调控作用,60℃保温得到的是手性的产物,而室温保温得到的则是非手性的产物。(6)产物磷酸锌钠具有手性又具有微孔结构,在催化方面有一定的应用前景。 第二章:手性磷酸锌钠催化芳香醛与氰乙酸乙酯的Knoevenagel缩合反应,反应产率较高。实验结果表明:(1)通过对缩合产物的红外谱图的分析表明,产物中含有碳碳双键、CN叁键、酯基,苯环的存在,基本上符合缩合产物的结构特征。(2)用气质联用仪分析缩合产物,证明产

【Abstract】 Chapter One: The crystals of chiral sodium zincophosphate were synthesized via solid state reaction at low-heating temperature, when ZnSO4·7H2O reacts with Na3PO4·12H2O using PEG-400 as template. The experimental results showed that (1) Chiral sodium zincophosphate was synthesized via solid state reaction at low-heating temperature for the first time, when ZnSO4·7H2O reacted with Na3PO4·12H2O using PEG-400 as template. The products were characterized by XRD which indicated that the product was NaZnPO4H2O. (2) The products of chiral sodium zincophosphate had spontaneously crystallized to form ideal crystals within 20 minutes grinding time and warming at 60℃. On the contrary, the byproduct would be formed by long deposited time. (3)The products were synthesized by different phosphates and different zinc salts, pH value played key role in controlling composition of the products. (4) Adding glycine L—glutamate L—arginine, amino acid structure effected products structure. (5)Temperature played a key role in controlling the chiral structure. The products were chiral when the aged temperature was 60℃, and the products were achiral when the aged temperature was room temperature. (6)NaZnPO4·H2O with chiral and microporous structure has an ideal perspective catalysis.

  • 【网络出版投稿人】 广西大学
  • 【网络出版年期】2006年 12期
  • 【分类号】O643.32
  • 【下载频次】193
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