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以溴酸根插层锌铝水滑石(Zn/Al-Br O3–-LDHs)为载体,与Br-等还原剂构建形成新型溴源体系。为实现溴源体系在实际应用中的有效控溴,对Zn/Al-Br O3–-LDHs中Br O3–的释放行为进行了研究,并考察了温度、交换离子类型、p H值等因素对Br O3–释放行为的影响。结果表明:升高温度会加快Br O3–的释放,交换离子的交换性越强,Br O3–释放得越快,在p H值为9.0的磷酸盐缓冲溶液中的释放速率要比在p H值为4.0的磷酸盐缓冲溶液中快。采用4种动力学模型对水滑石中Br O3–的释放过程进行动力学拟合,结果表明:LDHs-Br O3–中Br O3–的释放行为符合Bhaskar方程,属粒内扩散控制过程。用LDHs-Br O3–/Br–构建的溴源体系合成了3,5-二溴-2-氨基苯甲酸甲酯,收率为94.7%,纯度为99.8%。
Brominated intercalated zinc - aluminum hydrotalcite (Zn / Al - Br O3 - LDHs) as carrier, and Br - and other reducing agents to form a new bromine source system. In order to achieve effective bromine control in practical application of bromine source system, the release behavior of Br O3- in Zn / Al-Br O3 - LDHs was studied, and the effects of temperature, exchange ion type and p H value on Br O3-release behavior. The results showed that the higher the temperature, the faster the Br O3- release. The higher the exchangeability of the exchangeable ions, the faster the release of Br O3-. The release rate in the phosphate buffer solution with p H value 9.0 was higher than that in p H Value of 4.0 in phosphate buffer solution fast. Four kinetic models were used to fit the kinetics of Br O3- release in hydrotalcite. The results show that the release of Br O3- in LDHs-Br O3- accords with the Bhaskar equation and is controlled by intragranular diffusion. Methyl 3,5-dibromo-2-aminobenzoate was synthesized by bromine source system constructed with LDHs-Br O3- / Br-. The yield and purity of methyl 3,5-dibromo-2-aminobenzoate were 94.7% and 99.8% respectively.