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通过ZnCl2的醇解(95%的乙醇),在聚乙烯醇(50℃的饱和溶液)作为乳化剂的条件下,与饱和的硼砂(N a2B4O7.10H2O)溶液发生反应,生成硼酸锌ZB(x ZnO.yB2O3.zH2O)。采用正交实验法研究了温度、搅拌速度、聚乙烯醇的用量、乙醇的用量及配比对合成产品的影响。找出合成硼酸锌的最佳工艺条件是乙醇的用量为120mL,聚乙烯醇的用量3mL,原料配比为3∶1,搅拌速度为1200 r/min,温度为30℃。采用化学滴定法测出其中ZnO和B2O3的质量分数,加热失重的方法得到结晶水的含量,对合成的产品进行X-衍射、TEM等表征,表明合成的产品为类球型空心颗粒及链状颗粒,粒度分布比较均匀,80%左右的颗粒都集中分布在30~50nm。
The zinc borate (N a2B4O7.10H2O) solution was reacted by alcoholysis of ZnCl2 (95% ethanol) in the presence of polyvinyl alcohol (saturated solution at 50 ℃) as an emulsifier to produce zinc borate ZB (x ZnO.yB2O3.zH2O). The effects of temperature, stirring speed, the amount of polyvinyl alcohol, the amount of ethanol and the proportion of the synthesized product were studied by orthogonal experiment. The optimum technological conditions for the synthesis of zinc borate were 120 mL of ethanol, 3 mL of polyvinyl alcohol, 3: 1 ratio of raw materials, stirring speed of 1200 r / min and temperature of 30 ℃. The chemical components of ZnO and B2O3 were determined by chemical titration method, and the content of water of crystallization was obtained by weight loss method. The synthesized products were characterized by X-ray diffraction (XRD) and transmission electron microscopy (TEM). The results showed that the synthesized products were spheroidal hollow particles and chains Particles, particle size distribution is more uniform, about 80% of the particles are concentrated in 30 ~ 50nm.