超空心纳米非晶态硼酸锌阻燃剂的制备

Preparation of nano-zinc borate with ultra-hollow spheres as flame retardant

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（x ZnO · yB2O3· zH2O）was prepared from the reaction of ZnC12 by atcoholysis （95M, ethanol）and the saturated solution of borax （Na2B407 · 10 H2O） under the conditions that polyvinyl alcohol （saturated so- lution in 50℃ ） as emulsifier. Using of orthogonal test, the effect of products studied in different the temperature, stirring speed,the consumption of polyvinyl alcohol and alcohol, the proportion of raw material. The optimum conditions of syn- thetic zinc borate was observed as Group 5.-the stirring speed was 1200r/min, the temperature was 30℃, the consumption of ethanol was 120mL, the consumption of PVA was 3mL, the ratio of raw material was 3 ： 1. And the respective content of zinc oxide and boron oxide was measured by using chemical titration, crystal-water content of the synthesis was produc- ted by the use of heating method. It was studied by the X-ray and TEM, it showed that synthetic products was hollow spherical particles and attached together to certain structure, more of them was uniform size, 80% of the particles are con- centrated from 30 nm to 50nm.