双指标参数响应面优化制备多金属磷钼酸复盐

袁爱群, 陈心怡, 黄云龙, 黄增尉, 吴胜富, 韦冬萍

现代化工 ›› 2020, Vol. 40 ›› Issue (10) : 131 -136.

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现代化工 ›› 2020, Vol. 40 ›› Issue (10) : 131-136. DOI: 10.16606/j.cnki.issn0253-4320.2020.10.027
科研与开发

双指标参数响应面优化制备多金属磷钼酸复盐

    袁爱群, 陈心怡, 黄云龙, 黄增尉, 吴胜富, 韦冬萍
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Optimization of polymetallic phosphomolybdate compound salts preparation by double-indicator response surface

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摘要

采用共沉淀法制备多金属磷钼酸复盐,考察了PO43-/MoO42-摩尔比、Fe3+/Zn2+摩尔比、反应pH、反应温度、反应时间对产物中磷酸根、钼酸根质量分数的影响。以磷酸根质量分数、钼酸根质量分数双指标参数为响应值,采用中心复合设计响应面优化制备工艺条件,并利用SEM、XRD、TEM对产物进行表征,通过盐雾试验测定其防锈性能。结果表明,当磷酸根与钼酸根摩尔比为5:1时,4个因素影响顺序为:铁锌离子摩尔比 > 反应pH > 反应温度 > 反应时间。在铁锌离子摩尔比为0.98:1、pH=5.5、温度为78℃、时间为79 min的最佳条件下,磷酸根与钼酸根质量分数分别可达到34.79%和5.15%。盐雾试验结果表明,其耐盐雾时间与红丹接近,优于进口同类产品及市售磷酸锌。

Abstract

Zinc-iron phosphomolybdate composite material is prepared by co-precipitation method.The effects of PO43-/MoO42- molar ratio,Fe3+/Zn2+ molar ratio,reaction pH value,as well as reaction temperature and reaction time on the contents of phosphate and molybdate radicals in the product are investigated.Taking the contents of phosphate and molybdate radicals as the double-indicator response values,reaction conditions are optimized by the central composite design response surface.Product samples are characterized by SEM,XRD and FT-IR,and their anti-rust properties are detected through salt spray test.The results show that as the mole ratio of phosphate to molybdate is 5:1,the molar ratio of iron to zinc ions has the biggest effect,followed by reaction pH value,reaction temperature and reaction time in turn.The optimal conditions are as follows:the mole ratio of iron ion to zinc ion is 0.98:1,pH is 5.5,the temperature maintains at 78℃ and the time is 79 min.Under these optimal conditions,the contents of phosphate and molybdate radicals can reach 34.79% and 5.15%,respectively.Salt spray test verifies that the salt spray resistance time of the composite materials is close to that of red lead,and longer than that of similar imported products and commercial zinc phosphate.

关键词

磷钼酸复盐 / 防锈颜料 / 磷酸盐

Key words

phosphomolybdate compound salt / antirust pigment / phosphates

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双指标参数响应面优化制备多金属磷钼酸复盐[J]. 现代化工, 2020, 40(10): 131-136 DOI:10.16606/j.cnki.issn0253-4320.2020.10.027

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