化学蚀刻废磷酸制备饲料级磷酸脲的研究
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摘要
研究了以化学蚀刻废磷酸和工业尿素为原料合成磷酸脲的工艺。考察了n(尿素)/n(磷)、反应时间、温度、搅拌速率对产率的影响,借助于X射线衍射仪对所制备产品进行表征,并采用农业行业标准NY/T 917—2004《饲料级磷酸脲》的检测标准对最终产品进行检测。结果表明,制备高纯度的饲料级磷酸脲的优化反应条件为:n(尿素)/n(磷)=1.0、搅拌速率为300 r/min、反应温度为60℃、反应时间为60 min、结晶温度为25℃、冷却结晶时间为4 h。在此条件下,磷酸回收率为68.71%,磷酸脲产品达到饲料级磷酸脲的标准。
The synthesis of urea phosphate with waste phosphoric acid from chemical etching and industrial urea as raw materials was studied.Effects of the amount of substance ratio of urea to P,reaction time,reaction temperature and mixing speed on product yield were investigated respectively.The resultant products were characterized by X-ray diffraction and tested according to the agricultural industry standard of Feed Grade Urea Phosphate,NY/T 917—2004.Results showed that high purity of feed-grade urea phosphate was obtained at the optimum preparation conditions as n(urea)/n(P) =1.0,stirring speed of300 r/min,reaction temperature of 60 ℃,reaction time of 60 min,crystallization temperature of 25 ℃ and cooling crystallization for 4 h.Under these conditions,the recovery of phosphate acid was 68.71%,and the products of urea phosphate met the requirement of feed-grade standard.
The synthesis of urea phosphate with waste phosphoric acid from chemical etching and industrial urea as raw materials was studied.Effects of the amount of substance ratio of urea to P,reaction time,reaction temperature and mixing speed on product yield were investigated respectively.The resultant products were characterized by X-ray diffraction and tested according to the agricultural industry standard of Feed Grade Urea Phosphate,NY/T 917—2004.Results showed that high purity of feed-grade urea phosphate was obtained at the optimum preparation conditions as n(urea)/n(P) =1.0,stirring speed of300 r/min,reaction temperature of 60 ℃,reaction time of 60 min,crystallization temperature of 25 ℃ and cooling crystallization for 4 h.Under these conditions,the recovery of phosphate acid was 68.71%,and the products of urea phosphate met the requirement of feed-grade standard.
引文
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[2]冯卫文.一种回收废铝蚀刻液中磷酸的方法:中国,103979509[P].2014-08-13.
[3]芝田隼次,山本秀树,井上兴一郎,等.从醋酸-硝酸-磷酸系混酸废液中分离回收磷酸的方法:中国,200510113482.2[P].2011-01-12.
[4]井上兴一郎,内野雄贵,小津毅.从乙酸-硝酸-磷酸系混酸废液中分离回收磷酸的方法:中国,201010126214.5[P].2015-04-01.
[5]李雯,吴文彪,李姗婷,等.光电行业废磷酸蚀刻液萃取除杂实验研究[J].广东化工,2016,43(17):157-159,169.
[6]陈志传,宋少华,毛谙章,等.化学抛光废磷酸的综合利用方法:中国,200810241481.X[P].2009-06-17.
[7]王卫红,武建刚,陈志传,等.利用磷酸-硝酸-醋酸废液制备肥料级磷酸铵浓缩液的方法:中国,201210356613.X[P].2012-12-19.
[8]吴文彪,张艳华,徐文彬,等.利用TFT-LCD磷酸蚀刻废液制备饲料级磷酸氢钙[J].广东化工,2017,44(18):66-68,23.
[9]周兆安,唐瑜钟,徐丽阳,等.回收利用含磷酸性废液制备三聚氰胺聚磷酸盐的方法:中国,201710391347.7[P].2017-09-22.
[10]慎义勇,周兆安,唐瑜钟,等.废化学抛光剂中含磷化合物的回收方法:中国,201710392425.5[P].2017-09-15.
[11]陈嘉甫,谭光薰.磷酸盐的生产与应用[M].成都:成都科技大学出版社,1989:354-359.
[12]杨帆,解田,刘飞.激光法测定饲料级磷酸脲在水中的溶解度[J].无机盐工业,2016,48(4):69-71.
[13]刘安强,雷兴家.磷酸脲的合成及应用[J].湖北化工,1992(1):13-16.