湿法磷酸选择性除杂制工业级磷酸二氢铵
收稿日期: 2020-10-13
网络出版日期: 2021-04-23
基金资助
国家自然科学基金项目(21978153);云南省高校本科教育教学改革研究项目(JG2018198);曲靖师范学院教学成果奖培育项目(JPCGPY201801)
Fabrication of industrial grade ammonium dihydrogen phosphate via selective removal of impurities from wet-process phosphoric acid
Received date: 2020-10-13
Online published: 2021-04-23
王智娟 . 湿法磷酸选择性除杂制工业级磷酸二氢铵[J]. 无机盐工业, 2021 , 53(4) : 48 -51 . DOI: 10.11962/1006-4990.2020-0253
Ammonium dihydrogen phosphate with high purity can be used as water-soluble fertilizer, flame retardant, feed and food additives and recently it has been studied for preparation of phosphate optical glass, cathode materials for lithium batteries and nonlinear optical materials.Due to its broad application prospect in the fields of agriculture, fire protection, food and materials, the demand for high purity ammonium dihydrogen phosphate is increasing.High purity ammonium dihydrogen phosphate can be fabricated via thermal phosphoric acid and extraction-purified wet-process phosphoric acid route.The formerroute is simple and can get high quality of product, but it is restricted to the influence of resources, energy and environment.While the latter route is complex and needs large investment.Hence, more researchers focus on the direct preparing high purity ammonium dihydrogen phosphate with raw wet-process phosphoric acid.But the lower P2O5 yield of product(25%~40%)inhibited its development due to the formation of a large amount of phosphorus-containing precipitates(e.g., metallic phosphate) during ammoniation.Therefore, herein modified-process with sodium fluoride was used to selectively precipitate metalcations to compounds containing no phosphorus(e.g., (NH4)x(Mg)y(Al)zF6(OH)6·2H2O, NaMgAlF6·XH2O, MgAl2F8, MgAlF5)before ammoniation and thus to promote P2O5 yield of the product.Meanwhile, the dosage of NaF was optimized.The influence of NaF on the XRD patterns and morphologies of precipitates, removal of cations and the residual fluoride content in phosphoric acid was analyzed.When mNaF/m(mass ratio of NaF to H3PO4 solution) was lower than 3.5%, precipitates mainly existed as NaMgAl(F, OH)6·H2O, XMgAlF6(X=K+or NH4 +).While mNaF/m was increased, the diffraction peaks intensity of NaMgAlF6 gradually increased.When mNaF/m was further increased to 6.0%, calcium-containing silicate or aluminate salts phases appeared.Significantly, the adding amount of NaF also influenced the filtration performance.The content of metal cations in phosphoric acid decreased with the increase of NaF content.When mNaF/m was 6.0%, the content of Mg, Al, Fe, K, Na and Ca was decreased to 0.029%, 0.002 7%, 0.012%, 0.014%, 0.018% and 0.037%, respectively.Albeit higher mNaF/m would result in higher removal efficiency of metal cations, the effect of NaF on the residual fluoride content in phosphoric acid was significant.When mNaF/m was in the range of 1.2%~2.5%, there were no obvious differences in residual fluorine content of phosphoric acid, but further increased to 5%, the residual fluorine content in phosphoric acid was sharply increased from 0.148% to 0.331%.Hence, balancing the removal efficiency of metal cations and residual fluorine content in phosphoric acid, mNaF/m was fixed at 2.5% for the following fabrication of ammonium dihydrogen phosphate.Ammonium dihydrogen phosphate with a purity of 98.53% was produced with a high P2O5 recovery ratio of 86.2% and low residual fluorine content of 0.23%, which met the class Ⅱ standard of industrial grade ammonium dihydrogen phosphate.
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