Study on removal of Fe3+ from sodium dihydrogen phosphate by emulsification solvent extraction

Wet-process phosphoric acid (WPA) is gradually paid attention to in recent years. However, there are some undesirable impurities (Fe³⁺, Al³⁺, Mg²⁺) in WPA, which will degrade the quality of sodium dihydrogen phosphate (NaH₂PO₄) products. To get the superior grade NaH₂PO₄, the WPA should be purified. Enhancing the pH of the solution, often to 4, can remove most of the metal ions, but there is still some Fe³⁺ which has great effect on the NaH₂PO₄ crystal products, seem to be irregular long strips. Therefore, before the neutralized NaH₂PO₄ solution is concentrated, the Fe³⁺ must be removed.The emulsification extraction of Fe³⁺ from sodium dihydrogen phosphate (NaH₂PO₄) solution by di(2-ethylhexyl)phosphoric acid (D2EHPA) is investigated. The good extraction efficiency of Fe³⁺ with D2EHPA from NaH₂PO₄ solution by emulsification extraction is verified. Meanwhile, to study the advantages of the emulsification extraction process, the major influencing factors, such as the D2EHPA volume fraction, the phase volume ratio, the initial pH of NaH₂PO₄ solution, the stirring time and agitation speed on the extraction efficiencies of Fe³⁺, are studied, and the optimal process conditions are obtained. The results of extraction experiments from practical NaH₂PO₄ solution show that superior grade NaH₂PO₄ can be obtained by three stages of extraction under appropriate condition.     

乳化萃取法脱除Mg2+制备工业级磷酸二氢钠的研究

本文以高效的二(2-乙基己基磷酸)(D2EHPA)为萃取剂,采用乳化萃取技术来提取NaH2PO4溶液中的Mg2+杂质,通过考察萃取剂浓度,水相溶液pH值,相比(水相:有机相),乳化速度等对萃取Mg2+萃取率的影响,求得适宜工艺条件:D2EHPA体积分数:75%,相比(A/O):2∶1,起始NaH2PO4溶液pH值为4,搅拌速度:3000r.min-1;实验结果表明,在适宜工艺条件下,经过三级萃取,可制取工业级NaH2PO4。     

萃取法制备工业级磷酸二氢铵-萃取剂的反萃取研究

本课题以高效的2-乙基己基磷酸(D2EHPA)为萃取剂,采用溶剂萃取法来提取MAP溶液中的Mg2++杂质,从而实现生产高品质MAP的目的;但是实现其产业化的难点之一,就是反萃取剂的选择,而在选择反萃取剂时关键是实现络合物D2EHPA-Fe3+的有效分离,因为络合物D2EHPA-Fe3+是非常稳定的,而且Fe3+的富集能使萃取剂老化.因此,选择有效的反萃取剂来实现D2EHPA的循环回收利用是非常有必要的.以H2SO4+添加剂A为反萃取剂,通过考察反萃取剂浓度,相比,反应温度,反应时间,搅拌速度等对反萃取Fe3+反萃取率的影响,求得最佳工艺条件为H2SO4浓度:4mol· L-1,反应温度45℃,相比为1∶1,搅拌速度550r· min-1,搅拌时间0.5h.     

Fractionation of Soybean Globulins Using Ca<Superscript>2+</Superscript> and Mg<Superscript>2+</Superscript>: A Comparative Analysis

The substitution of CaCl₂ by MgCl₂ was undertaken in Deak’s two-step process of separating the soybean 11S and 7S globulins, aiming at higher purities and lower phytic acid (PA) contents of recovered protein fractions. The effects of pH and the addition of NaCl were also evaluated. Compared with CaCl₂, MgCl₂ reduced the PA content of the 11S-rich fraction by 63–71% but increased that of the 7S-rich fraction by 14–28%, depending on pH. Correspondingly, more Ca²⁺ was recovered in the 11S-rich fraction, while more Mg²⁺ co-precipitated with the 7S-rich fraction. NaCl increased the purity of the 11S-rich fraction and reduced its PA content, but the purity of the 7S-rich fraction was reduced by using 50–100 mM NaCl. Lowering pHs from 6.4 and 4.8 to 5.6 and 4.0 in the two precipitation steps increased the yield of both fractions. The optimized fractionating procedure was as follows: the 11S-rich fraction was precipitated at pH 5.8 by using 5 mM MgCl_2, 10 mM NaHSO₃ and 20 mM NaCl, followed by the precipitation of the 7S-rich fraction at pH 4.5. The new method provided both fractions with satisfactory protein yields (22% for 11S and 16% for 7S), purities (88% for 11S and 80% for 7S) and PA contents (0.356% for 11S and 0.882% for 7S).     

甲醇沉淀法净化湿法稀磷酸制磷酸氢二铵

介绍了甲醇沉淀法净化杂质含量较高的湿法稀磷酸(五氧化二磷质量分数25.71%)制备高品质磷酸氢二铵(DAP)的方法.详细研究了碳酸氢铵用量、甲醇用量、反应温度及反应时间对湿法稀磷酸中杂质去除率和五氧化二磷损失率的影响.得到了优化的工艺条件:碳酸氢铵用量,即氮、磷物质的量比为0.25～0.50;甲醇用量,即甲醇与磷酸质量比为4;反应温度65℃,反应时间1.25～1.50 h.用净化后的湿法稀磷酸制备出了18-46-0规格的DAP.新方法为利用中低品位磷矿制备高品质肥料磷酸氢二铵提供了一条可行的途径.     

湿法磷酸净化的萃余酸联产磷酸二氢铵和磷酸氢二钠

湿法磷酸净化及滴灌施肥技术是近年来推广应用的先进技术.湿法磷酸净化技术可大幅度节能,而滴灌施肥可达到节水及高效吸收肥效的目的.提出了用湿法磷酸净化装置副产的萃余酸制滴灌磷酸二氢铵(MAP)和工业级磷酸氢二钠(DSHP)的工艺方案.将滴灌MAP和DSHP的生产结合起来,既充分利用了萃余酸中的钠离子,又克服了萃余酸不能单独生产滴灌MAP的不足,同时生产两种产品可降低成本.该联产工艺的特点在于用生产滴灌MAP后的母液来生产DSHP.实验证明该工艺合理可行,可生产出高品质的滴灌MAP和DSHP,而且生产成本低,有较大的市场竞争力.     

Removal of iron from Cr-electroplating solution by extraction with di(2-ethylhexyl)phosphoric acid in kerosene

The extraction of iron(III) from aqueous sulphate solution was studied using di(2-ethylhexyl)phosphoric acid (HA) mixed with kerosene. Distribution ratios were investigated as a function of the concentration of sulphuric acid, extractant, metal, hydrogen ion as well as the phase ratio and loading capacity of the extractant. The extracted iron species was suggested as [Fe(HA₂)₃] and the extraction constant was found to equal (9.1 ± 0.5) × 10². The thermodynamic functions calculated from the temperature dependence data referred to the endothermic nature of the extraction process. The method of extraction was successfully applied to remove the iron from the chromium electroplating solution giving purification percent of about 97.5%.     

Effects of co-ion initial concentration ratio on removal of Pb<Superscript>2+</Superscript> from aqueous solution by modified sugarcane bagasse

A modified sugarcane bagasse (SCB) fixed bed column was used to remove Pb²⁺ from aqueous solution. To determine the optimal condition for Pb²⁺ separation, Ca²⁺ was chosen as the model interfering ion, and effects of Ca²⁺ and Pb²⁺ initial concentration ratio (C ₀ ^Ca : C ₀ ^Pb ) on the adsorption of Pb²⁺ were investigated. Results showed that adsorption amount ratio of Ca²⁺ and Pb²⁺ (q _e ^Ca : q _e ^Pb ) had a good linear relationship with C ₀ ^Ca : C ₀ ^Pb . Mass ratio of Pb²⁺ absorbed on the modified SCB was higher than 95% at C ₀ ^Ca : C ₀ ^Pb <1.95, illustrating that Pb²⁺ could be selectively removed from aqueous solution. To verify that, simulated waste water containing co-ions of K⁺, Na⁺, Cd²⁺ and Ca²⁺ was treated, and results showed that the equilibrium amount of Pb²⁺, K⁺, Na⁺, Cd²⁺ and Ca²⁺ adsorbed was 134.14, 0.083, 0.058, 1.28, and 1.28mg g^?1, respectively, demonstrating that the modified SCB could be used to remove Pb²⁺ from aqueous solution in the investigated range.     

湿法磷酸生产磷酸二氢钾杂质净化率研究

采用批量实验研究了结晶法净化湿法磷酸与氯化钾复分解反应生产磷酸二氢钾新工艺各阶段杂质的净化率。结果表明 :该工艺不同阶段对杂质有不同脱除效果 ,利用该工艺生产的磷酸二氢钾能够达到HG2 32 1-92标准     

Efficient manganese luminescence induced by Ce<Superscript>3+</Superscript>-Mn<Superscript>2+</Superscript> energy transfer in rare earth fluoride and phosphate nanocrystals

Manganese materials with attractive optical properties have been proposed for applications in such areas as photonics, light-emitting diodes, and bioimaging. In this paper, we have demonstrated multicolor Mn²⁺ luminescence in the visible region by controlling Ce³⁺-Mn²⁺ energy transfer in rare earth nanocrystals [NCs]. CeF₃ and CePO₄ NCs doped with Mn²⁺ have been prepared and can be well dispersed in aqueous solutions. Under ultraviolet light excitation, both the CeF₃:Mn and CePO₄:Mn NCs exhibit Mn²⁺ luminescence, yet their output colors are green and orange, respectively. By optimizing Mn²⁺ doping concentrations, Mn²⁺ luminescence quantum efficiency and Ce³⁺-Mn²⁺ energy transfer efficiency can respectively reach 14% and 60% in the CeF₃:Mn NCs.     

复盐结晶法生产磷酸二氢钾结晶动力学研究

研究了用三聚氰胺结晶法由湿法磷酸生产磷酸二氢钾的结晶动力学过程。考察了搅拌、振动、杂质对结晶过程的影响及不同降温速率对结晶习性的影响,拟合并给出结晶动力学方程,采用差热分析和热重分析仪测试了结晶产品的脱水特性。     

结晶法净化湿法磷酸生产磷酸二氢钾研究

研究了三聚氰胺结晶法净化湿法磷酸复分解生产精细磷酸二氢钾工艺中磷酸三聚氰胺与氯化钾反应生产磷酸二氢钾的工艺条件。采用二次正交组合实验设计,对反应过程中反应温度,反应时间,搅拌速度,氯化钾用量,氯化钾初始浓度等诸因素的一次作用,二次作用及交互作用对五氧化二磷转化率的影响进行了研究,得到了适宜的工艺条件,所得磷酸二氢钾达到HG2321－91质量标准。     

湿法磷酸、硫酸钾萃取法制取磷酸二氢钾工艺的可行性分析

分析了国内外工业化KH2PO4的各种生产方法,提出了以湿法磷酸与K2SO4为原料萃取法生产KH2PO4工艺路线。该方法具有原料易得、操作简便、无环境污染等优点,其工业化KH2PO4产品ω(KH2PO4)≥97%,ω(SO42-)≤2.0%。     

Efficacy of tri-n-octylamine,tri-n-butyl phosphate and di-(2-ethylhexyl) phosphoric acid for reactive separation of protocatechuic acid

ABSTRACT

Owing to its chemical and pharmacological significances, the efficacy of reactive separation of protocatechuic acid (0.001–0.01 kmol m^?3) from aqueous stream by means of tri-n-octylamine (TOA), di-2-ethylhexyl phosphoric acid (D2EHPA) as well as tri-n-butyl phosphate (TBP) in octanol has been investigated, in terms of extraction efficiency, loading ratio, equilibrium complexation constants, and distribution coefficients. Extraction ability was obtained in the order TOA (91.2%) > TBP (88.64%) > D2EHPA (86.43%). In all cases, 1:1 protocatechuic acid:extractant complex is obtained. Further, diffusion coefficients, number of stages for extraction systems, and relative basicity model were used for relating the efficacy.     

以湿法磷酸生产磷酸钾铵的研究

探讨以湿法磷酸、硫酸钾和氨为原料生产一种由磷酸二氢钾和磷酸二氢铵组成的高浓度复合肥料的技术路线。并通过实验,确定了操作条件,试制品为白色晶体,易溶于水,其三元素含量容易控制在55014。     

Effect of Ni<Superscript>2+</Superscript>, V<Superscript>4+</Superscript> and Mo<Superscript>6+</Superscript> concentration on iron oxidation by <Emphasis Type="Italic">Acidithiobacillus ferrooxidans</Emphasis>

The ferrous oxidation ability of Acidithiobacillus ferrooxidans was studied in the presence of Ni²⁺, V⁴⁺ and Mo⁶⁺ in 9 K media in order to implement the culture in the bioleaching of spent catalyst. The rate of iron oxidation decreased with increasing concentration of metal ions, but the rate of inhibition was metal-ion dependent. The tolerance limit was critical at a concentration of 25 g/L Ni²⁺, 5 g/L V⁴⁺ and 0.03 g/L Mo⁶⁺. The growth rate of microorganisms was negligible at concentrations of 6 g/L V⁴⁺ and 0.04 g/L Mo⁶⁺. Levels and degree of toxicity of these ions have been quantified in terms of a toxicity index (TI). The toxicity order of metal ions was found to be Mo⁶⁺>V⁴⁺>Ni²⁺. The significance and relevance of multi-metal ion tolerance in Acidithiobacillus ferrooxidans has been highlighted with respect to bioleaching of spent refinery catalyst.     

湿法磷酸净化试验研究

对以磷酸三丁酯作萃取溶剂净化湿法磷酸的工艺、流程和相关技术进行了研究,完成了1 000 t/a P2O5湿法磷酸净化中试。试验结果表明工艺流程合理可行设计制造的振动筛板塔、萃取槽等关键设备运行稳定、效率高制取的净化磷酸成本低、质量优,为工业放大提供了可靠依据。     

Preparation and characterization of layered silicate magadiite intercalated by Cu<Superscript>2+</Superscript> and Zn<Superscript>2+</Superscript> for antibacterial behavior

The purpose of this work is the synthesis of two series of layered silicate materials with different ratios (10, 30, 50, 80 and 100) of Cu(NO₃)₂, or Zn(NO₃)₂ by ion-exchange method. Several analysis techniques have been used such as X-ray diffraction, energy dispersive X-ray spectroscopy, thermogravimetric analysis, scanning electron microscope and Fourier transform infrared spectroscopy. The results revealed that ion-exchange method of copper and zinc with different ratios did not affect the structure of Na-magadiite. The gap between the theoretical and experimental ion-exchange are in agreement. Antibacterial activity test against Escherichia coli, Rhizobium sp. and Staphylococcus demonstrate that when ratio was (30, 50, 80 and 100) the antibacterial activity of the layered silicate materials showed high antibacterial activity.     

磷酸分解亚硫酸铵制磷铵的研究

将硫酸生产尾气中的 SO2 回收后生成的亚硫酸铵进行深度加工。用磷酸分解使亚硫酸铵变为磷铵和高浓度 SO2 ,这样既解决了 SO2 的回收利用问题 ,又生产了磷铵复合肥料。本文对磷酸分解亚硫酸铵的过程进行了研究 ,分析了实验中的主要影响因素 ,找到了最适宜的工艺操作条件