萃取法制取磷酸二氢钠的研究

研究了以湿法净化磷酸和工业氯化钠为原料,利用有机溶剂萃取法制取磷酸二氢钠的新方法。确定了一种水溶性小、萃取效率高、对盐酸萃取选择性好的萃取剂,并研究了萃取温度、萃取时间、磷酸与氯化钠物质的量比、萃取剂与氯化钠物质的量比、稀释剂加入量等对萃取率和分配比的影响。通过单因素实验确定了较优工艺条件:萃取温度为50℃;萃取时间为20 min;磷酸与氯化钠物质的量比为1.0~1.2;萃取剂与氯化钠物质的量比为1.2~1.3;稀释剂加入量为3%~20%(体积分数);反萃取时间为15 min。在此条件下,五氧化二磷收率可达95.64%,产品二水合磷酸二氢钠纯度可达99.5%以上,氯离子质量分数小于0.1%。     

萃取法制取磷酸二氢钠的试验研究

中国磷酸钠盐的生产一般是以工业磷酸和碳酸钠或氢氧化钠为原料,生产成本较高。开发了一种以湿法磷酸、氯化钠为原料,采用连续萃取法制取工业级磷酸二氢钠的方法,并进行了连续化的模式试验研究。结果表明:在控制溶配液中磷酸与氯化钠物质的量比为1.1,溶配液(五氧化二磷质量分数为14.45%)与萃取剂的体积比为1:7,萃取温度为40～50℃,磷酸二氢钠料液的pH为4.2～4.5,盐洗液的pH为5.0～6.5,氯化铵液的pH为8.0～9.0的工艺条件下,试验得到的磷酸二氢钠产品质量可达到工业级磷酸二氢钠(HG/T2767—1996)指标要求。阐述了试验的基本原理、连续萃取法的工艺条件、产品质量和消耗,提出了直接采用湿法磷酸、氯化钠为原料生产工业磷酸钠盐的可行性。     

固液反萃湿法磷酸生产磷铵的工艺研究

通过连续逆流萃取对原料湿法磷酸先进行净化,萃取后的有机溶剂相直接用氨反萃取生成磷铵晶体,再沉降使晶体与有机萃取剂分离,实现磷铵直接反萃结晶和萃取剂的循环利用。结果表明用氨直接固液反萃湿法磷酸生产磷铵的最佳工艺条件是：萃取剂组成为V(磷酸三丁酯)∶V(稀释剂)=1∶1,原料磷酸浓度为w（P₂O₅）=40%～50%,萃取剂用量为V(萃取剂)∶V(原料磷酸)≈3∶1,萃取搅拌时间约为5 min,氨用量控制为氨反萃结晶后的液相pH≈7,固液反萃-结晶温度为15～20 ℃。最终所得的磷铵晶体中w(氮)＞20%、w(五氧化二磷)＞50%,原料湿法磷酸中的五氧化二磷一次性利用率接近50%。该法所得磷铵晶体中氮磷含量均接近工业磷酸二铵(98%)标准,远大于国家肥料级农用磷铵产品标准。     

利用磷酸三丁酯在硫酸-磷酸体系中萃取净化低浓度湿法磷酸工艺的研究

研究了利用磷酸三丁酯在硫酸-磷酸体系中萃取净化低浓度湿法磷酸工艺,获得了萃取性能较好的萃取体系。实验表明,稀释剂（煤油）添加量为磷酸三丁酯与稀释剂总质量的10％时,萃取净化较佳工艺条件为：萃取相比4,萃取温度40℃,搅拌时间15min,硫酸添加量为原料湿法磷酸的1％;SO42^-去除率-80％,Fe、Al去除率99％以上,P2O5,损失率约60％,所得净化稀磷酸P2O5,7．5％,可作为热法磷酸吸收剂。     

酶法转化体系中L-苯丙氨酸的络合萃取

L-苯丙氨酸的分离提取对于促进酶法制备工艺的产业化进程具有重要价值。利用络合萃取分配系数、分离选择性高的特点,对苯丙酮酸酶法制备L-苯丙氨酸转化体系中L-苯丙氨酸的络合萃取进行了研究。以二(2-乙基己基)磷酸为萃取剂,研究了水相平衡pH、萃取剂浓度和稀释剂的种类对分配系数的影响;并利用D2EHPA-正辛醇体系对酶法制备L-苯丙氨酸的转化液进行了络合萃取研究,经4次萃取和1次反萃,L-苯丙氨酸的萃取率达到98 15%;经1次反萃,L-苯丙氨酸的收率达94 33%。     

含金属离子赖氨酸水溶液的萃取分离

采用二(2-乙基己基)磷酸(P204)作萃取剂,航空煤油作稀释剂,对含有钙、镁、钠、钾等金属离子的赖氨酸水溶液进行萃取,以蒸馏水作为反萃取剂对有机相进行反萃取分离实验.结果表明,原料液初始pH值在4～5、P204与煤油体积比为3:2、有机相与水相比为2:1、反应萃取时间大于30min、搅拌转速约200rpm时,能够取得较好的萃取效果.以初始pH值≥3.5的蒸馏水为反萃取剂,蒸馏水与有机相体积比4:1,在150rpm的转速下搅拌20min能够较为完全地分离出赖氨酸,然后在其它条件相同的情况下,用初始pH＜1的蒸馏水对有机相再次反萃取可分离出金属离子,从而实现萃取剂的重复利用.     

撞击流—旋转填料床处理含苯酚废水的单级试验研究

以撞击流—旋转填料床(IS—RPB)作为萃取器和反萃取器,以磷酸三了酯(TBP)作为络合萃取剂,以煤油为稀释剂,以氢氧化钠溶液为反萃剂,对含苯酚废水进行了萃取与反萃取的单级试验研究。在研究IS—RPB两个主要操作参数撞击流初速ν_0和转速N,油水比R以及TBP在油相中的体积分数对级分配率D的影响基础上,找到了最适宜的工艺条件,在此条件下得到了高达95％以上的除酚率。     

溶剂萃取法净化湿法磷酸的研究进展

介绍了溶剂萃取净化湿法磷酸的研究进展情况.近期研究得出的结论有:选用与水不溶的萃取剂;稀释剂的适宜加入量为总溶剂量的10%～30%;萃取体系适宜的相比为:萃取相比(有机相/水相)3:1,洗涤相比(有机相/水相)18:1,反萃相比(有机相/水相)10:1.研究的创新点有:萃取设备采用振动筛板塔;开发了三次脱硫技术;磷酸精制和渣酸制肥结合;萃取稀释剂便宜易得;化学沉淀法与溶剂萃取法结合;脱硫、脱色、脱氟在同一工序中进行.     

湿法磷酸萃取制取高品质磷酸二氢钾工艺研究

磷酸二氢钾在当前的磷酸盐工业中具有重要的实用价值,其应用涉及到工业、农业、医药以及食品等多个行业。以尽可能低成本的原材料与更简易的工艺流程来生产具备更高品质特性的磷酸二氢钾为时下所需。以湿法磷酸与氯化钾为原料,进行了有机溶剂萃取法制备磷酸二氢钾的工艺研究。研究内容包括：在溶配过程中氯化钾与磷酸物质的量比对氟离子脱除率的影响;氯化钾与磷酸物质的量比、反应时间、反应温度以及萃取相比对萃取率及杂质脱除率的影响;不同洗涤相比对五氧化二磷洗涤率的影响;反萃取以及磷酸二氢钾浓缩结晶的相关工艺。通过实验确定湿法磷酸萃取制取高品质磷酸二氢钾适宜工艺条件：反应温度为60 ℃,反应时间为30 min,氯化钾与磷酸物质的量比为1.0,洗涤相比为12。在此工艺条件下所得磷酸二氢钾产品纯度高达97%,达到磷酸二氢钾农用级优等品标准的要求,同时五氧化二磷回收率可达到96%。     

溶剂萃取法制取三聚磷酸钠

利用高分子胺作缔合剂，以湿法磷酸、芒硝为主要原料，萃取制取磷酸二氢钠，经过中和、聚合后，生产高质量的三聚磷酸钠。     

钨萃取平衡分配比的研究

使用一套溶剂萃取平衡的试验装置，选择膦酸三丁酯（ＴＢＰ）为萃取剂，苯为稀释剂，系统地测定了钨的溶剂萃取平衡及萃取条件对萃取平衡分配的影响，可为工业过程设计、工程优化和计算机模拟提供依据。     

Research on extraction of Cr(III) by D2EHPA/n-octanol/sulphonated kerosene

Chromium is an important industrial raw material. As far as China is concerned, chromium is in great demand, which is dependent on imports and large emissions. So recovery of chromium has important economic and environmental protection value. The extraction and back extraction of Cr(III) from solution by the extractant diisooctyl phosphate (di-2-ethylhexylphosphoric acid [D2EHPA]) with n-octanol as assistant and sulphonated kerosene as diluent was studied. The effects of saponification rate, phase ratio, temperature, condensation of extract, aging of extractant, and pH of aqueous phase on extraction equilibrium were discussed, and the formulation of extractant was optimized. The coordination number of the extraction reaction under specific conditions was discussed by the saturation capacity method. The extraction reaction kinetics were mathematically characterized by binary linear regression. The advantages and disadvantages of back extraction with H₂SO₄ or NaOH were compared. At last, a process to realize the recycling of extractant was obtained.     

Modeling of Phosphoric Acid Purification by Liquid‐Liquid Extraction

Phosphoric acid is an important industrial chemical. It is mainly produced by the wet process which consists of an attack of the phosphate rock by sulphuric acid leading to a complex solution containing a large number of impurities such as metal ions like Fe³⁺, Al³⁺, Mg²⁺, Cd²⁺ etc., which can effectively be recovered by solvent extraction process. In this present work a model of the liquid‐liquid extraction process is presented. It is mainly based on thermodynamics, where two different routes have been tested for the modeling of the complexation process. The method has been tested using a model system with Al³⁺ as the contaminant, dodecyl naphthalene sulphonic acid (HDDNSA) as the complexing agent and kerosene as the diluent. The study has also investigated the influence of various parameters such as the pH of the aqueous phase and the initial concentration of the phosphoric acid.     

Parameters Influencing Third‐Phase Formation in the Extraction of Th(NO3)4 by some Trialkyl Phosphates

Third‐phase formation in the extraction of Th(IV) by trialkyl phosphates (TalP) such as tri‐n‐butyl phosphate (TBP), tri‐iso‐butyl phosphate (TiBP), tri‐sec‐butyl phosphate (TsBP), tri‐n‐amyl phosphate (TAP), tri‐2‐methylbutyl phosphate (T2MBP), tri‐iso‐amyl phosphate (TiAP), tri‐sec‐amyl phosphate (TsAP), and tri‐cyclo‐amyl phosphate (TcyAP) has been investigated under various conditions. Formation of a third phase in the extraction of Th(IV) by TBP/n‐dodecane as a function of TBP concentration at 303 K was studied. Measurements were also carried out on the extraction of Th(IV) from its solution with near‐zero free acidity by various phosphate/diluent binary solutions (1.1 M) as a function of temperature. Third‐phase formation in the extraction of Th(IV) by 1.1 M TalP in various diluents from nitric acid media has also been studied as a function of equilibrium aqueous‐phase acidity at 303 K. Empirical equations to predict limiting organic concentration with respect to various parameters for third‐phase formation in the extraction of Th(IV) by TBP and TAP from nitric acid media have been derived. Some of the above phosphates have been investigated for the distribution of Th(NO₃)₄ between the “diluent‐rich phase” (DP) and “third‐phase” (TP) in the extraction of Th(IV) by 1.1 M TalP in various diluents from its saturated solution with near‐zero free acidity at 303 K. Results of the above studies are presented in this paper. Based on these studies, the effects of extractant concentration, the temperature, the nature of the diluent, the equilibrium aqueous‐phase acidity, and the structure of the extractant on third‐phase formation behavior of trialkyl phosphates are described in this paper.     

Extraction of copper from aqueous solutions with carboxylic acids

The distribution equilibrium data at 25°C for the extraction of copper from aqueous solutions, containing sodium nitrate or sodium sulphate, by carboxylic acids using toluene, benzene and carbon tetrachloride as diluents have been measured. The carboxylic acids used are n-myristic, n-lauric and n-capric. The results obtained led to the conclusion that the composition of the extracted species corresponds to (CuR₂.HR)₂, being irrespective of both the nature of organic phase and the aqueous phase. The addition of sodium sulphate, instead of sodium nitrate, decreases the extraction efficiency due to the formation a CuSO₄ ion-pair into the aqueous phase. The diluent effect has been related to the activity of the dimerised carboxylic acid in the diluent.     

钨钼混合溶液萃取平衡的测定与研究

采用一套溶剂萃取平衡测定装置,在酸性介质中,选择D2EHPA[二－（2－乙基己基）磷酸酯]为萃取剂,煤油为稀释剂,仲辛醇为改质剂,EDTA为络合剂,系统完整地测定了不同条件下两种浓度范围的含大量钨和少量钼的溶液的钨钼萃取分离平衡数据,分析和研究了各种因素对钨钼萃取分离的影响．分别用萃取平衡的经验模型和化学模型对该萃取体系进行了关联计算,得出了一套可以在工业计算中使用的经验模型和化学模型,为工业过程设计、工程优化和计算机模拟提供了基础．     

HYDROFLUORIC ACID EXTRACTION BY TBP AND BY AMINES: I. A CRITICAL REVIEW OF THE HF-H2O-EXTRACTANT SYSTEM

Literature on HF extraction by amines and by tributyl phosphate is critically reviewed. The system amine-HF-H₂O shows an interesting feature concerning properties such as distribution curves compared to those for extraction of other acids, similarity to extraction by TBP, water extraction, selectivity, effect of amine type and dilution and diluent effect These properties sharply change (or even invert) when HF/amine molar ratio exceeds 2.