CN1132104A - 用十二烷基膦酸二乙酯萃取水溶液中的酸和金属盐的方法 - Google Patents
用十二烷基膦酸二乙酯萃取水溶液中的酸和金属盐的方法 Download PDFInfo
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- 239000002184 metal Chemical class 0.000 title claims abstract description 26
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- -1 dodecyl diethyl phosphonate Chemical compound 0.000 claims description 14
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- JPGXOMADPRULAC-UHFFFAOYSA-N 1-[butoxy(butyl)phosphoryl]oxybutane Chemical compound CCCCOP(=O)(CCCC)OCCCC JPGXOMADPRULAC-UHFFFAOYSA-N 0.000 description 28
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- AKYZQUHZKDCACI-UHFFFAOYSA-N 1-dibutoxyphosphoryloctane Chemical compound CCCCCCCCP(=O)(OCCCC)OCCCC AKYZQUHZKDCACI-UHFFFAOYSA-N 0.000 description 3
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- 229910052500 inorganic mineral Inorganic materials 0.000 description 3
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- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical group [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 2
- LCKIEQZJEYYRIY-UHFFFAOYSA-N Titanium ion Chemical compound [Ti+4] LCKIEQZJEYYRIY-UHFFFAOYSA-N 0.000 description 2
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- 230000015572 biosynthetic process Effects 0.000 description 2
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- 239000011593 sulfur Substances 0.000 description 2
- 229910052714 tellurium Inorganic materials 0.000 description 2
- 238000004448 titration Methods 0.000 description 2
- ZTEHOZMYMCEYRM-UHFFFAOYSA-N 1-chlorodecane Chemical compound CCCCCCCCCCCl ZTEHOZMYMCEYRM-UHFFFAOYSA-N 0.000 description 1
- LJKDOMVGKKPJBH-UHFFFAOYSA-N 2-ethylhexyl dihydrogen phosphate Chemical compound CCCCC(CC)COP(O)(O)=O LJKDOMVGKKPJBH-UHFFFAOYSA-N 0.000 description 1
- KXDHJXZQYSOELW-UHFFFAOYSA-N Carbamic acid Chemical class NC(O)=O KXDHJXZQYSOELW-UHFFFAOYSA-N 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- VTLYFUHAOXGGBS-UHFFFAOYSA-N Fe3+ Chemical compound [Fe+3] VTLYFUHAOXGGBS-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
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- 229910052770 Uranium Inorganic materials 0.000 description 1
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- 150000001412 amines Chemical class 0.000 description 1
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- 229910052785 arsenic Inorganic materials 0.000 description 1
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- 229910052794 bromium Inorganic materials 0.000 description 1
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- LXCYSACZTOKNNS-UHFFFAOYSA-N diethoxy(oxo)phosphanium Chemical compound CCO[P+](=O)OCC LXCYSACZTOKNNS-UHFFFAOYSA-N 0.000 description 1
- HRKQOINLCJTGBK-UHFFFAOYSA-N dihydroxidosulfur Chemical compound OSO HRKQOINLCJTGBK-UHFFFAOYSA-N 0.000 description 1
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- 229910052732 germanium Inorganic materials 0.000 description 1
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- QWPPOHNGKGFGJK-UHFFFAOYSA-N hypochlorous acid Chemical compound ClO QWPPOHNGKGFGJK-UHFFFAOYSA-N 0.000 description 1
- 229910052738 indium Inorganic materials 0.000 description 1
- 229910000765 intermetallic Inorganic materials 0.000 description 1
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- 229910052743 krypton Inorganic materials 0.000 description 1
- 229910052745 lead Inorganic materials 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
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- 229910052754 neon Inorganic materials 0.000 description 1
- 229910052758 niobium Inorganic materials 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- QVLTXCYWHPZMCA-UHFFFAOYSA-N po4-po4 Chemical compound OP(O)(O)=O.OP(O)(O)=O QVLTXCYWHPZMCA-UHFFFAOYSA-N 0.000 description 1
- 229910052699 polonium Inorganic materials 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000012063 pure reaction product Substances 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
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- 229910052707 ruthenium Inorganic materials 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 229910052711 selenium Inorganic materials 0.000 description 1
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- 229910052712 strontium Inorganic materials 0.000 description 1
- 125000000547 substituted alkyl group Chemical group 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 150000003460 sulfonic acids Chemical class 0.000 description 1
- 150000003467 sulfuric acid derivatives Chemical class 0.000 description 1
- 230000002277 temperature effect Effects 0.000 description 1
- 229910052716 thallium Inorganic materials 0.000 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
- BDZBKCUKTQZUTL-UHFFFAOYSA-N triethyl phosphite Chemical class CCOP(OCC)OCC BDZBKCUKTQZUTL-UHFFFAOYSA-N 0.000 description 1
- DNYWZCXLKNTFFI-UHFFFAOYSA-N uranium Chemical compound [U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U] DNYWZCXLKNTFFI-UHFFFAOYSA-N 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
- 229910052727 yttrium Inorganic materials 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B17/00—Sulfur; Compounds thereof
- C01B17/69—Sulfur trioxide; Sulfuric acid
- C01B17/90—Separation; Purification
- C01B17/901—Recovery from spent acids containing metallic ions, e.g. hydrolysis acids, pickling acids
- C01B17/903—Recovery from spent acids containing metallic ions, e.g. hydrolysis acids, pickling acids by liquid-liquid extraction
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/46—Preparation involving solvent-solvent extraction
- C01B25/461—Preparation involving solvent-solvent extraction the phosphoric acid present in the medium obtained after reaction being first extracted from the liquid phase formed or separated then re-extracted as free acid by using water or as a phosphate by using a basic compound
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/04—Solvent extraction of solutions which are liquid
- B01D11/0492—Applications, solvents used
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- C01B7/00—Halogens; Halogen acids
- C01B7/01—Chlorine; Hydrogen chloride
- C01B7/07—Purification ; Separation
- C01B7/0706—Purification ; Separation of hydrogen chloride
- C01B7/0731—Purification ; Separation of hydrogen chloride by extraction
- C01B7/0737—Purification ; Separation of hydrogen chloride by extraction hydrogen chloride being extracted
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/26—Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds
- C22B3/38—Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds containing phosphorus
- C22B3/383—Tervalent phosphorus oxyacids, esters thereof
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- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/001—Preparation involving a liquid-liquid extraction, an adsorption or an ion-exchange
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- C22B34/00—Obtaining refractory metals
- C22B34/10—Obtaining titanium, zirconium or hafnium
- C22B34/12—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08
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- C22B34/1259—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08 obtaining titanium or titanium compounds from ores or scrap by wet processes, e.g. by leaching treatment or purification of titanium containing solutions or liquors or slurries
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Abstract
十二烷基膦酸二乙酯(DEDP)在萃取水溶液中的酸和金属盐中的用途。
Description
本发明涉及十二烷基膦酸二乙酯在萃取水溶液中的酸和金属盐的用途。
现有技术中已知磷酸三丁酯(TBP)用作磷酸、铀、稀土元素、锌、铁和其它金属的萃取剂(见Science and Technololgy ofTributyl Phosphate;W.W.Schultz,J.D.Navratil;CRC Press,Boca Raton,Floria(1987)Vol.IIA,第65-121页)。它的萃取作用是基于电中性酸分子或金属盐的亲脂性溶剂化物的形成。许多金属如锌或铁在盐酸溶液中会形成氯络合物,它们能以高分配系数(C有机相/C水相)被萃取形成象ZnCl2·2TBP或HFeCl4·2TBP。在硝酸溶液中镧系元素或锕系元素会形成稳定的硝酸络合物,它们同样能以高分配系数被萃取出来。在这类情况中,用磷酸三丁酯就可以获得满意的萃取效果。
用于含硫酸盐的溶液时它就会完全不同。硫酸络合物的稳定性一般比氯或硝酸络合物的稳定性稳定性低,正因为如此,几乎所有的金属用TBP时,只能以低分配系数从硫酸溶液中被萃取出来。在大多数酸的萃取中也会发现低分配系数。由于它们的低分配系数和低萃取率令人值得怀疑这类萃取工艺的经济性。
为此,有人在专利文献中已经提出其它的萃取剂如丁基膦酸二丁酯(DBBP),它可以用于那些难萃取的物质如硫酸溶液中的硫酸氧钛(DE-OS 3643711)。丁基膦酸二丁酯比TBP能够产生更高的分配系数,但它的缺点是在水中的溶解度高。纯TBP在水中的溶解度为400mg/l,而纯DBBP在水中的溶解度为1200mg/l,戊基膦酸二戊酯(DPPP)和辛基膦酸二丁酯(DBOP)在水中的溶解度分别为100mg/l和10mg/l,明显优于DBBP,但在分配系数上明显不如DBBP,同样较低。
本发明目的就是为难于萃取的物质提供一种适当的萃取剂,它除了可以用一种简单的方法制备外在水中的溶解度很低并且分配系数很高。这一目的是用十二烷基膦酸二乙酯作为萃取剂来实现的。
本发明涉及十二烷基膦酸二乙酯(DEDP)在作为萃取溶液中的酸和金属盐的萃取剂的用途。
可用作DEDP的是亚磷酸三乙酯和1-氯代癸烷纯反应产物的同分异构体或1-十二烷烯和亚磷酸二乙酯的反应产物,它除了正十二烷基磷酸二乙酯为主要成分外还含有其它C12异构体的化合物。
用DEDP作萃取剂可以不稀释,也可以用选自于脂肪族烃类,脂环烃类或芳香烃类中的一种溶剂稀释。如果需要防止第三相的形成,也可以加入象异癸醇或壬酚类的调节剂。
最好把DEDP与其它中性、酸性或碱性萃取剂混合使用。例如,用含中性萃取剂磷酸三丁酯的DEDP混合物萃取磷酸。用含酸性萃取剂双-(2-乙基己基)磷酸的DEDP混合物从无机酸溶液中萃取钼。另外,DEDP还可以作为萃取长链胺的调节剂。
被萃取的酸既可以是无机酸也可以是有机酸。
术语″无机酸″包括无机强酸如HPO4、H2SO4,HNO3,或HCl;无机弱酸如H3BO3或H2O2;也可包括许多金属、半金属和非金属的含氧酸如HReO4,H2SeO4或HClO4。后面的酸最好是由元素周期表中第4到第8副族元素和第5到第7主族元素形成的,因为这些元素在高氧化态下优先形成酸性或两性氧化物或氢氢化物。如果除了水相外还有一种无机酸如H2SO4的话,最后提取的酸的萃取会有特别高的产率。
术语″有机酸″包括单一和多官能团羧酸类,羟基羧酸类,氨基羧酸类,磺酸类,酚类,硫醇类和醇类。
被萃取的金属盐包括周期表中除碱金属盐和碱土金属盐以外的所有金属和半金属盐。
从含氯化物的溶液中优先萃取出除铝盐外周期表中第3到第6主族的金属和半金属盐、第1到第3副族的金属盐和第8副族以及锕系元素的金属盐。
从含硝酸盐的溶液中优先萃取出钪,镱,镧,镧系元素和锕系元素的盐。
从含硫酸盐或硝酸盐的溶液中优先萃取出以高氧化态存在时的周期表第2副族和第4到第8副族的金属盐,以及周期表中第4到第6主族的金属和半金属盐。这里的术语″高氧化态″是指金属的正氧化态,等于周期表族号GM或族号减去一:GM-1,如Ti(IV),V(V)或Cr(VI)。
在这方面,我们列出元素周期表来明确各族元素的下列含义:
第1副族 Cu,Ag,Au GM=1
第2副族 Zn,Cd,Hg GM=2
第3副族 Sc,Y,La,Ac GM=3
第4副族 Ti,Zr,Hf GM=4
第5副族 V,Nb,Ta GM=5
第6副族 Cr,Mo,W GM=6
第7副族 Mn,Te,Re GM=7
第8副族 Fe,Ru,Os GM=8
Co,Rh,Ir
Ni,Pd,Pt
第1主族 Li,Na,K,Rb,Cs,Fr
第2主族 Be,Mg,Ca,Sr,Ba,Ra
第3主族 B,Al,Ga,In,Tl
第4主族 C,Si,Ge,Sn,Pb
第5主族 N,P,As,Sb,Bi
第6主族 O,S,Se,Te,Po
第7主族 F,Cl,Br,I,At
第8主族 Ne,Ar,Kr,Xe,Rn
在所有这些的应用中,DEDP与开始提到的萃取剂TBP,DBBP和DPPP比较具有的优点是它在水中的溶解度很低。尽管十二烷基膦酸二乙酯(DEDP)比戊基膦酸二戊酯(DPPP)仅多一个碳原子,但它的水溶解度为5mg/l,却低20倍。此外,尽管辛基膦酸二丁酯(DBOP)与DEDP具有相同数量的碳原子,但辛基膦酸二丁酯(DBOP)在水中的溶解度却反为DEDP的两倍。用对比测量法就能驳到首先想到的一个正常的假设,即由于在DEDP分子中有两个乙氧基团,它应该比DPPP或DBOP具有更加敏感的水解性。化合物DEDP,DPPP和DBOP甚至在40℃、3摩尔/升H2SO4中保持6周也没有出现分解现象。但是,在用DEDP时,相的分离明显比用DPPP或DBOP时发生的更快更完全。
总之,与烷基膦酸二烷基酯如DBBP,DPPP和DBOP相比,DEDP在水中的溶解度明显较低,同时可以保持恒定的抗水解作用,并且还具有更好地相分离。使用DEDP可以使萃取过程中萃取剂的损耗很低,并且可以显著提高整个过程的经济。上述有关萃取工艺的优点与所萃取的物质种类无关。
萃取以高氧化态存在的第2副族和第4到第8副族元素的化合物和周期表第4到第6主族的金属和半金属化合物证明了使用DEDP的另一个优点。
这些元素一般只能用常用的低分配系数的萃取剂如TBP或DBBP从硫酸或硝酸溶液中萃取。但是,当溶液中酸浓度较低时就需要更高的分配系数。在这些应用中,DEDP比DBBP具有更高的分配系数,这令人极为惊奇,因为DEDP的分子量明显高于DBBP的分子量,所以人们以为它比DBBP有更低的分配系数。但是,DBOP完全具有所预料的性能,由于它有与DEDP相同的分子量,所以它有明显比DBBP低的分配系数。在这方面相反,DBOP和DEDP的性能却令人惊奇,因为两个化合物都有不对称取代烷基、相同的分子量和相同数量的碳原子。在下文中的实施例1和表1中通过从硫酸溶液中萃取钛(IV)来举例说明这一点。然后在表1中可以看到DEDP的分配系数比DBBP的和DBOP的更高,特别是在较低的硫酸浓度中。因此,这是非常有利的,因为在高浓度硫酸中,硫酸中的硫酸氧钛解度会明显下降,这还因为对钛的萃取来说,高浓度的范围仅用于特殊的情况。
在磷酸或盐酸的萃取中也会看到DEDP比DBBP和DBOP有更高的分配系数(见下文的表2和表3)。
把有机相和水或一种碱水溶液混合用公知的方式可以分离金属盐和酸,其中碱水溶液含有象NaOH,NaHCO3,K3PO4,NH3或其它碱性物质。这种分离也受高于萃取温度的的温度影响。
就所给出的物质种类而言,在很多情况下可以选择性地使用DEDP进行萃取,以便使多次分离成为可能。
例如,使用DEDP可以将下面的物质从硫酸或硝酸溶液中萃取出来:
—周期表中除铅和硼外第4到第7主族的酸和金属盐;
—金属氧化态等于该金属的族号GM或族号减去一:GM-1(高氧化态)时的周期表中第2副族与第4到第8副族的酸和金属盐。
相反,不能从硫酸或硝酸溶液中萃取的物质实例有:
—金属氧化态低于族号减去一GM-1(低氧化态)时的周期表中第2副族与第4到第8副族的酸和金属盐;
—周期表中第1到第3主族(不含硼)和第1副族的酸和金属盐。
从这里可以证明从硫酸或硝酸溶液中选择性地萃取能把除铅外的周期表第4到第7主族(包括硼)的酸和金属盐以及周期表中第2副族和第4到第8副族的高氧化态金属与不能萃取的第2副族和第4到第8副族低氧化态的金属物质和周期表中第1到第3主族(不含硼)以及第1副族的金属分离。
可行性应用例包括:
—有选择性地从TiO2生产过程的硫酸浸提液或沉淀液中萃取钛(IV)[在Al(III)(第3主族),Mg(II)(第2主族),Fe(II)(第8副族,低氧化价(GM-6),Cr(III)(第6副族,低氧化态GM-3)和V(III)(第5副族,低氧化态GM-2)的存在下选择性地萃取Ti(IV)(第4副族.,高氧化态GM)。
—有选择地从含磷酸的无机物浸提液中萃取磷酸[在Al(III)(第3主族)和Fe(III)(第8副族,低氧化态(GM-5)的存在下有选择地萃取H3PO4(酸,第5主族)]。
本发明将通过下面的实施例作更详细的阐述。实施例1
用DEDP萃取硫酸溶液中萃取的Ti(IV)(与用DBBP和DBOP对照)
起始含量为50到70kg/钛/kg溶液与1-5摩尔硫酸/升溶液的几种硫酸氧钛的硫酸水溶液在室温下与未稀释的DEDP、DBBP或DBOP充分搅拌15分钟)(相比率约为1/1)。相分离之后,直接测定水相(萃取液)中钛的含量,用H2SO4/H2O2浸提后,通过原子吸收光谱法测定有机相中钛的含量。为了测定酸的含量,先用水以1/100的比率稀释水相,并加热回流一小时。随后再用氢氧化钠滴定来测定酸的总含量。结果见表1。
表1用DEDP,DBBP和DBDP萃取硫酸中的钛的结果
萃取剂 | 萃取液中酸的总含量(以摩尔H2SO4/l计算) | 萃取液中钛的含量(g/kg) | 钛的分配系数(C有机相/C水相) |
DEDP | 2.31 | 46 | 0.16 |
DEDP | 3.41 | 37 | 0.32 |
DEDP | 4.31 | 31 | 0.47 |
DEDP | 4.96 | 24 | 0.74 |
DEDP | 5.60 | 17 | 1.2 |
DBBP | 2.48 | 65 | 0.009 |
DBBP | 3.51 | 59 | 0.059 |
DBBP | 4.53 | 50 | 0.23 |
DBBP | 4.97 | 43 | 0.41 |
DBBP | 5.35 | 36 | 0.69 |
DBOP | 3.49 | 39 | 0.04 |
DBOP | 4.45 | 33 | 0.15 |
DBOP | 5.20 | 28 | 0.45 |
实施例2
用DEDP萃取磷酸(与用TBP对照)
未稀释的萃取剂,预先用水饱和,再室温下与起始含量为1-50%,H3PO4水溶液充分搅拌15分钟。相分离后,用KOH滴定来测定水相和有机相中酸的浓度。结果见表2。
表2用DEDP和TBP萃取磷酸的结果
萃取相 | 水相中酸的浓度(摩尔HPO4/升) | H3PO4的分配系数C有机相/C水相 |
DEDP | 0.393 | 0.38 |
DEDP | 0.798 | 0.38 |
DEDP | 1.22 | 0.39 |
DEDP | 2.70 | 0.37 |
TBP | 0.480 | 0.10 |
TBP | 0.766 | 0.12 |
TBP | 1.453 | 0.17 |
TBP | 2.993 | 0.24 |
实施例3
用DEDP萃取盐酸(与用DBBP和DBOP对照)
除用盐酸代替磷酸外,其它步骤与实施例2相似。结果见表3。
表3:用DEDP,DBBP和DBOP萃取盐酸的结果
萃取相 | 水相中酸的浓度(摩尔HCl/升) | 盐酸的分配系数C有机相/C水相 |
DEDP | 0.461 | 0.238 |
DEDP | 1.80 | 0.37 |
DEDP | 3.43 | 0.41 |
DBBP | 0.501 | 0.10 |
DBBP | 1.49 | 0.19 |
DBBP | 3.22 | 0.34 |
DBOP | 0.54 | 0.06 |
DBOP | 1.59 | 0.13 |
DBOP | 3.47 | 0.25 |
很显然说明书和实施例是用来详细说明,而不是限定本发明的,本领域技术人员会提出属于本发明构思和范围内的其它实施方案。
Claims (11)
1.一种从水溶液中萃取至少一种酸或金属盐的方法,包括将所述的溶液与十二烷基膦酸二乙酯混合,使混合物分层,并分离各层。
2.根据权利要求1所述的方法,其中十二烷基膦酸二乙酯是与脂族烃、脂环烃或芳香烃混合使用的。
3.根据权利要求1所述的方法,其中混合是在调节剂存在下进行的。
4.根据权利要求3所述的方法,其中调节剂至少包括异癸醇或壬酚中的一种。
5.根据权利要求1所述的方法,其中十二烷基膦酸二乙酯是与酸性、中性或碱性的辅助萃取剂混合来用于酸或金属盐的萃取。
6.根据权利要求1所述的方法,其中水溶液包括一种酸。
7.根据权利要求1所述的方法,其中酸或金属盐是以硫酸或硝酸的溶液中存在的,并且选自于周期表中第4到第7主族和硼(除去铅)或,氧化态与副族金属的族号GM或族号减一GM-1相对应的周期表中第2副族和第4到第8副族中的一种可萃取的酸或金属盐。
8.根据权利要求1所述的方法,其中水溶液包括硫酸氧钛的硫酸溶液。
9.根据权利要求7所述的方法,其中溶液中还包括至少一种不能被萃取的金属盐,它选自于周期表中第2副族和第4到第8副族中氧化态比相应的族号减一GM-1低的一种金属,以及周期表中第1到第3主族和第1副族的一种金属中,这些多余的金属盐不能被萃取。
10.根据权利要求1所述的方法,其中酸或金属盐存在于磷酸或硝酸或一种硝酸盐溶液中,并且选自于钪,镱,镧,一种镧系元素和锕系元素中。
11.根据权利要求1所述的方法,其中酸或金属盐存在于盐酸或一种氯化物溶液中,并且选自于周期表第3到第7主族中(除去铝)的一种金属,周期表中第1到第3副族和第8副族中的一种金属和一种锕系金属元素中的一种金属。
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US7736610B2 (en) * | 2004-09-24 | 2010-06-15 | Battelle Energy Alliance, Llc | Actinium radioisotope products of enhanced purity |
US7157061B2 (en) * | 2004-09-24 | 2007-01-02 | Battelle Energy Alliance, Llc | Process for radioisotope recovery and system for implementing same |
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US2864668A (en) * | 1956-11-23 | 1958-12-16 | Willis H Baldwin | Uranium extraction process |
US2859094A (en) * | 1957-02-07 | 1958-11-04 | John M Schmitt | Uranium extraction process using synergistic reagents |
US3312623A (en) * | 1963-12-23 | 1967-04-04 | Monsanto Co | Antiseptic detergent compositions |
US3493639A (en) * | 1965-10-27 | 1970-02-03 | Shell Oil Co | Process for producing pentavalent phosphorus derivatives |
US3751555A (en) * | 1972-03-22 | 1973-08-07 | Molybdenum Corp | Solvent extraction process for the recovery of molybdenum and rhenium from molybdenite |
DE2239591A1 (de) * | 1972-08-11 | 1974-02-28 | Bayer Ag | Verfahren zur extraktion von zink, cadmium und/oder indium aus metallsalzloesungen |
FR2298361A1 (fr) * | 1973-02-27 | 1976-08-20 | Pierre Delvalle | Procede de separation par voie chimique |
US4371504A (en) * | 1977-02-28 | 1983-02-01 | Uranium Recovery Corporation | Extractant and process for extracting uranium wet-process phosphoric acid |
US4255392A (en) * | 1978-07-13 | 1981-03-10 | Wyoming Mineral Corp. | Method of separating iron from uranium |
US4544530A (en) * | 1980-10-10 | 1985-10-01 | Institute Of Nuclear Energy Research | Separation process for the recovery of uranium from wet-process phosphoric acid |
FR2515630B1 (fr) * | 1981-10-30 | 1985-10-04 | Rhone Poulenc Spec Chim | Procede d'extraction et de separation de l'uranium, du thorium et des terres rares par traitement de solutions aqueuses de chlorures de ces elements |
FR2523466B1 (fr) * | 1982-03-19 | 1986-09-12 | Rhone Poulenc Sa | Procede de recuperation et de purification d'un acide sulfurique residuaire contenant des sels de titane |
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DE3643711A1 (de) * | 1986-12-20 | 1988-06-30 | Bayer Antwerpen Nv | Verfahren zur herstellung von hochwertigem titandioxid nach dem sulfatverfahren |
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- 1995-10-18 AU AU34331/95A patent/AU689316B2/en not_active Ceased
- 1995-10-19 US US08/545,454 patent/US5682593A/en not_active Expired - Fee Related
- 1995-10-20 JP JP7295939A patent/JPH08224403A/ja active Pending
- 1995-10-23 CA CA002161180A patent/CA2161180A1/en not_active Abandoned
- 1995-10-24 FI FI955069A patent/FI955069A/fi unknown
- 1995-10-25 KR KR1019950037005A patent/KR960013414A/ko not_active Application Discontinuation
- 1995-10-25 ZA ZA959027A patent/ZA959027B/xx unknown
- 1995-10-25 BR BR9504542A patent/BR9504542A/pt not_active Application Discontinuation
- 1995-10-26 CN CN95120299A patent/CN1132104A/zh active Pending
Also Published As
Publication number | Publication date |
---|---|
DE4438174C2 (de) | 1996-08-29 |
EP0709471A1 (de) | 1996-05-01 |
KR960013414A (ko) | 1996-05-22 |
CA2161180A1 (en) | 1996-04-27 |
FI955069A0 (fi) | 1995-10-24 |
AU3433195A (en) | 1996-05-09 |
BR9504542A (pt) | 1997-05-27 |
JPH08224403A (ja) | 1996-09-03 |
TR199501248A2 (tr) | 1996-06-21 |
DE4438174A1 (de) | 1996-05-02 |
ZA959027B (en) | 1996-05-23 |
US5682593A (en) | 1997-10-28 |
FI955069A (fi) | 1996-04-27 |
AU689316B2 (en) | 1998-03-26 |
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