CN105777789A - Thiele acid uranyl complex, preparation method thereof and Thiele acid application - Google Patents
Thiele acid uranyl complex, preparation method thereof and Thiele acid application Download PDFInfo
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- CN105777789A CN105777789A CN201610219061.6A CN201610219061A CN105777789A CN 105777789 A CN105777789 A CN 105777789A CN 201610219061 A CN201610219061 A CN 201610219061A CN 105777789 A CN105777789 A CN 105777789A
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- 239000002253 acid Substances 0.000 title claims abstract description 61
- 125000005289 uranyl group Chemical group 0.000 title claims abstract description 46
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- JFALSRSLKYAFGM-UHFFFAOYSA-N uranium(0) Chemical compound [U] JFALSRSLKYAFGM-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229910052770 Uranium Inorganic materials 0.000 claims abstract description 12
- 238000006243 chemical reaction Methods 0.000 claims abstract description 9
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 5
- 238000000605 extraction Methods 0.000 claims abstract description 5
- 239000002994 raw material Substances 0.000 claims abstract description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 27
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 claims description 14
- 229910052751 metal Inorganic materials 0.000 claims description 10
- 239000002184 metal Substances 0.000 claims description 10
- 238000000034 method Methods 0.000 claims description 9
- 239000002002 slurry Substances 0.000 claims description 7
- 229910000030 sodium bicarbonate Inorganic materials 0.000 claims description 7
- 235000017557 sodium bicarbonate Nutrition 0.000 claims description 6
- 238000001556 precipitation Methods 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- 229910052768 actinide Inorganic materials 0.000 claims description 3
- 150000001255 actinides Chemical class 0.000 claims description 3
- 238000007605 air drying Methods 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 239000007787 solid Substances 0.000 claims description 3
- 238000012546 transfer Methods 0.000 claims description 3
- ZSLUVFAKFWKJRC-IGMARMGPSA-N 232Th Chemical compound [232Th] ZSLUVFAKFWKJRC-IGMARMGPSA-N 0.000 claims description 2
- UIIMBOGNXHQVGW-DEQYMQKBSA-M Sodium bicarbonate-14C Chemical compound [Na+].O[14C]([O-])=O UIIMBOGNXHQVGW-DEQYMQKBSA-M 0.000 claims description 2
- 229910052776 Thorium Inorganic materials 0.000 claims description 2
- 229910052767 actinium Inorganic materials 0.000 claims description 2
- QQINRWTZWGJFDB-UHFFFAOYSA-N actinium atom Chemical compound [Ac] QQINRWTZWGJFDB-UHFFFAOYSA-N 0.000 claims description 2
- 230000000536 complexating effect Effects 0.000 abstract description 4
- 238000001027 hydrothermal synthesis Methods 0.000 abstract description 4
- 229910002007 uranyl nitrate Inorganic materials 0.000 abstract description 2
- 238000002329 infrared spectrum Methods 0.000 description 8
- 229910002651 NO3 Inorganic materials 0.000 description 6
- 150000001875 compounds Chemical class 0.000 description 5
- 239000000047 product Substances 0.000 description 5
- 238000010521 absorption reaction Methods 0.000 description 4
- 238000011160 research Methods 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 3
- 238000001819 mass spectrum Methods 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 125000002915 carbonyl group Chemical group [*:2]C([*:1])=O 0.000 description 2
- 150000001732 carboxylic acid derivatives Chemical class 0.000 description 2
- ZSWFCLXCOIISFI-UHFFFAOYSA-N cyclopentadiene Chemical compound C1C=CC=C1 ZSWFCLXCOIISFI-UHFFFAOYSA-N 0.000 description 2
- WYICGPHECJFCBA-UHFFFAOYSA-N dioxouranium(2+) Chemical compound O=[U+2]=O WYICGPHECJFCBA-UHFFFAOYSA-N 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000003758 nuclear fuel Substances 0.000 description 2
- 125000004430 oxygen atom Chemical group O* 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- STCOOQWBFONSKY-UHFFFAOYSA-N tributyl phosphate Chemical group CCCCOP(=O)(OCCCC)OCCCC STCOOQWBFONSKY-UHFFFAOYSA-N 0.000 description 2
- VEMKTZHHVJILDY-PMACEKPBSA-N (5-benzylfuran-3-yl)methyl (1r,3s)-2,2-dimethyl-3-(2-methylprop-1-enyl)cyclopropane-1-carboxylate Chemical compound CC1(C)[C@@H](C=C(C)C)[C@H]1C(=O)OCC1=COC(CC=2C=CC=CC=2)=C1 VEMKTZHHVJILDY-PMACEKPBSA-N 0.000 description 1
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 description 1
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 1
- -1 Thiele ' sAcid Chemical compound 0.000 description 1
- 150000001257 actinium Chemical class 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- KRHOUGAQUGCCJI-UHFFFAOYSA-N cyclopenta-1,3-diene-1-carboxylic acid Chemical compound OC(=O)C1=CC=CC1 KRHOUGAQUGCCJI-UHFFFAOYSA-N 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 230000005595 deprotonation Effects 0.000 description 1
- 238000010537 deprotonation reaction Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000002330 electrospray ionisation mass spectrometry Methods 0.000 description 1
- 238000001437 electrospray ionisation time-of-flight quadrupole detection Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 235000019253 formic acid Nutrition 0.000 description 1
- 239000012634 fragment Substances 0.000 description 1
- 238000009432 framing Methods 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- QQVIHTHCMHWDBS-UHFFFAOYSA-N isophthalic acid Chemical compound OC(=O)C1=CC=CC(C(O)=O)=C1 QQVIHTHCMHWDBS-UHFFFAOYSA-N 0.000 description 1
- 239000003446 ligand Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 235000010755 mineral Nutrition 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 150000007524 organic acids Chemical class 0.000 description 1
- 239000013110 organic ligand Substances 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 238000012805 post-processing Methods 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 238000012958 reprocessing Methods 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 238000010183 spectrum analysis Methods 0.000 description 1
- 239000002915 spent fuel radioactive waste Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 229920002994 synthetic fiber Polymers 0.000 description 1
- 229940077390 uranyl nitrate hexahydrate Drugs 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F5/00—Compounds containing elements of Groups 3 or 13 of the Periodic Table
- C07F5/003—Compounds containing elements of Groups 3 or 13 of the Periodic Table without C-Metal linkages
-
- 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
- C22B3/32—Carboxylic acids
- C22B3/324—Naphthenic acids
-
- 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
- C22B60/00—Obtaining metals of atomic number 87 or higher, i.e. radioactive metals
- C22B60/02—Obtaining thorium, uranium, or other actinides
-
- 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
- C22B60/00—Obtaining metals of atomic number 87 or higher, i.e. radioactive metals
- C22B60/02—Obtaining thorium, uranium, or other actinides
- C22B60/0204—Obtaining thorium, uranium, or other actinides obtaining uranium
- C22B60/0217—Obtaining thorium, uranium, or other actinides obtaining uranium by wet processes
- C22B60/0252—Obtaining thorium, uranium, or other actinides obtaining uranium by wet processes treatment or purification of solutions or of liquors or of slurries
- C22B60/026—Obtaining thorium, uranium, or other actinides obtaining uranium by wet processes treatment or purification of solutions or of liquors or of slurries liquid-liquid extraction with or without dissolution in organic solvents
-
- 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
- C22B60/00—Obtaining metals of atomic number 87 or higher, i.e. radioactive metals
- C22B60/02—Obtaining thorium, uranium, or other actinides
- C22B60/0291—Obtaining thorium, uranium, or other actinides obtaining thorium
-
- 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
- C22B60/00—Obtaining metals of atomic number 87 or higher, i.e. radioactive metals
- C22B60/02—Obtaining thorium, uranium, or other actinides
- C22B60/0295—Obtaining thorium, uranium, or other actinides obtaining other actinides except plutonium
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Environmental & Geological Engineering (AREA)
- Geochemistry & Mineralogy (AREA)
- Compounds Of Unknown Constitution (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a Thiele acid uranyl complex, a preparation method thereof and Thiele acid application.The preparation method comprises the following steps that Thiele, Thiele acid and uranyl nitrate are used as raw materials, and the Thiele acid uranyl complex is synthesized through a hydrothermal method.The invention further provides a uranyl complex.The uranyl complex is prepared according to the preparation method.The Thiele acid uranyl complex is successfully synthesized through the hydrothermal method.In the preparation process of the complex, the preparation method is easy, convenient and practical, and the reaction efficiency is high.The product structure is determined through infrared and mass spectrograms, which further illustrates that Thiele acid has the strong complexing ability for uranyl and has the potential of becoming a uranium extraction agent.
Description
Technical field
The application belongs to the field of chemical synthesis, is specifically related to the preparation method of Di Aier acid Complexes of Uranyl, Di Aier acid purposes.
Background technology
In the peaceful use of nuclear energy, creating a considerable number of radwaste, wherein unreacted uranium accounts for (including uranium-238 and uranium-238) major part of spentnuclear fuel gross weight.How to process the important research direction that these uranium waste materials are ENVIRONMENTAL RADIOCHEMISTRY.The research processed for uranium both at home and abroad is concentrated mainly on uranyl absorption on mineral or other synthetic materials or the coordination that uranyl is in water solution system, and part is inorganic acid radical, or the organic ligand designed for obtaining the uranyl complex of certain novel structure.Nuclear fuel reprocessing extractant conventional at present is tributyl phosphate (TBP), and in order to overcome the shortcomings such as its radiation resistance difference, finding new extractant becomes research emphasis.
Organic polyacid is widely used as bridge ligand and constructs high thermal stability Inorganic-Organic Hybrid Material, and the multiple oxygen atoms in its carboxylic acid all can participate in coordination as part, and its abundant coordination mode causes the multiformity of structural framing.The coordination compound of the organic polyacid such as neighbour/M-phthalic acid, 6,6 '-dinitro-2,2 '-diphenic acid and uranyl ion has been reported.
The selection of existing uranium nuclear fuel post processing extractant is fewer, and has various limitation.The new extractant finding complexing efficiency good becomes research emphasis.
Summary of the invention
In view of drawbacks described above of the prior art or deficiency, it is desirable to provide the Di Aier acid Complexes of Uranyl that a kind of complexing efficiency is higher.
The preparation method that the present invention also provides for the simple Di Aier acid Complexes of Uranyl of a kind of preparation method.
The present invention provides again a kind of above-mentioned Di Aier acid as the purposes of metal extraction agent.
First aspect, the preparation method that the present invention provides a kind of Di Aier acid Complexes of Uranyl, comprise the following steps:
With Thiele, Di Aier acid with uranyl nitrtate for raw material, go out Thiele acid Complexes of Uranyl with water heat transfer.
Second aspect, the present invention also provides for a kind of Di Aier acid Complexes of Uranyl, prepares according to above-mentioned preparation method.
The third aspect, the present invention provides again a kind of above-mentioned Di Aier acid as the purposes of metal extraction agent, and described metal is selected from actinides.
The present invention successfully synthesizes Thiele acid Complexes of Uranyl by hydro-thermal method.In the process preparing above-claimed cpd, preparation method is simple and practical, and reaction efficiency is higher.The structure of product is confirmed by infrared and mass spectrogram, further illustrates the coordination ability that Thiele acid is stronger to uranyl, has the potentiality becoming Novel Uranium extractant.
Accompanying drawing explanation
By reading the detailed description that non-limiting example is made made with reference to the following drawings, other features, purpose and advantage will become more apparent upon:
The infrared spectrum of the Thiele acid that Fig. 1 provides for the embodiment of the present invention；
The infrared spectrum of the uranyl nitrtate that Fig. 2 provides for the embodiment of the present invention；
The infrared spectrum of the product Thiele acid Complexes of Uranyl that Fig. 3 provides for the embodiment of the present invention；
The mass spectrum of the Fig. 4 Thiele acid Complexes of Uranyl for providing for the embodiment of the present invention.
Detailed description of the invention
Below in conjunction with drawings and Examples, the application is described in further detail.It is understood that specific embodiment described herein is used only for explaining related invention, but not the restriction to this invention.It also should be noted that, for the ease of describing, accompanying drawing illustrate only and invent relevant part.
It should be noted that when not conflicting, the embodiment in the application and the feature in embodiment can be mutually combined.Describe the application below with reference to the accompanying drawings and in conjunction with the embodiments in detail.
The preparation method that the present invention provides a kind of Di Aier acid Complexes of Uranyl, comprises the following steps:
With Thiele, Di Aier acid with uranyl nitrtate for raw material, under weak basic condition, synthesize Thiele acid Complexes of Uranyl by hydro-thermal method.
Currently preferred technical scheme, the preparation method of a kind of Di Aier acid Complexes of Uranyl, comprise the following steps:
(1) in the water slurry of Thiele acid, add reaction of sodium bicarbonate, be then heated to the first preset temperature, until solid all dissolves；
(2) in above-mentioned solution, add uranyl nitrtate, and reaction vessel is sealed, react under the second preset temperature, and stir, produce precipitation；
(3) described precipitation collected and washed with water, then air drying, obtaining Complexes of Uranyl.
The present invention selects organic acid Thiele acid as uranyl part, and the oxygen atom in its carboxylic acid all can participate in coordination as part, test result indicate that complexing efficiency is higher.In the process preparing above-claimed cpd, preparation method is simple and practical, and reaction efficiency is higher.The structure of product is confirmed by infrared and mass spectrogram.
Preferably, described first preset temperature is 50-60 DEG C, and heat time heating time is 1.5-2.5 hour.
Preferably, described second preset temperature is 100-120 DEG C, and the time of described stirring is 3-5 days.
Preferably, in the water slurry of described Thiele acid, the ratio of Thiele acid and water is 0.20g-1.20gThiele acid/100mL water；The mass ratio that described sodium bicarbonate is sour with Thiele is 1:1.3-2.6.
Preferably, described uranyl nitrtate is 2.28:1 with the mass ratio of Thiele acid.
The present invention also provides for a kind of Di Aier acid Complexes of Uranyl, prepares according to above-mentioned preparation method.
The present invention provides again a kind of above-mentioned Di Aier acid as the purposes of metal extraction agent, and described metal is selected from actinides.
Preferably, described metal is actinium, thorium, protactinium or uranium.
The present invention selects Dimeric Cyclopentadiene Carboxylic Acid, i.e. Thiele ' sAcid, the acid of Di Aier, as part, adopt water heat transfer Thiele, Di Aier acid Complexes of Uranyl, and its Nomenclature Composition and Structure of Complexes being characterized according to experimental result and spectral data, evaluates it as the effect of Novel Uranium extractant and feature.The present invention is sour as part using Thiele, it is possible to expanded metal selects to other elements of actinium series.
Below by specific embodiment, the present invention is described further:
The selection of reagent of the present invention and instrument: uranyl nitrtate (UO2(NO3)2·6H2O, A.R., Beijing coupling Science and Technology Ltd.), sodium bicarbonate (NaHCO3, A.R., Beijing Chemical Plant), experimental water is deionized water.Thiele acid is laboratory early stage synthesis gained or commercially available prod.
Key instrument has infrared spectrometer (IR, Bruker, Tensor27), electrospray ionization mass spectrometry (MS, BrukerDaltonics, ESI-Q-TOF).
Embodiment 1
The preparation method of a kind of Di Aier acid Complexes of Uranyl, comprises the following steps:
(1) in 20mL water, add 0.220g, 1.0mmolThiele acid, form suspension.Adding 0.168g, 2.0mmol sodium bicarbonate in above-mentioned water slurry, reactant mixture, 55 DEG C of heating, has gas to generate, and after 2 hours, solid all dissolves, and generates without gas again.
(2) in above-mentioned solution, add 0.502g, 1.0mmol uranyl nitrate hexahydrate, and reaction tube is sealed.React and stir 4 days at 110 DEG C, produce a large amount of brown precipitate.Above-mentioned precipitation is collected and fully washs (10mL × 6 time) with water, then air drying, namely to place 1-2 days in laboratory table, natural drying, obtain 0.457g product, productivity is 93%, and its structure is confirmed by infrared and mass spectrogram.
Referring to Fig. 1, infrared spectrometer test draw infrared spectrum, analyze infrared spectrum it can be seen that the characteristic absorption peak of Thiele acid is at 1672cm-1Place is VC=OStretching vibration absworption peak；2973cm-1Left and right is the V of hydroxyl in-COOHO-HStretching vibration absworption peak.Referring to Fig. 3, infrared spectrometer test draw infrared spectrum, in the spectrogram of Thiele acid Complexes of Uranyl, at 1672cm-1The carbonyl peak red shift at place is to 1619cm-1Place, Δ VC=OFor 53cm-1, this shows that part passes through carbonyl and the direct coordination of uranium；2973cm-1The peak of left and right disappears substantially, and this shows that part there occurs the deprotonation of-COOH；And 3358cm-1The characteristic peak that place occurs is probably in product containing water of crystallization.
Referring to Fig. 2, infrared spectrometer test drawing infrared spectrum, the characteristic absorption peak of uranyl nitrtate is respectively at 942cm-1Place (O-U-O), 1531cm-1Place (NO3 ˉ), 1266cm-1Place (NO3 ˉ), 1020cm-1Place (NO3 ˉ) and 735cm-1Place (NO3 ˉ).In spectrogram referring to Fig. 3, Thiele acid Complexes of Uranyl, at 915cm-1There is the last one absworption peak at place, for UO2 2+Antisymmetric stretching vibration peak；And NO3 ˉPeak be wholly absent, illustrate coordination compound does not have NO3 ˉExist；466cm-1The strong absworption peak at place is regarded as in carbonyl oxygen and the absorption (U-O) of uranium.
The above data are consistent with the infrared spectrum characterization of the similar coordination compound of existing mono-crystalline structures uranium, change from characteristic group's frequency of vibration of above coordination compound, certain interaction is there is between uranyl ion and Thiele acid molecule, coordination compound contains Thiele acid and water, therefore, infer that its molecular formula is shown in figure below.
Reaction equation is:
Referring to Fig. 4, by MS spectrum analysis it can be seen that due to the cyclopentadiene easy reversible polymerization of formic acid monomer of Thiele acid, its mass spectra peak exists multiformity.The peak that such as several intensity are relatively larger is presumed as follows, and m/z356 is [2M+4Na-H]3+, m/z535 is [M+2Na-H]+, m/z374 and m/z397 is fragment peak.
The mass-to-charge ratio value of X-axis-ion in Fig. 4, Y-axis-intensity, wherein intens is intensity, and+MS is expressed as positive ion mass spectrum, and 0.1-0.6min is experiment duration, and Deconvoluted represents that data are deconvolution.
Embodiment 2
Adopt the method identical with embodiment 1, the difference is that: in water slurry: Thiele acid is 0.20gThiele acid/100mL water with the ratio of water；The mass ratio that described sodium bicarbonate is sour with Thiele is 1:2.0.
Embodiment 3
Adopt the method identical with embodiment 1, the difference is that: in water slurry: Thiele acid is 1.20gThiele acid/100mL water with the ratio of water；The mass ratio that described sodium bicarbonate is sour with Thiele is 1:2.6.
Above description is only the preferred embodiment of the application and the explanation to institute's application technology principle.Skilled artisan would appreciate that, invention scope involved in the application, it is not limited to the technical scheme of the particular combination of above-mentioned technical characteristic, when also should be encompassed in without departing from described inventive concept simultaneously, other technical scheme being carried out combination in any by above-mentioned technical characteristic or its equivalent feature and being formed.Such as features described above and (but not limited to) disclosed herein have the technical characteristic of similar functions and replace mutually and the technical scheme that formed.
Claims (9)
1. the preparation method of Yi Zhong Di Aier acid Complexes of Uranyl, it is characterised in that comprise the following steps:
With Thiele, Di Aier acid with uranyl nitrtate for raw material, go out Thiele acid Complexes of Uranyl with water heat transfer.
2. preparation method according to claim 1, it is characterised in that comprise the following steps:
(1) in the water slurry of Thiele acid, add reaction of sodium bicarbonate, be then heated to the first preset temperature, until solid all dissolves；
(2) in above-mentioned solution, add uranyl nitrtate, and reaction vessel is sealed, react under the second preset temperature, and stir, produce precipitation；
(3) described precipitation collected and washed with water, then air drying, obtaining Complexes of Uranyl.
3. method according to claim 2, it is characterised in that described first preset temperature is 50-60 DEG C, heat time heating time is 1.5-2.5 hour.
4. method according to claim 2, it is characterised in that described second preset temperature is 100-120 DEG C, the time of described stirring is 3-5 days.
5. the method according to any one of claim 1-4, it is characterised in that in the water slurry of described Thiele acid, the ratio of Thiele acid and water is 0.20g-1.20gThiele acid/100mL water；The mass ratio that described sodium bicarbonate is sour with Thiele is 1:1.3-2.6.
6. method according to claim 5, it is characterised in that the mass ratio that described uranyl nitrtate is sour with Thiele is 2.28:1.
7. Yi Zhong Di Aier acid Complexes of Uranyl, it is characterised in that the preparation method described in any one of claim 1-6 prepares.
8. Yi Zhong Di Aier acid is as the purposes of metal extraction agent, and described metal is selected from actinides.
9. purposes according to claim 8, it is characterised in that described metal is actinium, thorium, protactinium or uranium.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107955026A (en) * | 2016-10-15 | 2018-04-24 | 宁波大学 | One kind one is hydrated malonic acid uranyl cadmium ferroelectric function material and preparation method thereof |
| CN111215145A (en) * | 2018-11-26 | 2020-06-02 | 宁波大学 | 2-nitro terephthalic acid uranyl complex photocatalyst |
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| CN105352897A (en) * | 2015-09-02 | 2016-02-24 | 中国原子能科学研究院 | Method for determination of complex extraction equilibrium constant of double extraction agent organic phase system |
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| CN105352897A (en) * | 2015-09-02 | 2016-02-24 | 中国原子能科学研究院 | Method for determination of complex extraction equilibrium constant of double extraction agent organic phase system |
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| CN107955026A (en) * | 2016-10-15 | 2018-04-24 | 宁波大学 | One kind one is hydrated malonic acid uranyl cadmium ferroelectric function material and preparation method thereof |
| CN107955026B (en) * | 2016-10-15 | 2019-10-22 | 宁波大学 | One kind one is hydrated malonic acid uranyl cadmium ferroelectric function material and preparation method thereof |
| CN111215145A (en) * | 2018-11-26 | 2020-06-02 | 宁波大学 | 2-nitro terephthalic acid uranyl complex photocatalyst |
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