CN105854842A - Method for adsorption and separation of molybdenum from aqueous phase - Google Patents
Method for adsorption and separation of molybdenum from aqueous phase Download PDFInfo
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- CN105854842A CN105854842A CN201610334997.3A CN201610334997A CN105854842A CN 105854842 A CN105854842 A CN 105854842A CN 201610334997 A CN201610334997 A CN 201610334997A CN 105854842 A CN105854842 A CN 105854842A
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/103—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate comprising silica
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/26—Synthetic macromolecular compounds
- B01J20/264—Synthetic macromolecular compounds derived from different types of monomers, e.g. linear or branched copolymers, block copolymers, graft copolymers
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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
- C22B34/00—Obtaining refractory metals
- C22B34/30—Obtaining chromium, molybdenum or tungsten
- C22B34/34—Obtaining molybdenum
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/46—Materials comprising a mixture of inorganic and organic materials
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- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4806—Sorbents characterised by the starting material used for their preparation the starting material being of inorganic character
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4812—Sorbents characterised by the starting material used for their preparation the starting material being of organic character
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Abstract
The invention discloses a method for adsorption and separation of molybdenum from an aqueous phase. The method comprises the following steps: an adsorbent is mixed with a nitric acid aqueous solution containing a variety of metal ions, molybdate ions in the nitric acid aqueous solution are adsorbed by the adsorbent to be separated, and the adsorbent is prepared by compounding a compound as shown in formula I and a carrier. Each gram of the adsorbent is mixed with 15 to 25 milliliters of the nitric acid aqueous solution. The carrier is macroporous SiO2 of which the surface is coated with a polymer, and the concentration of nitric acid in the nitric acid aqueous solution is 0.4 to 6.0 mol/L. According to the invention, a diluent with special performance is not required to dilute or dissolve in the adsorption process, and the method is good selectivity, fast in separation speed, simple to operate and easy to popularize.
Description
Technical field
The present invention relates to molybdenum element separation technology field, be specifically related to a kind of from aqueous phase adsorbing separation molybdenum
Method.
Background technology
Owing to Binding Forces Between Atoms is extremely strong, metal molybdenum intensity at ambient and elevated temperatures is the highest.Molybdenum swollen
Swollen coefficient is little, and conductance is big, good heat conductivity.The most not with hydrochloric acid, hydrofluoric acid and aqueous slkali
There is chemical reaction, be only soluble in nitric acid, chloroazotic acid or the concentrated sulfuric acid, to most of liquid metals, nonmetal
Slag and melten glass also quite stable.Therefore, molybdenum and alloy thereof are in metallurgical, agricultural, electric, change
The important departments such as work, environmental protection and aerospace have a wide range of applications and good prospect, become national economy
Middle a kind of important raw material and irreplaceable strategic material.
Molybdenum-99 is one of radio isotope of molybdenum, is used for preparing technetium-99 in hospital.Technetium-99 is one
Plant radio isotope, after clothes for patients, can be used for internal organs radiography.Molybdenum-99 for this kind of purposes
It is stored in relatively small container after generally absorbing with alumina powder, generates technetium when molybdenum-99 decays
-99, technetium-99 can be taken out from container when needed and issue patient
Molybdenum in China aboundresources, explored molybdenum reserves 8,400,000 tons, occupy second place of the world, molybdenum
Product yield occupies third place in the world, accounts for the 24～25% of World Molybdenum total output.Although molybdenum in China resource phase
When abundant, but can have sense of crisis, mineral resources are non-renewable resources, always have a day of exhaustion.
Along with the continuous expansion of Mo resource application, the demand of molybdenum and compound thereof is also constantly being increased
Greatly.Rely solely on extraction molybdenum and compound from natural crystal and can not meet the need of production development
Want, and molybdenum is as a kind of limited resources, it is impossible to it is carried out unconfined exploitation, so to molybdenum
The recycling of resource just has important strategic importance.In recent years, China's pay attention to day by day to molybdenum one
The comprehensive utilization of secondary resource and the recycling of secondary resource.
The regenerated resources of molybdenum are less, and its source is main by three below approach:
(1) recycling of Mo resource in dead catalyst；
(2) recycling of the molybdenum in all kinds of metallurgical process molybdenum-containing waste slags；
(3) recycling of molybdenum in metallic article waste material.
The Chinese patent literature of Publication No. CN 103342769A discloses the separation resin of a kind of molybdenum
Preparation method, the separation resin of molybdenum prepared by the method, its Stability Analysis of Structures, for extract and separate
During molybdenum, the fastness of extraction chromatography is preferable, substantially increases the α-benzoinoxime selectivity to molybdenum.
But the preparation method of this separation resin is more numerous and diverse, and selectivity to this molybdenum separation resin is not ground
Study carefully, it is impossible to realize, from complex environment, molybdenum is carried out Selective Separation.
Nuclear power is owing to energy density is big, it is few to pollute in recent years, will not discharge cause greenhouse gases and
Obtain flourish, but spentnuclear fuel can be inevitably generated in the middle of nuclear power operation.Locate after spentnuclear fuel
The produced high activity liquid waste (HLLW) of reason, is a kind of peracidity, high radioactivity and highly toxic mixing
Solution, wherein contains a certain amount of molybdenum, if it is possible to separate Mo resource therein, it is achieved return
Receive and utilize, significant, but, in present stage high activity liquid waste, the separation of molybdenum element is still in research rank
Section, does not the most find high efficiency recovery approach.
Summary of the invention
It is an object of the invention to provide a kind of method from aqueous phase adsorbing separation molybdenum, simple to operate, choosing
Selecting property is good, and separative efficiency is high, it is easy to carry out industrial application.
A kind of method from aqueous phase adsorbing separation molybdenum, comprise the steps: by adsorbent with containing multiple
The aqueous solution of nitric acid mixing of metal ion, the molybdenum acid ion in aqueous solution of nitric acid is adsorbed by adsorbent point
Compound preparing is carried out by the compound as shown in structural formula I and carrier from, described adsorbent:
Compound name as shown in structural formula I is: the double (5,6-dihexyl-1,2,4-triazine-3-of 6,6'-
Base)-2,2'-bipyridyl, referred to as: C6-BTBP.
In the present invention, described carrier is the macro-pore SiO that surface is coated to polymer2。
Described surface is coated to the macro-pore SiO of polymer2For silica-based-styrene-divinylbenzene polymer
(SiO2-P), it is a class novel inorganic/organic support material, disclosed in United States Patent (USP) US6843921
Silica-based-styrene-divinylbenzene polymer, SiO2-P is a kind of containing porous SiO2Particle organic
High polymer complex carrier, its preparation method is as follows:
(1) by the SiO of macropore2It is washed till neutrality by red fuming nitric acid (RFNA) washing, suction filtration, deionized water, repeats
More than ten times, it is dried.
(2) vacuum under the conditions of having argon shield, with 1,2,3-trichloropropanes and m-dimethylbenzene are solvent,
To macro-pore SiO2The m/p-formyl styrene of middle addition 48.7g, the m/p-divinylbenzene of 8.9g,
72.2g dioctylphthalate, 54.0g benzoin methyl acid sodium, 0.56g α, α-idol bis-isobutyronitrile
With 0.57g 1,1 '-even dicyclohexyl amine-1-nitrile, room temperature it is gradually heated to 90 DEG C, and keeps 13 hours,
Afterwards, room temperature progressively it is cooled to.
(3) respectively with acetone and methyl alcohol washing, the above-mentioned product of suction filtration, repeat more than 10 times, be dried.
In the present invention, the preparation method of described adsorbent is as follows:
Compound as shown in structural formula I is dissolved in organic solvent, adds in gained solution and carry
Body mixes, and after rotation is evaporated off organic solvent, obtains adsorbent.
As preferably, every gram of compound as shown in structural formula I is dissolved in 100～200 milliliters of organic solvents
In.
In adsorbent, as shown in structural formula I, the content of compound will affect separating effect, when content is too low,
The adsorption capacity of adsorbent is more weak；During too high levels, the preparation cost of adsorbent will be increased.As excellent
Choosing, as shown in structural formula I, compound is 1:2～10 with the mass ratio of carrier.Further preferably, such as knot
Compound shown in structure Formulas I is 1:8～10 with the mass ratio of carrier.
Described organic solvent is chloroform, dichloromethane, acetone and 1, at least one in 2-dichloroethanes,
It is preferably at least one in chloroform and dichloromethane.
When rotation is steamed, make majority of organic solvent evaporate into nearly dry state, inhale in capillarity and physics
Under attached effect, compound molecule enters in the hole of carrier, and the material of the most dry state exists
It is vacuum dried at 45～55 DEG C at least 24 hours, obtains adsorbent.
In order to ensure separating effect, it is preferable that every gram of adsorbent and 15～25 milliliters of aqueous solution of nitric acid mix
Close.Further preferably, every gram of adsorbent and 20 milliliters of aqueous solution of nitric acid mixing.
Adsorbent and aqueous solution of nitric acid mixing and absorption, adsorption temp is 298～318K, and adsorption time is
5～210min.Adsorbent will affect separating effect with the time of contact of the aqueous solution, and time of contact is too short,
Absorption is not yet complete, and time of contact is long, reduces separative efficiency.Further preferably, adsorption temp is
298K, adsorption time is 60～120min.
Adsorbent and aqueous solution of nitric acid mixing and absorption, mixing and absorption is carried out under oscillating condition, vibration speed
Rate is 120～150rpm.
In aqueous solution of nitric acid, the concentration of every metal ion species is 5.0 × 10-4～5.0 × 10-2Mol/L.Nitre
In aqueous acid, the concentration of metal ion can affect separating effect, and the excessive concentration of metal ion has
The adsorbing separation ability of adsorbent can be can exceed that；The concentration of metal ion is too low, then can reduce separation effect
Rate.Further preferably, the concentration of every metal ion species is 2.0 × 10-3～5.0 × 10-3Mol/L.
In aqueous solution of nitric acid, the concentration of nitric acid is 0.4～6.0 mol/L.The concentration of nitric acid can affect point
From effect, it is preferable that the concentration of nitric acid is 2.0～6.0 mol/L, further preferably, nitric acid is dense
Degree is 2.0 mol/L.
Containing Mo (VI) and other metal ions in described aqueous solution of nitric acid, other metal ions are
Li(I)、Na(I)、K(I)、Rb(I)、Cs(I)、Ca(Ⅱ)、Mg(Ⅱ)、Sr(Ⅱ)、Ba(Ⅱ)、La(Ⅲ)、
At least one in Nd (III), Ru (III), Yb (III), Y (III), Fe (III) and Zr (IV).
The invention provides a kind of method from aqueous phase adsorbing separation molybdenum, without using in adsorption process
The diluent with property is diluted or dissolves, it is not necessary to add other organic compounds, dirty
Contaminating little, the best, separative efficiency is high, simple to operate, it is easy to promote.
Accompanying drawing explanation
Fig. 1 be the adsorbent utilizing embodiment 1 from aqueous solution of nitric acid the distribution coefficient of Separation of Molybdenum with nitre
The graph of a relation of acid concentration change；
Fig. 2 be the adsorbent utilizing embodiment 1 from aqueous solution of nitric acid the distribution coefficient of Separation of Molybdenum with temperature
The graph of a relation of degree change.
Detailed description of the invention
Embodiment 1
0.5 gram is had double (5,6-dihexyl-1,2,4-triazine-3-base)-2,2'-bipyridyl of 6,6'-of structural formula I
It is dissolved in 60.0 milliliters of dichloromethane, fully dissolves and obtain golden transparent solution；Golden yellow to this
Solution adds 4.5 grams of SiO2-P stirs, and makes SiO2-P mixes with compound, through decompression rotation
Turning evaporation makes dichloromethane major part evaporate into material to nearly dry state, inhales in capillarity and physics
Organic molecule is made to enter SiO under attached effect2In-P hole, the material of the most dry state is at 55 DEG C
Lower vacuum drying 24h, obtains C6-BTBP/SiO2-P composite, i.e. adsorbent.
Embodiment 2
0.5 gram is had double (5,6-dihexyl-1,2,4-triazine-3-base)-2,2'-bipyridyl of 6,6'-of structural formula I
It is dissolved in 50.0 milliliters of dichloromethane, fully dissolves and obtain golden transparent solution；Golden yellow to this
Solution adds 4.0 grams of SiO2-P stirs, and makes SiO2-P mixes with compound, through decompression rotation
Turning evaporation makes dichloromethane major part evaporate into material to nearly dry state, inhales in capillarity and physics
Organic molecule is made to enter SiO under attached effect2In-P hole, the material of the most dry state is at 55 DEG C
Lower vacuum drying 24h, obtains C6-BTBP/SiO2-P composite, i.e. adsorbent.
Embodiment 3
0.5 gram is had double (5,6-dihexyl-1,2,4-triazine-3-base)-2,2'-bipyridyl of 6,6'-of structural formula I
It is dissolved in 75.0 milliliters of dichloromethane, fully dissolves and obtain golden transparent solution；Golden yellow to this
Solution adds 5.0 grams of SiO2-P stirs, and makes SiO2-P mixes with compound, through decompression rotation
Turning evaporation makes dichloromethane major part evaporate into material to nearly dry state, inhales in capillarity and physics
Organic molecule is made to enter SiO under attached effect2In-P hole, the material of the most dry state is at 55 DEG C
Lower vacuum drying 24h, obtains C6-BTBP/SiO2-P composite, i.e. adsorbent.
Embodiment 4
0.5 gram is had double (5,6-dihexyl-1,2,4-triazine-3-base)-2,2'-bipyridyl of 6,6'-of structural formula I
It is dissolved in 60.0 milliliters of chloroforms, fully dissolves and obtain golden transparent solution；To this golden solution
4.0 grams of SiO of middle addition2-P stirs, and makes SiO2-P mixes with compound, rotates through decompression and steams
Send out and make dichloromethane major part evaporate into material to nearly dry state, at capillarity and physical absorption work
Organic molecule is made to enter SiO under with2In-P hole, the material of the most dry state is true at 45 DEG C
Empty dry 24h, obtains C6-BTBP/SiO2-P composite, i.e. adsorbent.
Embodiment 5～11
(1) by alkali nitrates LiNO3、NaNO3、KNO3、RbNO3、CsNO3；Alkali
Earth metal nitrate Mg (NO3)2、Ca(NO3)2、Sr(NO3)2、Ba(NO3)2；Transition metal salt
Fe(NO3)3、(NH4)6Mo7O24·4H2O、ZrO(NO3)2；The nitrate solution of noble metal Ru；Dilute
Soil metal oxide Y2O3, rare-earth metal nitrate La (NO3)3、Yb(NO3)3And Nd (NO3)3Deng
Addition red fuming nitric acid (RFNA) and deionized water are configured to contain the aqueous solution of nitric acid mother liquor of 17 metal ion species, nitre simultaneously
Concentration of nitric acid in aqueous acid mother liquor is 4.0 mol/L, and the concentration of each metal ion is
2.0～5.0 × 10-3Mol/L.
(2) in aqueous solution of nitric acid mother liquor, add red fuming nitric acid (RFNA) and deionized water, regulate aqueous solution of nitric acid
In concentration of nitric acid, concentration of nitric acid regulates respectively to 0.4,1.0,2.0,3.0,4.0,5.0 and 6.0 and rubs
You/liter, the concentration of every metal ion species is about 5.0 × 10-4Mol/L, occurrence by ICP-OES or
AA240 records.
(3) water of 7 that step (2) the is obtained different concentration of nitric acid containing 17 kinds of metallic elements
The adsorbent that solution is prepared with embodiment 1 respectively contacts mixing, and amount ratio during mixing is: every 3.0mL
Aqueous solution of nitric acid correspondence 0.15g adsorbent；
(4) 7 mixed liquors of step (3) gained are enterprising at TAITEC MM-10 type oscillator
Row adsorption experiment, the oscillation rate of oscillator is 150rpm, operates, during absorption under room temperature 298K
Between be 120min, absorption reach balance after, solid-liquid two-phase is separated, after separation fetch water phase, so
The content of each metallic element in the rear aqueous phase of measurement respectively.
The absorption result of embodiment 5～11 as it is shown in figure 1, in Fig. 1 abscissa be concentration of nitric acid, ordinate
For distribution coefficient.As seen from Figure 1, when concentration of nitric acid is 2.0 mol/L, separating element molybdenum
Effect is best, and the distribution coefficient of molybdenum reaches 76.0 mls/g, and divides for other 16 metal ion species
Distribution coefficient is less than 10 mls/g, illustrates that the adsorbent that the present invention provides is the strongest to molybdenum, is suitable for
From containing molybdenum efficiently separates multiple metallic element aqueous phase recovery, range of application is the widest.
Embodiment 12～16
Experiment condition and step are the same as in Example 9, and difference is, by aqueous solution of nitric acid,
Concentration of nitric acid is fixed as 4.0 mol/L, and adsorption time is 120min, changes adsorption temp successively and is
298K, 303K, 308K, 313K and 318K, gained separating resulting is as in figure 2 it is shown, horizontal seat in Fig. 2
Being designated as adsorption temp, ordinate is distribution coefficient.
As seen from Figure 2, along with the increase of temperature, the adsorption capacity of molybdenum is gradually lowered by this material,
When temperature is 298K, the distribution coefficient of molybdenum is the highest, reaches 78.0 mls/g, and for other 16 metals
The distribution coefficient of ion is less than 10 mls/g, illustrates that the adsorbent that the present invention provides is the strongest to molybdenum,
It is suitable for from containing molybdenum is efficiently separated recovery, range of application pole by multiple metallic element aqueous phase
Extensively.
Claims (9)
1. the method from aqueous phase adsorbing separation molybdenum, it is characterised in that comprise the steps: by
Adsorbent mixes with the aqueous solution of nitric acid containing many kinds of metal ions, the molybdate in aqueous solution of nitric acid from
Son is adsorbed by adsorbent separation, and described adsorbent is carried out with carrier by the compound as shown in structural formula I
It is combined and prepares:
2. as claimed in claim 1 from the method for aqueous phase adsorbing separation molybdenum, it is characterised in that every gram
Adsorbent and 15～25 milliliters of aqueous solution of nitric acid mixing.
3. as claimed in claim 1 from the method for aqueous phase adsorbing separation molybdenum, it is characterised in that described
Carrier is the macro-pore SiO that surface is coated to polymer2。
4. as claimed in claim 1 from the method for aqueous phase adsorbing separation molybdenum, it is characterised in that described
The preparation method of adsorbent is as follows:
Compound as shown in structural formula I is dissolved in organic solvent, adds carrier and mix,
After rotation is evaporated off organic solvent, obtain adsorbent.
5. as claimed in claim 4 from the method for aqueous phase adsorbing separation molybdenum, it is characterised in that every gram
Compound as shown in structural formula I is dissolved in 100～200 milliliters of organic solvents.
6. as claimed in claim 1 from the method for aqueous phase adsorbing separation molybdenum, it is characterised in that such as knot
Compound shown in structure Formulas I is 1:2～10 with the mass ratio of carrier.
7. as claimed in claim 1 from the method for aqueous phase adsorbing separation molybdenum, it is characterised in that nitric acid
In the aqueous solution, the concentration of every metal ion species is 5.0 × 10-4～5.0 × 10-2Mol/L.
8. as claimed in claim 1 from the method for aqueous phase adsorbing separation molybdenum, it is characterised in that nitric acid
In the aqueous solution, the concentration of nitric acid is 0.4～6.0 mol/L.
9. as claimed in claim 1 from the method for aqueous phase adsorbing separation molybdenum, it is characterised in that absorption
Agent and aqueous solution of nitric acid mixing and absorption, adsorption temp is 298～318K, and adsorption time is 5～210min.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106906047A (en) * | 2017-03-14 | 2017-06-30 | 浙江大学 | A kind of method of adsorbing and extracting soluble fine in aqueous solution from flower |
| CN109285616A (en) * | 2018-11-16 | 2019-01-29 | 中国原子能科学研究院 | From235It is extracted in U fission product99The device of Mo and utilization device extraction99The method of Mo |
| CN114717430A (en) * | 2022-04-19 | 2022-07-08 | 中国原子能科学研究院 | Method for extracting molybdenum from uranium fission products and ionic liquid system |
| CN116217785A (en) * | 2023-03-09 | 2023-06-06 | 核工业北京化工冶金研究院 | Molybdenum separation resin and preparation method and application thereof |
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