CN105854842B - A kind of method from water phase adsorbing separation molybdenum - Google Patents
A kind of method from water phase adsorbing separation molybdenum Download PDFInfo
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- CN105854842B CN105854842B CN201610334997.3A CN201610334997A CN105854842B CN 105854842 B CN105854842 B CN 105854842B CN 201610334997 A CN201610334997 A CN 201610334997A CN 105854842 B CN105854842 B CN 105854842B
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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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- 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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- 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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- 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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- 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 kind of method from water phase adsorbing separation molybdenum, include the following steps：Adsorbent is mixed with the aqueous solution of nitric acid containing various metals ion, the molybdenum acid ion in aqueous solution of nitric acid, which is adsorbed by adsorbent, to be separated, the adsorbent as the compound as shown in structural formula I with carrier is for composite is prepared.Every gram of adsorbent is mixed with 15~25 milliliters of aqueous solution of nitric acid.The carrier is coated with the macro-pore SiO of polymer for surface2.In aqueous solution of nitric acid, the concentration of nitric acid is 0.4~6.0 mol/L.The present invention is diluted or dissolves without using the diluent with property in adsorption process, and selectivity is good, and separating rate is fast, easy to operate, easy to spread.
Description
Technical field
The present invention relates to molybdenum element separation technology field, and in particular to a kind of method from water phase adsorbing separation molybdenum.
Background technology
Since Binding Forces Between Atoms are extremely strong, intensity is all very high at ambient and elevated temperatures for metal molybdenum.The coefficient of expansion of molybdenum is small, leads
Electric rate is big, good heat conductivity.Do not chemically reacted at normal temperatures with hydrochloric acid, hydrofluoric acid and aqueous slkali, be only soluble in nitric acid, chloroazotic acid
Or the concentrated sulfuric acid, to most of liquid metals, nonmetallic slag and melten glass also quite stable.Therefore, molybdenum and its alloy are in smelting
The important departments such as gold, agricultural, electric, chemical industry, environmental protection and aerospace have a wide range of applications and good prospect, become national economy
A kind of middle important raw material and irreplaceable strategic material.
Molybdenum -99 is one of radio isotope of molybdenum, and technetium -99 is used to prepare in hospital.Technetium -99 is that a kind of radioactivity is same
Position element, clothes for patients can be used for internal organs radiography after using.Molybdenum -99 for this kind of purposes stores after usually being absorbed with alumina powder
In relatively small container, technetium -99 are generated when molybdenum -99 decays, technetium -99 is taken out can from container issue disease when needed
People
Molybdenum in China aboundresources, explored 8,400,000 tons of molybdenum reserves, occupies second place of the world, and molybdenum product yield occupies generation
The 3rd, boundary, accounts for the 24~25% of World Molybdenum total output.Although China's Mo resource is quite abundant, cannot there is no sense of crisis, ore deposit
Production resource is non-renewable resources, is always had one day of exhaustion.Continuous with Mo resource application field expands, to molybdenum and its chemical combination
The demand of thing is also constantly increasing.Production development cannot be met by relying solely on extraction molybdenum and compound from natural crystal
Needs, and molybdenum is as a kind of limited resources, it is impossible to unconfined exploitation is carried out to it, so the recycling profit to Mo resource
With just there is important strategic importance.In recent years, comprehensive utilization and secondary resource of China's pay attention to day by day to the first resource of molybdenum
Recycling.
The regenerated resources of molybdenum are less, its source mainly passes through following three approach：
(1) in dead catalyst Mo resource recycling；
(2) recycling of the molybdenum in all kinds of metallurgical process molybdenum-containing waste slags；
(3) in metal product waste material molybdenum recycling.
The Chinese patent literature of Publication No. CN 103342769A discloses a kind of preparation method of the separation resin of molybdenum,
The separation resin of the molybdenum made from this method, its stable structure, during for extract and separate molybdenum, the fastness of extraction chromatography is preferable,
Substantially increase selectivity of the α-benzoinoxime to molybdenum.But the preparation method of the separation resin is more numerous and diverse, and the molybdenum is not separated
The selectivity of resin is studied, and can not realize and making choice property of molybdenum is separated from complex environment.
Nuclear power will not discharge since energy density is big, pollution is few and cause greenhouse gases and vigorously be sent out in recent years
Exhibition, but can be inevitably generated spentnuclear fuel among nuclear power operation.High activity liquid waste (HLLW) caused by spentnuclear fuel post processing,
It is a kind of peracidity, high radioactivity and highly toxic mixed solution, wherein containing a certain amount of molybdenum, if it is possible to molybdenum therein
Resource is separated, and is realized and is recycled, significant, still, at this stage in high activity liquid waste the separation of molybdenum element still in grinding
Study carefully the stage, do not find efficient recycling approach also.
The content of the invention
Easy to operate it is an object of the invention to provide a kind of method from water phase adsorbing separation molybdenum, selectivity is good, separation
It is efficient, it is easy to carry out industrial application.
A kind of method from water phase adsorbing separation molybdenum, includes the following steps：By adsorbent and contain various metals ion
Aqueous solution of nitric acid mixes, and the molybdenum acid ion in aqueous solution of nitric acid is adsorbed by adsorbent separation, and the adsorbent is by such as structural formula I
Shown compound with carrier is for composite is prepared：
Compound name as shown in structural formula I is：Double (5,6- dihexyl -1,2,4- triazine -3- the bases) -2,2'- of 6,6'-
Bipyridyl, referred to as：C6-BTBP.
In the present invention, the carrier is coated to the macro-pore SiO of polymer for surface2。
The surface is coated to the macro-pore SiO of polymer2For silicon substrate-styrene-divinylbenzene polymer (SiO2- P), be
A kind of novel inorganic/organic support material, silicon substrate-styrene-divinylbenzene polymerization is disclosed in United States Patent (USP) US6843921
Thing, SiO2- P is that one kind contains porous SiO2Organic high polymer complex carrier of particle, its preparation method are as follows：
(1) by the SiO of macropore2Washed, filtered with concentrated nitric acid, deionized water is washed till neutrality, repetition more than ten times, drying.
(2) vacuum and have under argon gas protective condition, with 1,2,3- trichloropropane and m- dimethylbenzene for solvent, to macro-pore SiO2
The m/p- formyl styrene of middle addition 48.7g, the m/p- divinylbenzenes of 8.9g, 72.2g dioctylphthalates,
54.0g benzoin methyl acid sodium, 0.56g α, α-idol bis-isobutyronitrile and 0.57g 1,1 '-idol dicyclohexyl amine -1- nitriles, by room temperature by
Step is heated to 90 DEG C, and keep 13 it is small when, afterwards, be progressively cooled to room temperature.
(3) washed respectively with acetone and methanol, filter above-mentioned product, repeated more than 10 times, it is dry.
In the present invention, the preparation method of the adsorbent is as follows：
Compound as shown in structural formula I is dissolved in organic solvent, carrier is added in resulting solution and is uniformly mixed,
After revolving removes organic solvent, adsorbent is obtained.
Preferably, every gram of compound as shown in structural formula I is dissolved in 100~200 milliliters of organic solvents.
The content of compound as shown in structural formula I will influence separating effect in adsorbent, when content is too low, the suction of adsorbent
Attached ability is weaker；During too high levels, the manufacturing cost of adsorbent will be increased.Preferably, compound is with carrying as shown in structural formula I
The mass ratio of body is 1：2~10.Further preferably, the mass ratio of compound and carrier as shown in structural formula I is 1：8~10.
The organic solvent is at least one of chloroform, dichloromethane, acetone and 1,2- dichloroethanes, is preferably chloroform
At least one of with dichloromethane.
During revolving, most of organic solvent is evaporated into closely dry state, under capillarity and physisorption, change
Adduct molecule enter carrier hole in, then the material of nearly dry state be dried in vacuo at 45~55 DEG C at least 24 it is small when,
Obtain adsorbent.
In order to ensure separating effect, it is preferable that every gram of adsorbent is mixed with 15~25 milliliters of aqueous solution of nitric acid.It is further excellent
Choosing, every gram of adsorbent are mixed with 20 milliliters of aqueous solution of nitric acid.
Adsorbent and aqueous solution of nitric acid mixing and absorption, adsorption temp is 298~318K, and adsorption time is 5~210min.Inhale
The time of contact of attached dose and aqueous solution will influence separating effect, and time of contact is too short, and absorption is not yet complete, and time of contact is long,
Reduce separative efficiency.Further preferably, adsorption temp 298K, adsorption time are 60~120min.
Adsorbent and aqueous solution of nitric acid mixing and absorption, mixing and absorption carry out under oscillating condition, oscillation rate for 120~
150rpm。
In aqueous solution of nitric acid, the concentration per metal ion species is 5.0 × 10-4~5.0 × 10-2Mol/L.Nitric acid is water-soluble
In liquid, the concentration of metal ion can influence separating effect, the excessive concentration of metal ion, it is possible to more than the absorption point of adsorbent
From ability；The concentration of metal ion is too low, then can reduce separative efficiency.Further preferably, the concentration per 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 influence separating effect, excellent
Selection of land, the concentration of nitric acid is 2.0~6.0 mol/Ls, and further preferably, the concentration of nitric acid is 2.0 mol/Ls.
Contain Mo (VI) and other metal ions in the 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)、Nd(Ⅲ)、Ru(Ⅲ)、Yb(Ⅲ)、Y
(III), at least one of Fe (III) and Zr (IV).
The present invention provides a kind of method from water phase adsorbing separation molybdenum, without using with particularity in adsorption process
The diluent of energy is diluted or dissolves, it is not necessary to other organic compounds are added, pollution is small, and selectivity is good, and separative efficiency is high,
It is easy to operate, it is easy to spread.
Brief description of the drawings
Fig. 1 is that the distribution coefficient of Separation of Molybdenum changes with concentration of nitric acid from aqueous solution of nitric acid using the adsorbent of embodiment 1
Graph of a relation；
Fig. 2 is the adsorbent pass that the distribution coefficient of Separation of Molybdenum varies with temperature from aqueous solution of nitric acid using embodiment 1
System's figure.
Embodiment
Embodiment 1
Double (5,6- dihexyl -1,2,4- triazine -3- the bases) -2,2'- bipyridyls of 0.5 gram of 6,6'- with structural formula I are molten
For solution in 60.0 milliliters of dichloromethane, fully dissolving obtains golden transparent solution；4.5 grams are added into this golden solution
SiO2- P is stirred evenly, and makes SiO2- P is uniformly mixed with compound, dichloromethane is largely evaporated into thing through depressurizing rotary evaporation
Expect closely dry state, organic molecule is entered SiO under capillarity and physisorption2In-P holes, then again will
The material of nearly dry state is dried in vacuo 24h at 55 DEG C, obtains C6-BTBP/SiO2- P composite materials, i.e. adsorbent.
Embodiment 2
Double (5,6- dihexyl -1,2,4- triazine -3- the bases) -2,2'- bipyridyls of 0.5 gram of 6,6'- with structural formula I are molten
For solution in 50.0 milliliters of dichloromethane, fully dissolving obtains golden transparent solution；4.0 grams are added into this golden solution
SiO2- P is stirred evenly, and makes SiO2- P is uniformly mixed with compound, dichloromethane is largely evaporated into thing through depressurizing rotary evaporation
Expect closely dry state, organic molecule is entered SiO under capillarity and physisorption2In-P holes, then again will
The material of nearly dry state is dried in vacuo 24h at 55 DEG C, obtains C6-BTBP/SiO2- P composite materials, i.e. adsorbent.
Embodiment 3
Double (5,6- dihexyl -1,2,4- triazine -3- the bases) -2,2'- bipyridyls of 0.5 gram of 6,6'- with structural formula I are molten
For solution in 75.0 milliliters of dichloromethane, fully dissolving obtains golden transparent solution；5.0 grams are added into this golden solution
SiO2- P is stirred evenly, and makes SiO2- P is uniformly mixed with compound, dichloromethane is largely evaporated into thing through depressurizing rotary evaporation
Expect closely dry state, organic molecule is entered SiO under capillarity and physisorption2In-P holes, then again will
The material of nearly dry state is dried in vacuo 24h at 55 DEG C, obtains C6-BTBP/SiO2- P composite materials, i.e. adsorbent.
Embodiment 4
Double (5,6- dihexyl -1,2,4- triazine -3- the bases) -2,2'- bipyridyls of 0.5 gram of 6,6'- with structural formula I are molten
For solution in 60.0 milliliters of chloroforms, fully dissolving obtains golden transparent solution；4.0 grams of SiO are added into this golden solution2-P
Stir evenly, make SiO2- P is uniformly mixed with compound, dichloromethane is largely evaporated into material through decompression rotary evaporation and is arrived
Closely dry state, makes organic molecule enter SiO under capillarity and physisorption2It is then nearly dry again in-P holes
The material of state is dried in vacuo 24h at 45 DEG C, obtains C6-BTBP/SiO2- P composite materials, i.e. adsorbent.
Embodiment 5~11
(1) by alkali nitrates LiNO3、NaNO3、KNO3、RbNO3、CsNO3；Alkaline earth 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；Noble metal Ru
Nitrate solution；Rare-earth oxide Y2O3, rare-earth metal nitrate La (NO3)3、Yb(NO3)3And Nd (NO3)3Deng plus
Enter concentrated nitric acid and deionized water is configured to the aqueous solution of nitric acid mother liquor that contains 17 metal ion species at the same time, in aqueous solution of nitric acid mother liquor
Concentration of nitric acid is 4.0 mol/Ls, and the concentration of each metal ion is 2.0~5.0 × 10-3Mol/L.
(2) concentrated nitric acid and deionized water are added in aqueous solution of nitric acid mother liquor, adjusts the concentration of nitric acid in aqueous solution of nitric acid,
Concentration of nitric acid is adjusted to 0.4,1.0,2.0,3.0,4.0,5.0 and 6.0 mol/Ls respectively, and the concentration per metal ion species is about
5.0×10-4Mol/L, occurrence are measured by ICP-OES or AA240.
(3) aqueous solution for 7 different concentration of nitric acid containing 17 kinds of metallic elements for obtaining step (2) respectively with implementation
Adsorbent contact mixing prepared by example 1, amount ratio during mixing are：0.15g adsorbents are corresponded to per 3.0mL aqueous solution of nitric acid；
(4) 7 mixed liquors obtained by step (3) are subjected to adsorption experiment on TAITEC MM-10 type oscillators, vibrated
The oscillation rate of device is 150rpm, is operated under room temperature 298K, adsorption time 120min, after absorption reaches balance, by solid-liquid
Two-phase is separated, phase of fetching water after separation, then measures the content of each metallic element in water phase respectively.
As shown in Figure 1, abscissa is concentration of nitric acid in Fig. 1, ordinate is the absorption result of embodiment 5~11 for distribution
Number.As seen from Figure 1, when concentration of nitric acid is 2.0 mol/L, the effect of separating element molybdenum is best, and the distribution coefficient of molybdenum reaches
It is less than 10 mls/g to 76.0 mls/g, and for the distribution coefficient of other 16 metal ion species, illustrates provided by the invention
Adsorbent is selectively strong to molybdenum, is suitable for that molybdenum is carried out from containing multiple metallic element water phase to efficiently separate recycling, using model
Enclose extremely wide.
Embodiment 12~16
Experiment condition and step are same as Example 9, and difference is, by aqueous solution of nitric acid, concentration of nitric acid is solid
It is set to 4.0 mol/Ls, adsorption time 120min, it is 298K, 303K, 308K, 313K and 318K to change adsorption temp successively,
For gained separating resulting as shown in Fig. 2, abscissa is adsorption temp in Fig. 2, ordinate is distribution coefficient.
As seen from Figure 2, as the increase of temperature, the material gradually reduce the adsorption capacity of molybdenum, temperature 298K
When, the distribution coefficient highest of molybdenum reaches 78.0 mls/g, and for other 16 metal ions distribution coefficient be less than 10 milliliters/
Gram, illustrate that adsorbent provided by the invention is selectively strong to molybdenum, be suitable for from containing multiple metallic element water phase carrying out molybdenum
Recycling is efficiently separated, application range is extremely wide.
Claims (9)
- A kind of 1. method from water phase adsorbing separation molybdenum, it is characterised in that include the following steps：By adsorbent and contain a variety of gold Belong to the aqueous solution of nitric acid mixing of ion, the molybdenum acid ion in aqueous solution of nitric acid is adsorbed by adsorbent separation, the adsorbent by Compound as shown in structural formula I with carrier is for composite is prepared：
- 2. as claimed in claim 1 from the method for water phase adsorbing separation molybdenum, it is characterised in that every gram of adsorbent and 15~25 millis Rise aqueous solution of nitric acid mixing.
- 3. as claimed in claim 1 from the method for water phase adsorbing separation molybdenum, it is characterised in that the carrier is coated to poly- for surface The macro-pore SiO of compound2。
- 4. as claimed in claim 1 from the method for water phase adsorbing separation molybdenum, it is characterised in that the preparation method of the adsorbent It is as follows：Compound as shown in structural formula I is dissolved in organic solvent, carrier is added and is uniformly mixed, is removed through revolving organic molten After agent, adsorbent is obtained.
- 5. as claimed in claim 4 from the method for water phase adsorbing separation molybdenum, it is characterised in that every gram of change as shown in structural formula I Compound is dissolved in 100~200 milliliters of organic solvents.
- 6. as claimed in claim 1 from the method for water phase adsorbing separation molybdenum, it is characterised in that the compound as shown in structural formula I Mass ratio with carrier is 1：2~10.
- 7. as claimed in claim 1 from the method for water phase adsorbing separation molybdenum, it is characterised in that in aqueous solution of nitric acid, Mei Zhongjin The concentration for belonging to ion is 5.0 × 10-4~5.0 × 10-2Mol/L.
- 8. as claimed in claim 1 from the method for water phase adsorbing separation molybdenum, it is characterised in that in aqueous solution of nitric acid, nitric acid Concentration is 0.4~6.0 mol/L.
- 9. as claimed in claim 1 from the method for water phase adsorbing separation molybdenum, it is characterised in that adsorbent is mixed with aqueous solution of nitric acid Absorption is closed, adsorption temp is 298~318K, and adsorption time is 5~210min.
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| CN109285616B (en) * | 2018-11-16 | 2020-08-21 | 中国原子能科学研究院 | From235Extraction from U fission products99Device for extracting Mo and extracting Mo by using device99Method for Mo |
| CN114717430B (en) * | 2022-04-19 | 2023-03-07 | 中国原子能科学研究院 | Method for extracting molybdenum from uranium fission products and ionic liquid system |
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