CN106622108A - Preparation method of double-shell phosphonyl modified silica magnetic microsphere for extracting uranium from brine - Google Patents
Preparation method of double-shell phosphonyl modified silica magnetic microsphere for extracting uranium from brine Download PDFInfo
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- CN106622108A CN106622108A CN201611158400.0A CN201611158400A CN106622108A CN 106622108 A CN106622108 A CN 106622108A CN 201611158400 A CN201611158400 A CN 201611158400A CN 106622108 A CN106622108 A CN 106622108A
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- C22B60/00—Obtaining metals of atomic number 87 or higher, i.e. radioactive metals
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Abstract
The invention discloses a preparation method of a double-shell phosphonyl modified silica magnetic microsphere for extracting uranium from brine. An inner shell of the double-shell phosphonyl modified silica magnetic microsphere is a compact silica layer and is used for coating a magnetic substance Fe3O4 in a core, so that dissolution of Fe3O4 during a using process is avoided; an outer shell of the double-shell phosphonyl modified silica magnetic microsphere is a phosphonyl modified silica layer having a developed and ordered mesoporous structure, so that the uranium can conveniently enter a hole for adsorption. The preparation method of the double-shell phosphonyl modified silica magnetic microsphere comprises the following steps: firstly coating the compact silica layer on the surfaces of magnetic Fe3O4 nanoparticles, then further coating a porous phosphonyl functionalized silica layer, and finally removing a template agent (P123) through reflux extraction, thus obtaining the double-shell phosphonyl modified silica magnetic microsphere. The double-shell phosphonyl modified silica magnetic microsphere disclosed by the invention can be used as an adsorbent, and can be used for realizing high-efficiency uranium extraction from the brine through adsorption by taking salt making brine in sea salt production as a raw material.
Description
Technical field
The present invention relates to a kind of bivalve layer phosphono for carrying uranium for bittern modifies the preparation side of silicone dioxide magnetic microsphere
Method, belongs to inorganic functional material field.
Background technology
Salt production salt manufacturing bittern is regarded as concentrated seawater, and it contains uranium concentration far above seawater, up to hundreds of μ g/L；And
Separate out partial salts (such as NaCl) in evaporating concentration process, be conducive to uranium absorption, therefore, these bittern are also important uranium
Resource, needs further exploitation, and carrying the bittern after uranium can be comprehensively utilized using existing salt chemical engineering technology.But due to halogen
Salinity water is high, and uranyl ion existing forms are complicated, and there are a large amount of interfering ions (such as Na+、K+、Mg2+Deng).Common adsorbents
(such as ion exchange resin, activated carbon, clay and natural sorbing material) due to chemical stability and bad mechanical strength, or by
It is relatively low in adsorptive selectivity and cost performance, it is difficult to be applied to bittern and carry uranium.Silicone dioxide magnetic microsphere with core shell structure is not
Only there is good chemical stability and mechanical strength, and specific surface area is high, be easy to modification, its prosperity it is order mesoporous
Structure is conducive to uranium to rapidly enter absorption in hole, therefore is preferable uranium absorption material；And silicone dioxide magnetic microsphere is utilized
Externally-applied magnetic field is easily isolated, and efficiently solves adsorbent and separates difficult problem.But the magnetic in silicone dioxide magnetic microsphere
Material (such as ferroso-ferric oxide) is easy to dissolution in actual adsorption uranium, additionally, silicone dioxide magnetic microsphere carries out bittern when carrying uranium
It is generally relatively low to the adsorption capacity and adsorptive selectivity of uranium.Therefore, the magnetisable material in silicone dioxide magnetic microsphere how is avoided
Dissolution when in use, and adsorption capacity and adsorptive selectivity of the silicone dioxide magnetic microsphere to uranium how is improved, it is to utilize two
Silicon oxide magnetic microspheres carry out bittern and put forward the problem that uranium must be solved.
The content of the invention
It is an object of the invention to provide a kind of bivalve layer phosphono modifies silicone dioxide magnetic microsphere, in the magnetic microsphere
Shell is fine and close silicon dioxide layer, for coating kernel magnetisable material ferroso-ferric oxide, it is to avoid four oxidation three during use
Iron dissolution；Outer shell is the modification silicon dioxide layer of the phosphono with flourishing ordered mesopore structure, is easy to uranium to enter duct interior suction
It is attached.The silicone dioxide magnetic microsphere can be as adsorbent, for Salt production salt manufacturing bittern as raw material, being realized by absorption high
Effect bittern carries uranium.
In order to solve the problems, such as that carrying out magnetisable material when bittern carries uranium using silicone dioxide magnetic microsphere is easy to dissolution, and
Adsorption capacity and adsorptive selectivity of the silicone dioxide magnetic microsphere to uranium is improved, the present invention provides a kind of bivalve layer phosphono modification
The preparation method of silicone dioxide magnetic microsphere, carries out bittern and carries uranium tool using bivalve layer phosphono modification silicone dioxide magnetic microsphere
Have the rate of adsorption fast, adsorption capacity is high, the good advantage of adsorptive selectivity, and the magnetic microsphere have good chemical stability,
Mechanical strength and uranium absorption performance, it is easy to Magneto separate；There are good adsorptive selectivity and higher absorption to hold to U in bittern (VI)
Amount.Adsorbent is reusable repeatedly, magnetisable material (Fe3O4) dissolution rate be less than 5%.The present invention is provided with Salt production salt manufacturing
Bittern is raw material, realizes that bittern efficiently carries the adsorbent of uranium by absorption method.
The invention solves the problems that the problems referred to above, the technical scheme for being adopted is：
A kind of bivalve layer phosphono modification silicone dioxide magnetic microsphere that uranium is carried for bittern, the magnetic microsphere is easy to magnetic point
From its hypostracum is fine and close silicon dioxide layer, for coating kernel magnetisable material ferroso-ferric oxide, it is to avoid four in adsorption process
Fe 3 O is aoxidized or dissolution；Outer shell is the modification silicon dioxide layer of the phosphono with flourishing ordered mesopore structure, is easy to uranium
It is attached into duct interior suction, at the same silicone dioxide magnetic microsphere can be significantly improved to the adsorption capacity of uranium by phosphono modification and
Adsorptive selectivity.
A kind of bivalve layer phosphono for carrying uranium for bittern modifies the preparation method of silicone dioxide magnetic microsphere, including：First
In magnetic Fe3O4Nanoparticle surface bag carries out fine and close silicon dioxide layer, and further bag carries out porous phosphoryl functionalization titanium dioxide
Silicon layer, most after Jing reflux extractions slough template (P123), obtain bivalve layer phosphono modified magnetic silicone dioxide magnetic microsphere.
A kind of bivalve layer phosphono for carrying uranium for bittern modifies the preparation method of silicone dioxide magnetic microsphere, concrete steps
For：
(1) silicone dioxide magnetic microsphere of individual layer bag shoe is prepared, Fe is labeled as3O4@SiO2
0.1g nanometer Fes3O4In adding to 50mL absolute ethyl alcohols, 25mL deionized waters, 1.5mL ammonia water mixtures, ultrasonic disperse
Uniformly, 0.1g tetraethyl orthosilicates are added, 5～10h of heating using microwave stirring reaction at 80 DEG C is centrifuged obtaining solid product
Afterwards, solid product deionized water is fully washed, and silicone dioxide magnetic microsphere is obtained after 60 DEG C of dryings；
(2) bivalve layer phosphono modified magnetic silicon dioxide microsphere is prepared
Add in the mixed liquor of the pore template of 60mL absolute ethyl alcohols, 80mL deionized waters, 1.5mL ammoniacal liquor and 1.5mL
Enter 0.2g Fe3O4@SiO2, ultrasonic disperse 30min, add tetraethyl orthosilicate 0.2g and phosphono functionalized reagent 0.01～
0.04g, gained mixture is placed in reactor, the stir about 1h at 40 DEG C, then microwave hydrothermal processes 6h, magnetic at being warming up to 80 DEG C
Deionized water and ethanol are fully washed after isolated solid product, and the product after washing is scattered in 100mL acidity second again
In alcoholic solution, flow back 12h at 60 DEG C, and to remove pore template, then Magneto separate products therefrom, deionized water and ethanol are abundant
After washing, it is vacuum dried at 70 DEG C, then the screened bivalve layer phosphono modified magnetic dioxy for obtaining particle diameter for 90-200 microns
SiClx magnetic microsphere.
Described pore template is PEO-PPOX-PEO triblock copolymer, referred to as
P123。
Described phosphono functionalized reagent and the mass ratio of tetraethyl orthosilicate is 5～20%.
Described phosphono functionalized reagent be diethyl phosphonyl triethoxysilane, abbreviation DPTS.
Described tetraethyl orthosilicate abbreviation TEOS.
It is an advantage of the current invention that：
1st, bittern is carried out using bivalve layer phosphono modification silicone dioxide magnetic microsphere and carries uranium have the rate of adsorption fast, absorption
Capacity is high, the good advantage of adsorptive selectivity, and the magnetic microsphere has good chemical stability, mechanical strength and uranium absorption
Can, it is easy to Magneto separate；There are good adsorptive selectivity and higher adsorption capacity to U in bittern (VI).Adsorbent is repeatable to be made
With multiple, magnetisable material (Fe3O4) dissolution rate be less than 5%.The present invention is provided with Salt production salt manufacturing bittern as raw material, by inhaling
Attached method realizes that bittern efficiently carries the adsorbent of uranium.
2nd, by adjusting phosphono functionalized reagent addition, that is, control DPTS/TEOS mass ratioes be respectively 5%, 10%,
When 15% and 20%, phosphono functional group content point in the layer phosphono modified magnetic silicone dioxide magnetic microsphere adsorbent of bivalve
Wei 0.78,1.05,1.38 and 1.56mmol/g.The adsorbent can be used for from sea salt to uranium absorption capacity upto 106mg/g
Production salt manufacturing bittern carries uranium, and time of equilibrium adsorption is less than 60min, and U (VI) can be realized with coexisting ion (K in bittern+、Na+、Mg2 +、Ca2+、Cl-And SO4 2-Deng) Selective Separation.Optimal adsorption condition is：Adsorption temp 298K, Optimal pH 6-7, adsorbent is used
Amount 0.4g/L, DPTS/TEOS mass ratioes 15%.
Description of the drawings
Fig. 1 is the preparation method schematic diagram of bivalve layer phosphono modified magnetic silicone dioxide magnetic microsphere.
Specific embodiment：
Technical scheme is further described with reference to specific embodiment.
Embodiment 1：
(1) silicone dioxide magnetic microsphere (Fe of individual layer bag shoe is prepared3O4@SiO2)
0.1g nanometer Fes3O4In adding to 50mL absolute ethyl alcohols, 25mL deionized waters, 1.5mL ammonia water mixtures, ultrasonic disperse
Uniformly.0.1g tetraethyl orthosilicates are added, 5～10h of heating using microwave stirring reaction at 80 DEG C is centrifuged obtaining solid product
Afterwards, solid product deionized water is fully washed, and silicone dioxide magnetic microsphere is obtained after 60 DEG C of dryings.
(2) bivalve layer phosphono modified magnetic silicon dioxide microsphere is prepared
In 60mL absolute ethyl alcohols, 80mL deionized waters, 1.5mL ammoniacal liquor and 1.5mL pore template (PEO-
PPOX-PEO triblock copolymer, P123) 0.2g Fe are added in mixed liquor3O4@SiO2, ultrasonic disperse
30min, then add tetraethyl orthosilicate (TEOS) 0.2g and phosphono functionalized reagent (diethyl by DPTS/TEOS mass ratioes 5%
Phosphono triethoxysilane, DPTS) 0.01g, gained mixture is placed in reactor, the stir about 1h at 40 DEG C, then heated up
Microwave hydrothermal processes 6h at 80 DEG C, and Magneto separate obtains fully being washed after solid product, and the product after washing is scattered in again
In 100mL acid ethanol solutions, flow back 12h at 60 DEG C, to remove template (P123).Magneto separate products therefrom again, spend from
After sub- water and ethanol are fully washed, it is vacuum dried at 70 DEG C, then the screened bivalve layer phosphono for obtaining particle diameter for 90-200 microns
Base modified magnetic silicone dioxide magnetic microsphere adsorbent.
The bivalve layer phosphono modified magnetic silicone dioxide magnetic microsphere adsorbent to uranium absorption capacity upto 64mg/g,
Can be used to carry uranium from Salt production salt manufacturing bittern, time of equilibrium adsorption is less than 60min, can realize being coexisted in U (VI) and bittern from
Son (K+、Na+、Mg2+、Ca2+、Cl-And SO4 2-Deng) Selective Separation.Adsorbent is reusable more than 5 times, magnetisable material
(Fe3O4) dissolution rate be less than 5%.
Embodiment 2：
Prepare bivalve layer phosphono modified magnetic silicon dioxide microsphere
In 60mL absolute ethyl alcohols, 80mL deionized waters, 1.5mL ammoniacal liquor and 1.5mL pore template (PEO-
PPOX-PEO triblock copolymer, P123) 0.2g Fe are added in mixed liquor3O4@SiO2, ultrasonic disperse
30min.DPTS/TEOS mass ratioes 10% are pressed again adds tetraethyl orthosilicate (TEOS) 0.2g and phosphono functionalized reagent (diethyl
Base phosphono triethoxysilane, DPTS) 0.02g, gained mixture is placed in reactor, the stir about 1h at 40 DEG C, then risen
Temperature to microwave hydrothermal at 80 DEG C processes 6h, and Magneto separate obtains fully being washed after solid product, and the product after washing is scattered in again
In 100mL acid ethanol solutions, flow back 12h at 60 DEG C, to remove template (P123).Magneto separate products therefrom again, spend from
After sub- water and ethanol are fully washed, it is vacuum dried at 70 DEG C, then the screened bivalve layer phosphono for obtaining particle diameter for 90-200 microns
Base modified magnetic silicone dioxide magnetic microsphere.
Remaining is with embodiment 1.
The bivalve layer phosphono modified magnetic silicone dioxide magnetic microsphere adsorbent to uranium absorption capacity upto 87mg/g,
Can be used to carry uranium from Salt production salt manufacturing bittern, time of equilibrium adsorption is less than 60min, can realize being coexisted in U (VI) and bittern from
Son (K+、Na+、Mg2+、Ca2+、Cl-And SO4 2-Deng) Selective Separation.Adsorbent is reusable more than 5 times, magnetisable material
(Fe3O4) dissolution rate be less than 5%.
Embodiment 3：
Prepare bivalve layer phosphono modified magnetic silicon dioxide microsphere
In 60mL absolute ethyl alcohols, 80mL deionized waters, 1.5mL ammoniacal liquor and 1.5mL pore template (PEO-
PPOX-PEO triblock copolymer, P123) 0.2g Fe are added in mixed liquor3O4@SiO2, ultrasonic disperse
30min.DPTS/TEOS mass ratioes 15% are pressed again adds tetraethyl orthosilicate (TEOS) 0.2g and phosphono functionalized reagent (diethyl
Base phosphono triethoxysilane, DPTS) 0.03g, gained mixture is placed in reactor, the stir about 1h at 40 DEG C, then risen
Temperature to microwave hydrothermal at 80 DEG C processes 6h, and Magneto separate obtains fully being washed after solid product.Product after washing is scattered in again
In 100mL acid ethanol solutions, flow back 12h at 60 DEG C, to remove template (P123).Magneto separate products therefrom again, spend from
After sub- water and ethanol are fully washed, it is vacuum dried at 70 DEG C, then the screened bivalve layer phosphono for obtaining particle diameter for 90-200 microns
Base modified magnetic silicone dioxide magnetic microsphere.
Remaining is with embodiment 1.
The bivalve layer phosphono modified magnetic silicone dioxide magnetic microsphere adsorbent is to uranium absorption capacity upto 106mg/
G, can be used to carry uranium from Salt production salt manufacturing bittern, and time of equilibrium adsorption is less than 60min, can realize being coexisted in U (VI) and bittern
Ion (K+、Na+、Mg2+、Ca2+、Cl-And SO4 2-Deng) Selective Separation.Adsorbent is reusable more than 5 times, magnetisable material
(Fe3O4) dissolution rate be less than 5%.
Embodiment 4：
Prepare bivalve layer phosphono modified magnetic silicon dioxide microsphere
In 60mL absolute ethyl alcohols, 80mL deionized waters, 1.5mL ammoniacal liquor and 1.5mL pore template (PEO-
PPOX-PEO triblock copolymer, P123) 0.2g Fe are added in mixed liquor3O4@SiO2, ultrasonic disperse
30min.DPTS/TEOS mass ratioes 20% are pressed again adds tetraethyl orthosilicate (TEOS) 0.2g and phosphono functionalized reagent (diethyl
Base phosphono triethoxysilane, DPTS) 0.04g, gained mixture is placed in reactor, the stir about 1h at 40 DEG C, then risen
Temperature to microwave hydrothermal at 80 DEG C processes 6h, and Magneto separate obtains fully being washed after solid product.Product after washing is scattered in again
In 100mL acid ethanol solutions, flow back 12h at 60 DEG C, to remove template (P123).Magneto separate products therefrom again, spend from
After sub- water and ethanol are fully washed, it is vacuum dried at 70 DEG C, then the screened bivalve layer phosphono for obtaining particle diameter for 90-200 microns
Base modified magnetic silicone dioxide magnetic microsphere.
Remaining is with embodiment 1.
The bivalve layer phosphono modified magnetic silicone dioxide magnetic microsphere adsorbent to uranium absorption capacity upto 93mg/g,
Can be used to carry uranium from Salt production salt manufacturing bittern, time of equilibrium adsorption is less than 60min, can realize being coexisted in U (VI) and bittern from
Son (K+、Na+、Mg2+、Ca2+、Cl-And SO4 2-Deng) Selective Separation.Adsorbent is reusable more than 5 times, magnetisable material
(Fe3O4) dissolution rate be less than 5%.
Claims (6)
1. a kind of bivalve layer phosphono for carrying uranium for bittern modifies silicone dioxide magnetic microsphere, it is characterized by：The magnetic microsphere
It is easy to Magneto separate, its hypostracum is fine and close silicon dioxide layer, for coating kernel magnetisable material ferroso-ferric oxide, it is to avoid absorption
During ferroso-ferric oxide oxidation or dissolution；Outer shell is the modification silica of the phosphono with flourishing ordered mesopore structure
Layer, is easy to uranium attached into duct interior suction, while can significantly improve silicone dioxide magnetic microsphere to uranium by phosphono modification
Adsorption capacity and adsorptive selectivity.
2. a kind of bivalve layer phosphono for carrying uranium for bittern as claimed in claim 1 modifies silicone dioxide magnetic microsphere, its
It is characterized as：Preparation method includes：First in magnetic Fe3O4Nanoparticle surface bag carries out fine and close silicon dioxide layer, and further bag is carried out
Porous phosphoryl functionalized SiO 2 layer, most after Jing reflux extractions slough pore template, obtain the modification of bivalve layer phosphono
Magnetic silica magnetic microsphere.
3. a kind of bivalve layer phosphono for carrying uranium for bittern modifies the preparation method of silicone dioxide magnetic microsphere, it is characterized by：
Concretely comprise the following steps：
(1) silicone dioxide magnetic microsphere of individual layer bag shoe is prepared, Fe is labeled as3O4@SiO2
0.1g nanometer Fes3O4In adding to 50mL absolute ethyl alcohols, 25mL deionized waters, 1.5mL ammonia water mixtures, ultrasonic disperse is uniform,
0.1g tetraethyl orthosilicates are added, 5～10h of heating using microwave stirring reaction at 80 DEG C is centrifuged obtaining after solid product, Gu
Phase product deionized water is fully washed, and silicone dioxide magnetic microsphere is obtained after 60 DEG C of dryings；
(2) bivalve layer phosphono modified magnetic silicon dioxide microsphere is prepared
Add in the mixed liquor of the pore template of 60mL absolute ethyl alcohols, 80mL deionized waters, 1.5mL ammoniacal liquor and 1.5mL
0.2g Fe3O4@SiO2, ultrasonic disperse 30min, add tetraethyl orthosilicate 0.2g and phosphono functionalized reagent 0.01～
0.04g, obtains mixture and is placed in reactor, the stir about 1h at 40 DEG C, then microwave hydrothermal processes 6h, magnetic point at being warming up to 80 DEG C
Fully wash from deionized water and ethanol after solid product is obtained, the product after washing is scattered in 100mL acidic ethanols again
In solution, flow back 12h at 60 DEG C, and to remove pore template, then Magneto separate products therefrom, deionized water and ethanol are fully washed
After washing, it is vacuum dried at 70 DEG C, then the screened bivalve layer phosphono modified magnetic titanium dioxide for obtaining particle diameter for 90-200 microns
Silicon magnetic microsphere.
4. a kind of bivalve layer phosphono for carrying uranium for bittern as claimed in claim 3 modifies the system of silicone dioxide magnetic microsphere
Preparation Method, it is characterized by：Described pore template is PEO-PPOX-PEO triblock copolymer
Thing, abbreviation P123.
5. a kind of bivalve layer phosphono for carrying uranium for bittern as claimed in claim 3 modifies the system of silicone dioxide magnetic microsphere
Preparation Method, it is characterized by：Described phosphono functionalized reagent and the mass ratio of tetraethyl orthosilicate is 5～20%.
6. a kind of bivalve layer phosphono for carrying uranium for bittern as claimed in claim 3 modifies the system of silicone dioxide magnetic microsphere
Preparation Method, it is characterized by：Described phosphono functionalized reagent be diethyl phosphonyl triethoxysilane, abbreviation DPTS.
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| CN108525648A (en) * | 2018-04-09 | 2018-09-14 | 东华理工大学 | A kind of method of amination magnetism poly phosphazene adsorbent and preparation and separation and enriched uranium |
| CN108745306A (en) * | 2018-06-27 | 2018-11-06 | 东华理工大学 | A kind of preparation method of epoxychloropropane cross-linked chitosan/aminated carbon nano tube composite aerogel |
| CN109317117A (en) * | 2018-09-26 | 2019-02-12 | 中国工程物理研究院核物理与化学研究所 | A kind of magnetic adsorbent and its preparation and the processing method to Actinides |
| CN114870759A (en) * | 2022-05-12 | 2022-08-09 | 中国科学院苏州生物医学工程技术研究所 | Preparation method of raspberry-shaped silicon hydroxyl magnetic microspheres |
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