CN102836696A - Preparation method of magnetic nano solid-phase extracting agent for Pb2+ separation - Google Patents
Preparation method of magnetic nano solid-phase extracting agent for Pb2+ separation Download PDFInfo
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- CN102836696A CN102836696A CN2012103522926A CN201210352292A CN102836696A CN 102836696 A CN102836696 A CN 102836696A CN 2012103522926 A CN2012103522926 A CN 2012103522926A CN 201210352292 A CN201210352292 A CN 201210352292A CN 102836696 A CN102836696 A CN 102836696A
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Abstract
The invention relates to a preparation method of a magnetic nano solid-phase extracting agent for Pb2+ separation, which comprises the following steps of: taking Fe3O4 nano particles as a magnetic nucleus, taking the mixed liquid of deionized water and ethanol as a solvent, adding 25 percent of stronger ammonia water accounting for 5 percent of the fraction of the total volume, stirring at constant temperature in a reaction container after mixing evenly, dripping A after heating in a water bath for 30 minutes, adding B after reacting for 1 hour, heating up to 60 DEG C, cooling after refluxing for 1 hour, washing, adding into an ethanol solvent or a chloroform solvent after drying, then adding C and stirring at constant temperature of 40 DEG C for 12 to 24 hours; and washing so as to obtain the magnetic nano solid-phase extracting agent for the Pb2+ separation after drying at low temperature. The modifier A contains ester orthosilicate, the modifier B contains a silica coupling agent with chlorine functionalization, and the modifier C contains radicals. The magnetic nano solid-phase extracting agent prepared by the preparation method of the magnetic nano solid-phase extracting agent for the Pb2+ separation has large adsorption quantity, high rate, a simple process and low cost, is green, is friendly to the environment and is suitable for large-scale industrial production.
Description
Technical field
The present invention relates to a kind of Pb of being used for
2+The preparation method of the magnetic nano solid extracting agent that separates.Be used for from containing the waste water Adsorption of Heavy Metal Ions of heavy metal ion.
Background technology
The technology of the improvement effluent containing heavy metal ions of many various countries researchers exploitation has: 1. chemical precipitation method; 2. oxidation-reduction method; 3. air supporting method; 4. electrolytic reduction; 5. absorption method (biological absorption, resin adsorption, physical absorption); 6. evaporate and freezing method; 7. ion-exchange; 8. solvent extraction; 9. 10. magnetic separation method, ferrite process, nano-solid extractant method, magnetic nano-solid extractant method of liquid film, milipore filter, counter-infiltration, electroosmose process.Wherein the processing cost of method such as ion-exchange, film separation is higher, is prone to cause secondary pollution; Chemical precipitation method, absorption method etc. can only shift the position of heavy metal ion existence mostly or shift its physics and chemical form; And can not thoroughly remove heavy metal ion; And absorption is the heavy metal ion of multiple class; The still mixed solution that obtains behind the wash-out is to certain heavy metal ion (Pb particularly
2+) still difficulty relatively of recycling; When adopting the normal temperature ferrite process to handle effluent containing heavy metal ions; Heavy metal ion type in the waste water is bigger to the property effect of magnetic product; The radius of heavy metal ion is more near iron ion; The stability of the rate of recovery of metal, magnetic product and saturated magnetization rate thereof are high more in the gained magnetic product, and the absorption of other heavy metal ion is removed and then is restricted; Problems such as the method for magnetism separate method butt joint magnetic kind, the selection of magnetic kind and the recovery of magnetic kind are still waiting research and improve; Nano particle can all have adsorption capacity to good multiple ion simultaneously; But the majority that uses is non-magnetic nano particle, has increased the difficulty of the recovery of heavy metal ion so undoubtedly, and adopts hydrogen bond link or directly coating mostly; Thereby make the nanometer extractant unstable; Resistance to acids and bases is poor, and adsorbance is little, and reusability is poor; Though magnetic nanometer is used for the existing report of Adsorption of Heavy Metal Ions, mostly these adsorbents are nonspecific, and selectivity is relatively poor, and adsorbance is little, and this is unfavorable for (the Pb particularly of certain heavy metal ion in the waste water
2+) resource, and the recovery of magnetic nano solid extracting agent and activation utilize problem also to be in the immature stage again.
Summary of the invention
To the defective that exists in the prior art said method, the present invention discloses a kind of Pb of being used for
2+The preparation method of the magnetic nano solid extracting agent that separates, not only cost of material is cheap, technology is simple, and economic environmental protection, is easy to realize industrialization.
Technical scheme of the present invention is achieved in that
A kind of Pb that is used for
2+The preparation method of the magnetic nano solid extracting agent that separates is with Fe
3O
4Nano particle is a magnetic nuclear, superscribes the A dressing agent, and link B dressing agent links the C dressing agent again on the B dressing agent on the A dressing agent; Said A dressing agent is positive silicate class, the silica coupling agent of the chloride functionalization of B dressing agent, and the C dressing agent contains
Group is through washing, promptly get after the low temperature drying and be used for Pb
2+The magnetic nano solid extracting agent that separates.
Be used for Pb
2+The preparation method of the magnetic nano solid extracting agent that separates, concrete preparation process is following:
A) with 1-5gFe
3O
4Nano particle is a magnetic nuclear, and ethanol and deionized water mixed liquor are solvent, and the volume ratio of ethanol and deionized water is 4:1; The concentrated ammonia liquor of adding 25% accounts for 5% of total volume fraction; Mix and be placed in the condensing reflux reaction vessel constant temperature and stir water-bath heat temperature raising to 45 ℃, drip the A dressing agent after keeping constant temperature, account for the 1-5% of total volume fraction;
B) the stable back of system adds the B dressing agent, accounts for the 1-5% of total volume fraction; Then reactor is warming up to 60 ℃, after treating fully to react, stops heating, make reactor naturally cool to room temperature; With deionized water, absolute ethanol washing product;
C) be distributed to once more in alcohol solvent or the chloroform solvent after the above-mentioned product drying, add the C dressing agent again, account for Fe
3O
4The 10%-50% of nano particle quality mixes and is placed in the reaction vessel constant temperature and stirs the water-bath heating, and 40 ℃ of constant temperature stirred 12-24 hour, with absolute ethyl alcohol, water or chloroform, water washing, promptly gets after the low temperature drying and is used for Pb
2+The magnetic nano solid extracting agent that separates.
Described tri-iron tetroxide is a nano-scale particle or by its aggregate of forming, grain diameter is less than 5 μ m.
Advantage of the present invention and good effect are:
1, production cost of the present invention is low, and equipment and technology are simple, makes whole preparation system make up easily, is convenient to suitability for industrialized production.
2, be used for Pb
2+The magnetic nano solid extracting agent that separates is soft magnetism or paramagnetic particle, and grain diameter is less than 5 μ m, thereby can separate the magnetic nano solid extracting agent of saturated absorption fast, and separates the magnetic nano solid extracting after resolving fast.
3, the prepared magnetic nano adsorber of the present invention has three-decker, and this structure has improved the applicability of absorption.Than Fe
3O
4Nano particle directly superscribes the B dressing agent, and the B dressing agent chains C dressing agent synthetic extractant and Fe again
3O
4Nano particle directly superscribes the synthetic extractant of C dressing agent and has stability and antiacid alkali ability preferably, and the consumption of B dressing agent, C dressing agent is less greatly, thereby has improved atom utilization.
4, through modifications such as link selective extractants, realize Pb
2+Carry out selective absorption, and the rate of adsorption is fast, the present invention is than Fe
3O
4Nano particle directly superscribes the B dressing agent, and the B dressing agent chains C dressing agent synthetic extractant and Fe again
3O
4It is big that nano particle directly superscribes the synthetic extractant chemisorbed amount of C dressing agent, is easier to fast resolving.
5, utilize the technology of the leaded magnetic nano-solid extractant of the quick separation of high-intensity magnetic field simple, environmental protection.
6, lead ion can regenerate extractant from desorption on the magnetic nano solid extracting agent, and regeneration rate is very high, and the present invention is than Fe
3O
4Nano particle directly superscribes the B dressing agent, and the B dressing agent chains C dressing agent synthetic extractant and Fe again
3O
4Nano particle directly superscribes the synthetic extractant repeated use number of times of C dressing agent and improves greatly, production cost is reduced greatly, again environmental protection.
Description of drawings
Fig. 1: be used for Pb
2+The structural representation of the magnetic nano solid extracting agent that separates;
Fig. 2: be used for Pb
2+The infrared spectrogram of the magnetic nano solid extracting agent that separates:
Fig. 3: get embodiment 1 synthetic be used for Pb
2+The magnetic nano solid extracting agent 10mg that separates puts into the Pb of 20 μ g
2+In the solution, lead ion content concerns sketch map in adsorption time and the mother liquor;
Fig. 4: get the magnetic nano solid extracting agent 10mg that 1 embodiment 2 synthesizes, put into the Pb of 20 μ g
2+In the solution, lead ion content concerns sketch map in adsorption time and the mother liquor;
Fig. 5: get the magnetic nano solid extracting agent 10mg that embodiment 6 synthesizes, put into the Pb of 20 μ g
2+In the solution, lead ion content concerns sketch map in adsorption time and the mother liquor;
Fig. 6: get the magnetic nano solid extracting agent 10mg that is used for the Pb2+ separation that embodiment 1 synthesizes, put into 10mg/L (10mL – 80mL) Pb respectively
2+In the solution, adsorption time is 5min.Concern sketch map in the adsorption rate of magnetic nano solid extracting agent and the mother liquor between the lead ion addition;
Fig. 7: get embodiment 1 synthetic adsorb saturated magnetic nano solid extracting agent 10mg, be put in the salpeter solution of 3mol/L, the parsing time is 20s, concerns sketch map in parsing time and the solution between the plumbum ion concentration;
Fig. 8: get embodiment 2 synthetic adsorb saturated magnetic nano solid extracting agent 10mg, be put in the salpeter solution of 3mol/L, the parsing time is 0-20s, concerns sketch map in parsing time and the solution between the plumbum ion concentration;
Fig. 9: get embodiment 6 synthetic adsorb saturated magnetic nano solid extracting agent 10mg, be put in the salpeter solution of 3mol/L, the parsing time is 0-20s, concerns sketch map in parsing time and the solution between the plumbum ion concentration.
The specific embodiment
Below in conjunction with accompanying drawing and embodiment the present invention is elaborated.
Below be used for Pb
2+The preparation method's of the magnetic nano solid extracting agent that separates embodiment is with Fe
3O
4Nano particle is a magnetic nuclear, superscribes the A dressing agent, and link B dressing agent links the C dressing agent again on the B dressing agent on the A dressing agent, after washing, low temperature drying, promptly gets to be used for Pb
2+The magnetic nano solid extracting agent that separates.Said A dressing agent is positive silane tetra-ethyl ester or positive silane four butyl esters; The B dressing agent is the organic matter that contains cl radical; With γ-chloropropyl triethoxysilane is example; The C dressing agent contains
group, is example with the dithizone; Tri-iron tetroxide is a nano-scale particle or by its aggregate of forming, grain diameter is less than 5 μ m.
Instance one:
With 1gFe
3O
4Nano particle is a presoma, is solvent with deionized water and ethanol, and the volume ratio of ethanol and deionized water is 4:1, mixes back constant temperature in reaction vessel and stirs the water-bath heating, adds the NH of volume fraction 25% in the time of 30 ℃
3H
2O, 5%, the 45 ℃ of heated at constant temperature that accounts for total volume fraction drips the A---tetraethyl orthosilicate after 30 minutes; Account for 1% of total volume fraction, react adding B---γ-chloropropyl triethoxysilane after 1 hour, account for 1% of total volume fraction; Be warming up to 60 ℃ of backflows after 1 hour; Again add again in the chloroform solvent after cooling, the washing back drying, add then 0.1g C---dithizone, 40 ℃ of constant temperature stirred 12-24 hour; After washing, drying, promptly get and be used for Pb
2+The magnetic nano solid extracting agent that separates.The relation of lead ion content is seen Fig. 3 in the adsorption time of product and the mother liquor, and the rate of adsorption is fast, can be in 20-25 absorption fully in second; Relation in the maximal absorptive capacity of product and adsorption rate and the mother liquor between the plumbum ion concentration is seen Fig. 6, and adsorbance can reach 50.71mg/g, and 0-300 μ g adsorption rate is more than 90%; Relation in the resolution factor of adsorption production and parsing time and the solution between the plumbum ion concentration is seen Fig. 7,5 second resolution factor can reach 99%.
Instance two:
With 1gFe
3O
4Nano particle is a presoma, is solvent with deionized water and ethanol, and the volume ratio of ethanol and deionized water is 4:1, mixes back constant temperature in reaction vessel and stirs the water-bath heating, adds the NH of volume fraction 25% in the time of 30 ℃
3H
2O, 5%, the 45 ℃ of heated at constant temperature that accounts for total volume fraction drips A---silicic acid four butyl esters after 30 minutes; Account for 1% of total volume fraction, react adding B---γ-chloropropyl triethoxysilane after 1 hour, account for 2% of total volume fraction; Be warming up to 60 ℃ of backflows after 1 hour; Again add in the chloroform solvent after cooling, the washing again, add 0.2g C---dithizone, 40 ℃ of constant temperature stirred 12-24 hour; After washing, drying, promptly get and be used for Pb
2+The magnetic nano solid extracting agent that separates.The relation of lead ion content is seen Fig. 4 in the adsorption time of product and the mother liquor, and the rate of adsorption is fast, can be in 20-25 absorption fully in second; The maximal absorptive capacity of product reaches 68.58mg/g, and 0-600 μ g adsorption rate is more than 90%; Relation in the resolution factor of adsorption production and parsing time and the solution between the plumbum ion concentration is seen Fig. 8,5 second resolution factor can reach 99%.
Instance three:
With 1gFe
3O
4Nano particle is a presoma, is solvent with deionized water and ethanol, and the volume ratio of ethanol and deionized water is 4:1, mixes back constant temperature in reaction vessel and stirs the water-bath heating, adds the NH of volume fraction 25% in the time of 30 ℃
3H
2O, 5%, the 45 ℃ of heated at constant temperature that accounts for total volume fraction drips A---silicic acid four butyl esters after 30 minutes; Account for 1% of total volume fraction, react adding B---γ-chloropropyl triethoxysilane after 1 hour, account for 3% of total volume fraction; Be warming up to 60 ℃ of backflows after 1 hour; Again add in the chloroform solvent after cooling, the washing again, add 0.3g C---dithizone, 40 ℃ of constant temperature stirred 12-24 hour; After washing, drying, promptly get and be used for Pb
2+The magnetic nano solid extracting agent that separates.
Instance four:
With 1gFe
3O
4Nano particle is a presoma, is solvent with deionized water and ethanol, and the volume ratio of ethanol and deionized water is 4:1, mixes back constant temperature in reaction vessel and stirs the water-bath heating, adds the NH of volume fraction 25% in the time of 30 ℃
3H
2O, 5%, the 45 ℃ of heated at constant temperature that accounts for total volume fraction drips A---silicic acid four butyl esters after 30 minutes; Account for 1% of total volume fraction, react adding B---γ-chloropropyl triethoxysilane after 1 hour, account for 4% of total volume fraction; Be warming up to 60 ℃ of backflows after 1 hour; Again add in the chloroform solvent after cooling, the washing again, add 0.4g C---dithizone, 40 ℃ of constant temperature stirred 12-24 hour; After washing, drying, promptly get and be used for Pb
2+The magnetic nano solid extracting agent that separates.
Instance five:
With 1gFe
3O
4Nano particle is a presoma, is solvent with deionized water and ethanol, and the volume ratio of ethanol and deionized water is 4:1, mixes back constant temperature in reaction vessel and stirs the water-bath heating, adds the NH of volume fraction 25% in the time of 30 ℃
3H
2O, 5%, the 45 ℃ of heated at constant temperature that accounts for total volume fraction dripped A after 30 minutes; Account for 1% of total volume fraction, react adding B---γ-chloropropyl triethoxysilane after 1 hour, account for 5% of total volume fraction; Be warming up to 60 ℃ of backflows after 1 hour; Again add in the chloroform solvent after cooling, the washing again, add C---dithizone (0.5g), 40 ℃ of constant temperature stirred 12-24 hour; After washing, drying, promptly get and be used for Pb
2+The magnetic nano solid extracting agent that separates.
Instance six:
With 1gFe
3O
4Nano particle is a presoma, is solvent with deionized water and ethanol, and the volume ratio of ethanol and deionized water is 4:1, mixes back constant temperature in reaction vessel and stirs the water-bath heating, adds the NH of volume fraction 25% in the time of 30 ℃
3H
2O, 5%, the 45 ℃ of heated at constant temperature that accounts for total volume fraction drips the A---tetraethyl orthosilicate after 30 minutes; Account for 2% of total volume fraction, react adding B---γ-chloropropyl triethoxysilane after 1 hour, account for 2% of total volume fraction; Be warming up to 60 ℃ of backflows after 1 hour; Again add in the chloroform solvent after cooling, the washing again, add C---dithizone (0.2g), 40 ℃ of constant temperature stirred 12-24 hour; After washing, drying, promptly get and be used for Pb
2+The magnetic nano solid extracting agent that separates.The relation of lead ion content is seen Fig. 5 in the adsorption time of product and the mother liquor, and the rate of adsorption is fast, can in 20 seconds, adsorb fully; The maximal absorptive capacity of product reaches 61.86mg/g, and 0-500 μ g adsorption rate is more than 90%; Relation in the resolution factor of adsorption production and parsing time and the solution between the plumbum ion concentration is seen Fig. 9,5 second resolution factor can reach 100%.
Instance seven:
With 1gFe
3O
4Nano particle is a presoma, is solvent with deionized water and ethanol, and the volume ratio of ethanol and deionized water is 4:1, mixes back constant temperature in reaction vessel and stirs the water-bath heating, adds the NH of volume fraction 25% in the time of 30 ℃
3H
2O, 5%, the 45 ℃ of heated at constant temperature that accounts for total volume fraction drips the A---tetraethyl orthosilicate after 30 minutes; Account for 3% of total volume fraction, react adding B---γ-chloropropyl triethoxysilane after 1 hour, account for 3% of total volume fraction; Be warming up to 60 ℃ of backflows after 1 hour; Again add in the chloroform solvent after cooling, the washing again, add C---dithizone (0.3g), 40 ℃ of constant temperature stirred 12-24 hour; After washing, drying, promptly get and be used for Pb
2+The magnetic nano solid extracting agent that separates.
Instance eight:
With 1gFe
3O
4Nano particle is a presoma, is solvent with deionized water and ethanol, and the volume ratio of ethanol and deionized water is 4:1, mixes back constant temperature in reaction vessel and stirs the water-bath heating, adds the NH of volume fraction 25% in the time of 30 ℃
3H
2O, 5%, the 45 ℃ of heated at constant temperature that accounts for total volume fraction drips the A---tetraethyl orthosilicate after 30 minutes; Account for 5% of total volume fraction, react adding B---γ-chloropropyl triethoxysilane after 1 hour, account for 1% of total volume fraction; Be warming up to 60 ℃ of backflows after 1 hour; Again add in the chloroform solvent after cooling, the washing again, add C---dithizone (0.1g), 40 ℃ of constant temperature stirred 12-24 hour; After washing, drying, promptly get and be used for Pb
2+The magnetic nano solid extracting agent that separates.
Instance nine:
With 1gFe
3O
4Nano particle is a presoma, is solvent with deionized water and ethanol, and the volume ratio of ethanol and deionized water is 4:1, mixes back constant temperature in reaction vessel and stirs the water-bath heating, adds the NH of volume fraction 25% in the time of 30 ℃
3H
2O, 5%, the 45 ℃ of heated at constant temperature that accounts for total volume fraction drips the A---tetraethyl orthosilicate after 30 minutes; Account for 5% of total volume fraction, react adding B---γ-chloropropyl triethoxysilane after 1 hour, account for 2% of total volume fraction; Be warming up to 60 ℃ of backflows after 1 hour; Again add in the chloroform solvent after cooling, the washing again, add C---dithizone (0.2g), 40 ℃ of constant temperature stirred 12-24 hour; After washing, drying, promptly get and be used for Pb
2+The magnetic nano solid extracting agent that separates.
Instance ten:
With 1gFe
3O
4Nano particle is a presoma, is solvent with deionized water and ethanol, and the volume ratio of ethanol and deionized water is 4:1, mixes back constant temperature in reaction vessel and stirs the water-bath heating, adds the NH of volume fraction 25% in the time of 30 ℃
3H
2O, 5%, the 45 ℃ of heated at constant temperature that accounts for total volume fraction drips the A---tetraethyl orthosilicate after 30 minutes; Account for 5% of total volume fraction, react adding B---γ-chloropropyl triethoxysilane after 1 hour, account for 3% of total volume fraction; Be warming up to 60 ℃ of backflows after 1 hour; Again add in the chloroform solvent after cooling, the washing again, add C---dithizone (0.3g), 40 ℃ of constant temperature stirred 12-24 hour; After washing, drying, promptly get and be used for Pb
2+The magnetic nano solid extracting agent that separates.
Instance 11:
With 1gFe
3O
4Nano particle is a presoma, is solvent with deionized water and ethanol, and the volume ratio of ethanol and deionized water is 4:1, mixes back constant temperature in reaction vessel and stirs the water-bath heating, adds the NH of volume fraction 25% in the time of 30 ℃
3H
2O, 5%, the 45 ℃ of heated at constant temperature that accounts for total volume fraction drips the A---tetraethyl orthosilicate after 30 minutes; Account for 5% of total volume fraction, react adding B---γ-chloropropyl triethoxysilane after 1 hour, account for 4% of total volume fraction; Be warming up to 60 ℃ of backflows after 1 hour; Again add in the chloroform solvent after cooling, the washing again, add C---dithizone (0.4g), 40 ℃ of constant temperature stirred 12-24 hour; After washing, drying, promptly get and be used for Pb
2+The magnetic nano solid extracting agent that separates.
Instance 12:
With 1gFe
3O
4Nano particle is a presoma, is solvent with deionized water and ethanol, and the volume ratio of ethanol and deionized water is 4:1, mixes back constant temperature in reaction vessel and stirs the water-bath heating, adds the NH of volume fraction 25% in the time of 30 ℃
3H
2O, 5%, the 45 ℃ of heated at constant temperature that accounts for total volume fraction drips the A---tetraethyl orthosilicate after 30 minutes; Account for 5% of total volume fraction, react adding B---γ-chloropropyl triethoxysilane after 1 hour, account for 5% of total volume fraction; Be warming up to 60 ℃ of backflows after 1 hour; Again add in the chloroform solvent after cooling, the washing again, add C---dithizone (0.5g), 40 ℃ of constant temperature stirred 12-24 hour; After washing, drying, promptly get and be used for Pb
2+The magnetic nano solid extracting agent that separates.
Instance 13:
With 1gFe
3O
4Nano particle is a presoma, is solvent with deionized water and ethanol, and the volume ratio of ethanol and deionized water is 4:1, mixes back constant temperature in reaction vessel and stirs the water-bath heating, adds the NH of volume fraction 25% in the time of 30 ℃
3H
2O, 5%, the 45 ℃ of heated at constant temperature that accounts for total volume fraction drips the A---tetraethyl orthosilicate after 30 minutes; Account for 1% of total volume fraction, react adding B---γ-chloropropyl triethoxysilane after 1 hour, account for 1% of total volume fraction; Be warming up to 60 ℃ of backflows after 1 hour; Again add in the alcohol solvent after cooling, the washing again, add C---dithizone (0.1g), 40 ℃ of constant temperature stirred 12-24 hour; After washing, drying, promptly get and be used for Pb
2+The magnetic nano solid extracting agent that separates.
Instance 14:
With 1gFe
3O
4Nano particle is a presoma, is solvent with deionized water and ethanol, and the volume ratio of ethanol and deionized water is 4:1, mixes back constant temperature in reaction vessel and stirs the water-bath heating, adds the NH of volume fraction 25% in the time of 30 ℃
3H
2O, 5%, the 45 ℃ of heated at constant temperature that accounts for total volume fraction drips the A---tetraethyl orthosilicate after 30 minutes; Account for 1% of total volume fraction, react adding B---γ-chloropropyl triethoxysilane after 1 hour, account for 2% of total volume fraction; Be warming up to 60 ℃ of backflows after 1 hour; Again add in the alcohol solvent after cooling, the washing again, add C---dithizone (0.1g), 40 ℃ of constant temperature stirred 12-24 hour; After washing, drying, promptly get and be used for Pb
2+The magnetic nano solid extracting agent that separates.
Claims (3)
1. one kind is used for Pb
2+The preparation method of the magnetic nano solid extracting agent that separates is characterized in that: with Fe
3O
4Nano particle is a magnetic nuclear, superscribes the A dressing agent, and link B dressing agent links the C dressing agent again on the B dressing agent on the A dressing agent; Promptly get after washing, the low temperature drying then and be used for Pb
2+The magnetic nano solid extracting agent that separates; Said A dressing agent contains positive silicate class, the silica coupling agent of the chloride functionalization of B dressing agent, and the C dressing agent contains
Group.
2. the Pb that is used for according to claim 1
2+The preparation method of the magnetic nano solid extracting agent that separates is characterized in that: concrete preparation process is following:
A) with 1-5gFe
3O
4Nano particle is a magnetic nuclear, and ethanol and deionized water mixed liquor are solvent, and the volume ratio of ethanol and deionized water is 4:1; The concentrated ammonia liquor of adding 25% accounts for 5% of total volume fraction; Mix and be placed in the condensing reflux reaction vessel constant temperature and stir water-bath heat temperature raising to 45 ℃, drip the A dressing agent after keeping constant temperature, account for the 1-5% of total volume fraction;
B) the stable back of system adds the B dressing agent, accounts for the 1-5% of total volume fraction; Then reactor is warming up to 60 ℃, after treating fully to react, stops heating, make reactor naturally cool to room temperature; With deionized water, absolute ethanol washing product;
C) be distributed to once more in alcohol solvent or the chloroform solvent after the above-mentioned product drying, add the C dressing agent again, account for Fe
3O
4The 10%-50% of nano particle quality mixes and is placed in the reaction vessel constant temperature and stirs the water-bath heating, and 40 ℃ of constant temperature stirred 12-24 hour, with absolute ethyl alcohol, water or chloroform, water washing, promptly gets after the low temperature drying and is used for Pb
2+The magnetic nano solid extracting agent that separates.
3. a kind of Pb that is used for according to claim 1
2+The preparation method of the magnetic nano solid extracting agent that separates is characterized in that: described tri-iron tetroxide is a nano-scale particle or by its aggregate of forming, grain diameter is less than 5 μ m.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104787861A (en) * | 2015-04-23 | 2015-07-22 | 中国科学技术大学 | Electric extraction process for simultaneously and efficiently extracting and recycling metal elements and functional organic compounds |
| CN106268651A (en) * | 2016-08-26 | 2017-01-04 | 云南贵悦金属材料科技有限公司 | Nano SiO 2 particle for adsorbing separation platinum and its preparation method and application |
| CN110961086A (en) * | 2019-12-15 | 2020-04-07 | 江西理工大学 | Extractant functionalized magnetic nano-adsorption material, preparation method and application |
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