CN103230779A - Preparation method for nanometer sphere capable of absorbing heavy metal ions - Google Patents
Preparation method for nanometer sphere capable of absorbing heavy metal ions Download PDFInfo
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- CN103230779A CN103230779A CN2013101855784A CN201310185578A CN103230779A CN 103230779 A CN103230779 A CN 103230779A CN 2013101855784 A CN2013101855784 A CN 2013101855784A CN 201310185578 A CN201310185578 A CN 201310185578A CN 103230779 A CN103230779 A CN 103230779A
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Abstract
The invention relates to a preparation method for a nanometer sphere capable of absorbing heavy metal ions. The preparation method comprises the following steps of: (a) adding siloxane ionic liquid and nanometer spheres in a mass proportion of 1:(1-10) and 50-100ml of solvents in a reaction container, carrying out ultrasonic processing for 0.5-1 hour to prepare suspension liquid, carrying out condensation and backflow for 24-48 hours under inert gas protection at 65-90 DEG C, and carrying out centrifuging to obtain rough products; (b) adding the solvents into the rough products obtained in the step (a) again, and repeatedly carrying out ultrasonic dispersion and the centrifuging for 3-5 times to obtain purified products; (c) dispersing the purified products obtained in the step (b) into a water solution with the concentration of 1*10<-5>-0.1mol/L for ion exchange for 24-72 hours, and carrying out the centrifuging to obtain ion-exchanged products; and (d) adding deionized water into the ion-exchanged products obtained in the step (c), repeatedly carrying out the ultrasonic dispersion and the centrifuging for 3-5 times, and drying to obtain final products. The preparation method provided by the invention has the advantages that the process is simple, the operation is convenient, and the yield is high; and the prepared nanometer sphere capable of absorbing the heavy metal ions can be used for recycling the different heavy metal ions and can be repeatedly used.
Description
Technical field
The present invention relates to nanometer particle process method, particularly a kind of preparation method of adsorbable heavy metal ion nanometer bead.
Background technology
Along with the increase of activity in production in the industry such as mining and metallurgy, machine-building, chemical industry, electronics, instrument, many production processes have all produced heavy metal wastewater thereby (as cadmium, lead, copper, mercury etc.).Heavy metal wastewater thereby is that environmental pollution is the most serious and the mankind are endangered one of maximum industrial wastewater, therefore, how to administer the generally attention that heavy metal wastewater thereby has been subjected to all circles.
At present, have for the effective treating method of removing metal ion: chemical precipitation method, ion-exchange, electrochemical treatments, membrane technology, evaporation coagulation, counter-infiltration and electrodialysis etc.The industrial chemical precipitation method that adopts is handled heavy metal wastewater thereby more, but the chemical precipitation method existence easily causes the water quality sclerosis, and is not thorough to the heavy metal ion processing of low concentration, causes shortcomings such as secondary pollution easily.Ion-exchange-resin process can be transferred to heavy metal ion on the resin, but resin is difficult to separate with heavy metal ion, no matter be all not enough to some extent aspect the recycling of resin or aspect the recovery of precious metal.Absorption method is a kind of method that is commonly used to handle heavy metal wastewater thereby, compares with additive method, and this method technology is simple, easy to operate.Wherein adopt merchandise active carbon is adsorbent more, has stronger adsorption capacity, the heavy metal removing rate height, but need through industry extraction and preparation, cost height.
Complex is by central atom, ligand and extraneous the composition.Part provides lone pair electrons or a plurality of delocalized electrons, and central atom is accepted lone pair electrons or a plurality of delocalized electrons, and the two is in conjunction with forming coordinate bond.Transition metal ions is common central ion, thereby heavy metal ion forms complex, group and heavy metal ion that complex can dissociate the original lone pair electrons of formation under certain condition with group (containing elements such as N, the O) combination that contains lone pair electrons easily.This special nature is simple for seeking a kind of making, and adsorption activity height, the heavy metal ion adsorbing material that can reuse provide may.
Summary of the invention
The present invention seeks to provide in order to overcome the deficiencies in the prior art a kind of preparation method who utilizes coordinate bond Adsorption of Heavy Metal Ions nanometer bead.
For solving above technical problem, a kind of technical scheme that the present invention takes is: a kind of preparation method of adsorbable heavy metal ion nanometer bead may further comprise the steps:
(a), in reaction vessel, press mass ratio 1:1～10 and add siloxanes ionic liquid, nanometer bead, 50～500ml solvent, ultrasonic 0.5～1h is configured to suspension, and under 65-90 ℃, inert gas shielding condensing reflux 24-48 hour, centrifugal crude product;
(b), in step (a) crude product, add solvent, ultrasonic dispersion, centrifugal again, repeat the product that to purify for 3～5 times;
(c), the product of purifying in the step (b) being dispersed in concentration is 1 * 10
-5～0.1mol/L's
Carry out ion-exchange 24～72 hours in the aqueous solution, the centrifugal product that gets ion-exchange;
(d), in the product of step (c) ion-exchange, add deionized water, ultrasonic dispersion, centrifugal, repeat 3～5 times dry end product.
The structural formula of wherein said siloxanes ionic liquid is
X is selected from a kind of among Cl, I, the Br in the formula, and n and m are separate to be 2 to 5 integer, and R is CH
3, CH
3CH
2, CH
3CH
2CH
2, CH
3CH
2CH
2CH
2In a kind of.
Optimally, described nanometer bead is a kind of in silica, titanium dioxide, zinc oxide, the aluminium oxide, and its particle diameter is 50～200nm.
Optimally, described solvent is a kind of in carrene, the chloroform.
Because technique scheme is used, the present invention compared with prior art has following advantage:
1, this procedure is simple, easy to operate and productive rate is high;
2, the adsorbable heavy metal ion nanometer bead that utilizes this method to prepare can be realized the recovery to different heavy metal ion, and can reuse.
The specific embodiment
Below be specific embodiments of the invention, technical scheme of the present invention is further described, but the present invention is not limited to these embodiment.
Embodiment 1
This example provides a kind of preparation method of adsorbable heavy metal ion nanometer bead, and its concrete steps are as follows:
(a), add 0.1g at reaction vessel
The nano silicon bead of 1g50nm, the 50ml solvent, ultrasonic 0.5h is configured to suspension, and condensing reflux is 48 hours under 65 ℃, inert gas shielding, centrifugal crude product;
(b), in step (a) crude product, add solvent, ultrasonic dispersion, centrifugal again, repeat the product that to purify for 3 times;
(c), the product of purifying in the step (b) being dispersed in concentration is 1 * 10
-5Mol/L's
Carry out ion-exchange 72 hours in the aqueous solution, the centrifugal product that gets ion-exchange;
(d), in the product of step (c) ion-exchange, add deionized water, ultrasonic dispersion, centrifugal, repeat 3 times dry end product.
Embodiment 1
This example provides a kind of preparation method of adsorbable heavy metal ion nanometer bead, and its concrete steps are as follows:
(a), add 1g at reaction vessel
The nano silicon bead of 1g500nm, the 500ml solvent, ultrasonic 1h is configured to suspension, and condensing reflux is 24 hours under 90 ℃, inert gas shielding, centrifugal crude product;
(b), in step (a) crude product, add solvent, ultrasonic dispersion, centrifugal again, repeat the product that to purify for 5 times;
(c), the product of purifying in the step (b) being dispersed in concentration is 0.1mol/L's
Carry out ion-exchange 24 hours in the aqueous solution, the centrifugal product that gets ion-exchange;
(d), in the product of step (c) ion-exchange, add deionized water, ultrasonic dispersion, centrifugal, repeat 5 times dry end product.
Above-described embodiment only is explanation technical conceive of the present invention and characteristics, and its purpose is to allow the personage who is familiar with this technology can understand content of the present invention and enforcement according to this, can not limit protection scope of the present invention with this.All equivalences that spirit essence is done according to the present invention change or modify, and all should be encompassed within protection scope of the present invention.
Claims (3)
1. the preparation method of an adsorbable heavy metal ion nanometer bead is characterized in that: may further comprise the steps:
(a), in reaction vessel, press mass ratio 1:1～10 and add siloxanes ionic liquid, nanometer bead, 50～500ml solvent, ultrasonic 0.5～1h is configured to suspension, and under 65-90 ℃, inert gas shielding condensing reflux 24-48 hour, centrifugal crude product;
(b), in step (a) crude product, add solvent, ultrasonic dispersion, centrifugal again, repeat the product that to purify for 3～5 times;
(c), the product of purifying in the step (b) being dispersed in concentration is 1 * 10
-5～0.1mol/L's
Carry out ion-exchange 24～72 hours in the aqueous solution, the centrifugal product that gets ion-exchange;
(d), in the product of step (c) ion-exchange, add deionized water, ultrasonic dispersion, centrifugal, repeat 3～5 times dry end product.
The structural formula of wherein said siloxanes ionic liquid is
X is selected from a kind of among Cl, I, the Br in the formula, and n and m are separate to be 2 to 5 integer, and R is CH
3, CH
3CH
2, CH
3CH
2CH
2, CH
3CH
2CH
2CH
2In a kind of.
2. the preparation method of adsorbable heavy metal ion nanometer bead according to claim 1 is characterized in that: described nanometer bead is a kind of in silica, titanium dioxide, zinc oxide, the aluminium oxide, and its particle diameter is 50～200nm.
3. the preparation method of adsorbable heavy metal ion nanometer bead according to claim 1 and 2 is characterized in that: described solvent is a kind of in carrene, the chloroform.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107417913A (en) * | 2017-08-22 | 2017-12-01 | 广东工业大学 | A kind of method of heavy metal in organic microporous polymer of nanometer and absorption drinking water |
Citations (4)
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| US6544419B1 (en) * | 1996-10-31 | 2003-04-08 | University Of Kentucky Research Foundation | Method of preparing a composite polymer and silica-based membrane |
| CN101612597A (en) * | 2009-07-27 | 2009-12-30 | 中国科学院长春应用化学研究所 | The organic-inorganic composite anion exchange resin and the method for making that are used for adsorbing hexavalent chromium ions |
| CN101785991A (en) * | 2009-12-12 | 2010-07-28 | 鲁东大学 | Preparation method of amino bonded silica gel glycerol adsorbent and prepared product thereof |
| US20110026024A1 (en) * | 2009-07-30 | 2011-02-03 | Industry-University Cooperation Foundation Sogang University | Method and apparatus for detecting metal ions, probe used for the same and preparation method thereof |
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2013
- 2013-05-20 CN CN201310185578.4A patent/CN103230779B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| US6544419B1 (en) * | 1996-10-31 | 2003-04-08 | University Of Kentucky Research Foundation | Method of preparing a composite polymer and silica-based membrane |
| CN101612597A (en) * | 2009-07-27 | 2009-12-30 | 中国科学院长春应用化学研究所 | The organic-inorganic composite anion exchange resin and the method for making that are used for adsorbing hexavalent chromium ions |
| US20110026024A1 (en) * | 2009-07-30 | 2011-02-03 | Industry-University Cooperation Foundation Sogang University | Method and apparatus for detecting metal ions, probe used for the same and preparation method thereof |
| CN101785991A (en) * | 2009-12-12 | 2010-07-28 | 鲁东大学 | Preparation method of amino bonded silica gel glycerol adsorbent and prepared product thereof |
Non-Patent Citations (1)
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| XIAOJIAN CHEN, ET AL: "Ionic liquid-tethered nanoparticle/poly(ionic liquid) electrolytes for quasi-solid-state dye-sensitized solar cells", 《JOURNAL OF POWER SOURCES》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107417913A (en) * | 2017-08-22 | 2017-12-01 | 广东工业大学 | A kind of method of heavy metal in organic microporous polymer of nanometer and absorption drinking water |
| CN107417913B (en) * | 2017-08-22 | 2020-04-14 | 广东工业大学 | Nano organic microporous polymer and method for adsorbing heavy metals in drinking water |
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| CN103230779B (en) | 2014-10-08 |
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Effective date of registration: 20151013 Address after: 224300 crossing economic zone of Haihe Town, Sheyang County, Jiangsu, Yancheng City Patentee after: YANCHENG YOUPU ENVIRONMENTAL PROTECTION TECHNOLOGY CO., LTD. Address before: 215123 Suzhou Industrial Park, Jiangsu Road, No. 199 Patentee before: Soochow University |