CN103861562A - Preparation method of carbon nano tube with function of selectively adsorbing lead ions - Google Patents
Preparation method of carbon nano tube with function of selectively adsorbing lead ions Download PDFInfo
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- CN103861562A CN103861562A CN201410133247.0A CN201410133247A CN103861562A CN 103861562 A CN103861562 A CN 103861562A CN 201410133247 A CN201410133247 A CN 201410133247A CN 103861562 A CN103861562 A CN 103861562A
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Abstract
The invention relates to a preparation method of a carbon nano tube with a function of selectively adsorbing lead ions. The method comprises the steps of adding an aminated carbon nano tube into distilled water, and dispersing; after that, feeding lead nitrate, and stirring for reaction for 3-15h at the temperature of 35-85 DEG C; and carrying suction filtration and vacuum drying, grinding the product into powder, washing and carrying out vacuum drying again to obtain the carbon nano tube. The material prepared by the invention can be used as a selective adsorbent for the lead ions in the blood and an inorganic particle additive for a functional filter membrane, thus being used in the aspects such as water treatment, blood purification and the like; the preparation method is simple in technology, convenient to operate and mild in conditions; and the prepared product is high in adsorption capacity and capable of selectively adsorbing the lead ions, and has excellent biological compatibility.
Description
Technical field
The invention belongs to the preparation field of lead ion sorbing material, particularly a kind of preparation method of the CNT with selective absorption lead ion.
Background technology
In recent years, heavy metal pollution becomes an importance of environmental pollution, and lead ion also just becomes one of material the most dangerous in the ecosystem.Lead is a kind of heavy metal of serious harm health, can enter human body by number of ways, but it can not be biodegradable and long half time in vivo, and many tracts and physiological function are all produced to harm.And children will be higher than adult to the sensitiveness of plumbous toxic action, due to children's brain development imperfection, facial pallor is easily accumulated at children's brain, causes children's central nervous system disorder.Research shows, can occur obvious lead poisoning phenomenon when blood lead exceedes 3.86 μ mol/L, and the diagnostic value of blood lead is fixed on to 2.9 μ mol/L.Therefore, enrichment is to analyze and process the indispensable link of lead poisoning with separating trace lead.
The material to the selective absorption of templated metal ion that metal ion imprinted material refers to take metal ion as template, utilizes engram technology to prepare.Metal ion engram technology is a branch direction of molecular imprinting research, is the cross discipline together growing up with organic molecule engram technology.At present, the more existing documents of method and the patent of preparing imprinted material are reported.Li Lujuan etc. are take plumbous (II) ion as template, salicylaldoxime is function monomer, GDMA is crosslinking agent, azodiisobutyronitrile is initator, adopt mass polymerization prepare imprinted polymer (Li Lujuan, Liu Huijun, Zhang Lei. the plumbous preparation of (II) ion imprinted polymer and the research [J] of absorption property thereof. chemistry circular, 2011,74 (6): 539-544.); Ren Yueming etc. (Chinese patent 201210105117.7) invent a kind of preparation method in water with selective recognition performance metal ion trace adsorbent; He Hua etc. (Chinese patent 201110310238.0) have invented a kind of New Type of Carbon nanotube surface molecularly imprinted polymer and preparation method thereof.But the preparation method who CNT is carried out to trace rarely has report at present.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of preparation method of the CNT with selective absorption lead ion, this invention combines the absorption property of CNT and metal ion engram technology, make CNT there is specific adsorption, energy selective absorption lead ion is the promising sorbing material of a kind of tool.
The preparation method of a kind of CNT with selective absorption lead ion of the present invention, comprising:
Aminated carbon nano tube is added in distilled water, disperse, then add plumbi nitras, under 35-85 ℃ of condition, stirring reaction 3-15h, suction filtration, vacuum drying, pulverize, obtain lead ion chelating aminated carbon nano tube, washing, then vacuum drying, must have the CNT of selective absorption lead ion; Wherein the mass ratio of aminated carbon nano tube and plumbi nitras is 5-9:1.
Described being separated under room temperature condition, ultrasonic dispersion 30-60min.
Described vacuum drying is 30-80 ℃ of vacuum drying 12-36h.
Described washing is for being first washed till and can't detect Pb with the HCL aqueous solution
2+, then be washed till solution with the NaOH aqueous solution and distilled water and be neutral and suction filtration.
Described HCL concentration of aqueous solution is 1～6mol/L; The concentration of the NaOH aqueous solution is 0.05～1mol/L.
The described CNT with selective absorption lead ion obtaining is 40～100mg/g to the adsorbance of lead ion.
The described CNT with selective absorption lead ion obtaining is as the inorganic particulate additive of the poisoning selective absorbent of blood lead ion, function filter membrane and for water treatment and blood purification.
beneficial effect
(1) the present invention combines the absorption property of CNT and metal ion engram technology, makes CNT have specific selectivity absorption;
(2) the present invention adopts aminated carbon nano tube, make lead ion can with aminated carbon nano tube on amino carry out chelatropic reaction, form lead ion hole, thereby be conducive to the selective absorption of lead ion;
(3) the lead ion trace CNT that the present invention obtains, has good mechanical performance, and to Pb
2+having specific adsorption and separation function, is the promising sorbing material of a kind of tool;
(4) simple, the easy to operate and mild condition of technique of the present invention, prepares product adsorption capacity large and can selective absorption lead ion, has good biocompatibility.
The specific embodiment
Below in conjunction with specific embodiment, further set forth the present invention.Should be understood that these embodiment are only not used in and limit the scope of the invention for the present invention is described.In addition should be understood that those skilled in the art can make various changes or modifications the present invention after having read the content of the present invention's instruction, these equivalent form of values fall within the application's appended claims limited range equally.
Embodiment 1
Get aminated carbon nano tube 5g, distilled water 100mL, joins respectively in there-necked flask, and the ultrasonic dispersion of normal temperature 30min, is uniformly dispersed aminated carbon nano tube.Then add 1g plumbi nitras, at 35 ℃ of magnetic agitation reaction 15h, make aminated carbon nano tube and Pb
2+fully reaction.Reaction finishes 30 ℃ of vacuum drying 36h of rear suction filtration, pulverize.Be washed till and can't detect Pb with the HCL aqueous solution of 1mol/L
2+, then be washed till solution with the NaOH aqueous solution of 0.05mol/L and distilled water and be neutral, suction filtration, 30 ℃ of vacuum drying 36h, obtain lead ion trace CNT, and this lead ion trace CNT is 40mg/g to the adsorbance of lead ion.
Take plumbi nitras, copper chloride, the each 0.1g of zinc sulfate and be dissolved in the plumbi nitras-copper chloride-zinc sulfate mixed solution that is configured to 1g/L in 100mL water, 0.3g lead ion trace CNT is added in above-mentioned solution, under room temperature, shake after 3h centrifugal.Detect the content of lead ion, copper ion, zinc ion in centrifuged supernatant, calculate the adsorption capacity of lead ion trace CNT to three metal ion species.Under same concentrations, lead ion trace CNT is respectively 39mg/g, 3.5mg/g and 1.5mg/g to the adsorption capacity of lead ion, copper ion, zinc ion.Known, lead ion trace CNT is to the selective absorption of lead ion.
Embodiment 2
Get aminated carbon nano tube 3g, distilled water 100mL, joins respectively in there-necked flask, and the ultrasonic dispersion of normal temperature 40min, is uniformly dispersed aminated carbon nano tube.Then add 0.5g plumbi nitras, at 45 ℃ of magnetic agitation reaction 13h, make aminated carbon nano tube and Pb
2+fully reaction.Reaction finishes 40 ℃ of vacuum drying 32h of rear suction filtration, pulverize.Be washed till and can't detect Pb with the HCL solution of 2mol/L
2+, then be washed till solution with the NaOH aqueous solution of 0.1mol/L and distilled water and be neutral, suction filtration, 40 ℃ of vacuum drying 32h, obtain lead ion trace CNT, and this lead ion trace CNT is 45mg/g to the adsorbance of lead ion.
The preparation of plumbi nitras-copper chloride-zinc sulfate mixed solution is as embodiment 1.Under same concentrations, lead ion trace CNT is respectively 43mg/g, 3.3mg/g and 1.2mg/g to the adsorption capacity of lead ion, copper ion, zinc ion.Known, lead ion trace CNT is to the selective absorption of lead ion.
Embodiment 3
Get aminated carbon nano tube 6g, distilled water 100mL, joins respectively in there-necked flask, and the ultrasonic dispersion of normal temperature 40min, is uniformly dispersed aminated carbon nano tube.Then add 1g plumbi nitras, at 55 ℃ of magnetic agitation reaction 11h, make aminated carbon nano tube and Pb
2+fully reaction.Reaction finishes 50 ℃ of vacuum drying 28h of rear suction filtration, pulverize.Be washed till and can't detect Pb with the HCL solution of 3mol/L
2+, then be washed till solution with the NaOH aqueous solution of 0.2mol/L and distilled water and be neutral, suction filtration, 50 ℃ of vacuum drying 28h, obtain lead ion trace CNT, and this lead ion trace CNT is 54mg/g to the adsorbance of lead ion.
The preparation of plumbi nitras-copper chloride-zinc sulfate mixed solution is as embodiment 1.Under same concentrations, lead ion trace CNT is respectively 53mg/g, 3.0mg/g and 1.0mg/g to the adsorption capacity of lead ion, copper ion, zinc ion.Known, lead ion trace CNT is to the selective absorption of lead ion.
Embodiment 4
Get aminated carbon nano tube 7g, distilled water 100mL, joins respectively in there-necked flask, and the ultrasonic dispersion of normal temperature 50min, is uniformly dispersed aminated carbon nano tube.Then add 1g plumbi nitras, at 55 ℃ of magnetic agitation reaction 9h, make aminated carbon nano tube and Pb
2+fully reaction.Reaction finishes 50 ℃ of vacuum drying 24h of rear suction filtration, pulverize.Be washed till and can't detect Pb with the HCL solution of 4mol/L
2+, then be washed till solution with the NaOH aqueous solution of 0.4mol/L and distilled water and be neutral, suction filtration, 50 ℃ of vacuum drying 24h, obtain lead ion trace CNT, and this lead ion trace CNT is 72mg/g to the adsorbance of lead ion.
The preparation of plumbi nitras-copper chloride-zinc sulfate mixed solution is as embodiment 1.Under same concentrations, lead ion trace CNT is respectively 70mg/g, 2.5mg/g and 0.8mg/g to the adsorption capacity of lead ion, copper ion, zinc ion.Known, lead ion trace CNT is to the selective absorption of lead ion.
Embodiment 5
Get aminated carbon nano tube 3.5g, distilled water 100mL, joins respectively in there-necked flask, and the ultrasonic dispersion of normal temperature 50min, is uniformly dispersed aminated carbon nano tube.Then add 0.5g plumbi nitras, at 65 ℃ of magnetic agitation reaction 7h, make aminated carbon nano tube and Pb
2+fully reaction.Reaction finishes 60 ℃ of vacuum drying 20h of rear suction filtration, pulverize.Be washed till and can't detect Pb with the HCL solution of 5mol/L
2+, then be washed till solution with the NaOH aqueous solution of 0.6mol/L and distilled water and be neutral, suction filtration, 60 ℃ of vacuum drying 20h, obtain lead ion trace CNT, and this lead ion trace CNT is 83mg/g to the adsorbance of lead ion.
The preparation of plumbi nitras-copper chloride-zinc sulfate mixed solution is as embodiment 1.Under same concentrations, lead ion trace CNT is respectively 80mg/g, 2.0mg/g and 0.6mg/g to the adsorption capacity of lead ion, copper ion, zinc ion.Known, lead ion trace CNT is to the selective absorption of lead ion.
Embodiment 6
Get aminated carbon nano tube 8g, distilled water 100mL, joins respectively in there-necked flask, and the ultrasonic dispersion of normal temperature 60min, is uniformly dispersed aminated carbon nano tube.Then add 1g plumbi nitras, at 75 ℃ of magnetic agitation reaction 5h, make aminated carbon nano tube and Pb
2+fully reaction.Reaction finishes 70 ℃ of vacuum drying 16h of rear suction filtration, pulverize.Be washed till and can't detect Pb with the HCL solution of 5mol/L
2+, then be washed till solution with the NaOH aqueous solution of 0.8mol/L and distilled water and be neutral, suction filtration, 70 ℃ of vacuum drying 16h, obtain lead ion trace CNT, and this lead ion trace CNT is 96mg/g to the adsorbance of lead ion.
The preparation of plumbi nitras-copper chloride-zinc sulfate mixed solution is as embodiment 1.Under same concentrations, lead ion trace CNT is respectively 94mg/g, 1.5mg/g and 0.5mg/g to the adsorption capacity of lead ion, copper ion, zinc ion.Known, lead ion trace CNT is to the selective absorption of lead ion.
Embodiment 7
Get aminated carbon nano tube 9g, distilled water 100mL, joins respectively in there-necked flask, and the ultrasonic dispersion of normal temperature 60min, is uniformly dispersed aminated carbon nano tube.Then add 1g plumbi nitras, at 85 ℃ of magnetic agitation reaction 3h, make aminated carbon nano tube and Pb
2+fully reaction.Reaction finishes 80 ℃ of vacuum drying 12h of rear suction filtration, pulverize.Be washed till and can't detect Pb with the HCL solution of 6mol/L
2+, then be washed till solution with the NaOH aqueous solution of 1mol/L and distilled water and be neutral, suction filtration, 80 ℃ of vacuum drying 12h, obtain lead ion trace CNT, and this lead ion trace CNT is 100mg/g to the adsorbance of lead ion.
The preparation of plumbi nitras-copper chloride-zinc sulfate mixed solution is as embodiment 1.Under same concentrations, lead ion trace CNT is respectively 98mg/g, 1.0mg/g and 0.2mg/g to the adsorption capacity of lead ion, copper ion, zinc ion.Known, lead ion trace CNT is to the selective absorption of lead ion.
Claims (7)
1. a preparation method with the CNT of selective absorption lead ion, comprising:
Aminated carbon nano tube is added in distilled water, disperse, then add plumbi nitras, under 35-85 ℃ of condition, stirring reaction 3-15h, suction filtration, vacuum drying, pulverize, washs, then vacuum drying, must have the CNT of selective absorption lead ion; Wherein the mass ratio of aminated carbon nano tube and plumbi nitras is 5-9:1.
2. the preparation method of a kind of CNT with selective absorption lead ion according to claim 1, is characterized in that: described in be separated under room temperature condition, ultrasonic dispersion 30-60min.
3. the preparation method of a kind of CNT with selective absorption lead ion according to claim 1, is characterized in that: described vacuum drying is 30-80 ℃ of vacuum drying 12-36h.
4. the preparation method of a kind of CNT with selective absorption lead ion according to claim 1, is characterized in that: described washing is for being first washed till and can't detect Pb with the HCL aqueous solution
2+, then be washed till solution with the NaOH aqueous solution and distilled water and be neutral and suction filtration.
5. the preparation method of a kind of CNT with selective absorption lead ion according to claim 4, is characterized in that: described HCL concentration of aqueous solution is 1～6mol/L; The concentration of the NaOH aqueous solution is 0.05～1mol/L.
6. the preparation method of a kind of CNT with selective absorption lead ion according to claim 1, is characterized in that: the CNT with selective absorption lead ion obtaining is 40～100mg/g to the adsorbance of lead ion.
7. the preparation method of a kind of CNT with selective absorption lead ion according to claim 1, is characterized in that: the CNT with selective absorption lead ion obtaining is as the inorganic particulate additive of the poisoning selective absorbent of blood lead ion, function filter membrane and for water treatment and blood purification.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104904574A (en) * | 2015-05-07 | 2015-09-16 | 天津师范大学 | Method for controlling accumulation of heavy metal in turfgrass by means of siduron and carbon nano tube interlayer |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2006047884A1 (en) * | 2004-11-04 | 2006-05-11 | Questair Technologies Inc. | Improved adsorbent material for selective adsorption of carbon monoxide and unsaturated hydrocarbons |
| CN101811024A (en) * | 2010-04-02 | 2010-08-25 | 同济大学 | Preparation of solid phase extractant for enriching lead ions and application method thereof |
-
2014
- 2014-04-03 CN CN201410133247.0A patent/CN103861562A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2006047884A1 (en) * | 2004-11-04 | 2006-05-11 | Questair Technologies Inc. | Improved adsorbent material for selective adsorption of carbon monoxide and unsaturated hydrocarbons |
| CN101811024A (en) * | 2010-04-02 | 2010-08-25 | 同济大学 | Preparation of solid phase extractant for enriching lead ions and application method thereof |
Non-Patent Citations (1)
| Title |
|---|
| GORAN D. VUKOVIC等: "Removal of lead from water by amino modified multi-walled carbon nanotubes", 《CHEMICAL ENGINEERING JOURNAL》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104904574A (en) * | 2015-05-07 | 2015-09-16 | 天津师范大学 | Method for controlling accumulation of heavy metal in turfgrass by means of siduron and carbon nano tube interlayer |
| CN104904574B (en) * | 2015-05-07 | 2017-10-10 | 天津师范大学 | Regulate and control the method for turfgrass heavy metal accumulation using Tupersan and CNT interlayer |
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Application publication date: 20140618 |