CN102553528A - Modified carbon nano tube material, method for removing mercury ions in water and method for regenerating modified carbon nano tube material - Google Patents
Modified carbon nano tube material, method for removing mercury ions in water and method for regenerating modified carbon nano tube material Download PDFInfo
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Abstract
The invention relates to a modified carbon nano tube material, a method for removing mercury ions in water and a method for regenerating the modified carbon nano tube material. The modified carbon nano tube material is a selenium modified nano particle load/iron oxide magnetic carbon nano tube composite material. According to the method for removing the mercury ions in the water, the modified carbon nano tube material is used as an adsorbent and is put into the water to be treated to adsorb the mercury ions in the water; and a method for preparing the modified carbon nano tube material comprises the following steps that: after being oxidized and activated by concentrated acid, a carbon nano tube material is coated with an iron oxide together with a ferric salt-containing solution on the surface of a carbon nano tube by a coprecipitation method and then is reacted with an aqueous solution containing Na2SeO3 and glucose to obtain the modified carbon nano tube material. The modified carbon nano tube material has high adsorptive capacity and selectivity on mercury, so that the solid-liquid separation of the adsorbent and the solution can be implemented conveniently under the action of an additional magnetic field. After being treated, the modified carbon nano tube material can be recycled; compared with the conventional adsorption material, the modified carbon nano tube material has high recycling performance; and the used adsorbent is easy to separate and recover, so the water treatment cost is saved, the possibility of secondary pollution is reduced, and the modified carbon nano tube material has good economic and environmental benefits.
Description
Technical field
The present invention relates to a kind of modified carbon nano tube tube material and utilize it to remove the method and the reclaiming method of mercury ion in the water; Relate in particular to a kind of selenium modification carbon nano-tube material and utilize its method and reclaiming method of removing mercury ion in the water, belong to water-treatment technology field.
Background technology
Poisonous element mercury can enter into environment through geology reason and artificial origin; The Trace Hg that is present in the environment can finally enter into water body through sedimentation etc.; Amplify with biological through hydrobiological biological concentration then; And in its biochemical cycles process, generate organomercurial compound, toxicity strengthens nearly thousand times.So, remove Trace Hg in the water body to preserving the ecological environment and human health has crucial meaning.
The Trace Hg that absorption method is removed in the water body has the advantage that additive method does not possess, as simple to operate, with low cost etc.CNT is the novel nano-material that was widely used in recent years, owing to have bigger specific area and stable physicochemical properties, successfully has been used for removing in the middle of the research of water body pollutant.But the adsorbable multiple pollutant of CNT makes the material chosen specificity not high, and the adsorption capacity of mercury is restricted.Simultaneously, because CNT has certain hydrophobicity, quality is bulk, in removing water body, is not easy in the process of pollutant to be disperseed and reclaim, and has increased difficulty and the cost used, thereby has also limited its range of application.In addition, the price of CNT is higher usually, can not recycle and limit CNT being widely used as adsorbent.
Summary of the invention
Technical problem to be solved by this invention is that the defective that overcomes prior art provides a kind of modified carbon nano tube tube material, and this material has characteristics such as many walls porous, magnetic effect, high adsorption capacity, easy separation; In addition, the present invention also will further provide the renovation process that utilizes this modified carbon nano tube tube material to remove mercury ion in the water and it is provided as adsorbent.
Technical problem according to the invention is realized by following technical scheme.
A kind of modified carbon nano tube tube material, said modified carbon nano tube tube material are selenium decorated nanometer particle load/ferriferous oxide magnetic carbon-nano tube composite material.
A kind of method for preparing above-mentioned modified carbon nano tube tube material, it coats ferriferous oxide with coprecipitation method in carbon nano tube surface with solution containing iron salts with carbon nano-tube material behind the concentrated acid oxidized activating, again with contain Na
2SeO
3With the reactant aqueous solution of glucose, promptly get selenium nano particles load/ferriferous oxide magnetic carbon-nano tube composite material.
Above-mentioned preparation method, specifically carry out as follows:
A, oxidized activating:
1. take by weighing carbon nano-tube material 0.5-1.0g, place 40-60 ml autoclave, adding 10-20 ml mass fraction is the red fuming nitric acid (RFNA) of 65-68%, airtight autoclave;
The autoclave that 2. will fill above-mentioned reactant places baking oven, under 100-105 ℃ of condition, keeps 10-15 min, is warming up to 150-160 ℃ then rapidly, and reaction 1.0-1.5 h after reacting completely, stops heating, naturally cools to room temperature;
3. in baking oven, take out and the unlatching agitated reactor, inclining the residue spent acid, is neutrality with washed with de-ionized water product to cleaning fluid;
4. above-mentioned product is dried 4-6 h down at 100-110 ℃, make the carbon nano-tube material of activation, subsequent use;
B, magnetic are modified:
1., the magnetic modification reaction of carbon nano-tube material is under the condition of ultrasonic wave and nitrogen protection, to carry out, reaction temperature is 45-55 ℃;
2., take by weighing the carbon nano-tube material 0.5-1.0 g after the activation, be suspended in 100-200 ml and contain (NH
4)
2Fe (SO
4)
26H
2O and NH
4Fe (SO
4)
212H
2In the mixed solution of O, the reaction system solid-to-liquid ratio, promptly the g/ml of activated carbon nano-tube/mixed solution is 1:200; The solute mass range is in the mixed liquor: (NH
4)
2Fe (SO
4)
26H
2O is 0.36-3.2g, NH
4Fe (SO
4)
212H
2O is 0.53-4.7g; Solute (NH
4)
2Fe (SO
4)
26H
2O and NH
4Fe (SO
4)
212H
2The mass ratio of O is 1.7:2.5;
3., above-mentioned system solution is placed reaction 10-15 min under the ultrasonic wave condition; Ultrasound condition is: supersonic frequency 40KHz, ultrasonic power 250W, heating power 400W; The ammoniacal liquor that dropwise adds 8mol/L in the course of reaction remains between the 11-12 pH value of mixed liquor;
4., after ultrasonic reaction finishes, carry out thoroughly, reaction system keeps 60-70min in 45-55 ℃ of water bath with thermostatic control, and the constant speed of carrying out 300-400r/min stirs for further guaranteeing reaction;
5., after reaction accomplishes, use distilled water and absolute ethanol washing 3-4 time respectively, vacuum drying 8-10 h makes the ferriferous oxide magnetic carbon-nano tube composite material under 50 ℃ of conditions, and is subsequent use;
C, selenium nano particles load:
1., get 0.0658 g Na
2SeO
3Placing volume with 0.198 g glucose is in the autoclave of 40-60mL jar, adds deionized water 12-20 ml then, is stirred to dissolving.
2., add 0.2-2g step B gained modified carbon nano tube tube material, autoclave is airtight;
3., autoclave is placed baking oven, be warming up to 140 ℃, keep 10min;
4., then, continue reaction 10h down at 180 ℃;
5., be cooled to room temperature, the brown precipitate thing filters the back water and washes repeatedly with absolute ethyl alcohol, and is colourless to cleaning solution, dries 8h down at 55 ℃, makes modified Nano particle load/ferriferous oxide magnetic carbon-nano tube composite material.
A kind of method of removing mercury ion in the water, it places pending water with the adsorbed water mercury ion as adsorbent the modified carbon nano tube tube material, and said modified carbon nano tube tube material is selenium decorated nanometer particle load/ferriferous oxide magnetic carbon-nano tube composite material.
The method of mercury ion in the above-mentioned removal water, said adsorbent are that the mercury ion in the water is removed in absorption under 20-60 ℃, the condition of pH5-9 in temperature.
The method of mercury ion in the above-mentioned removal water, when said absorption was carried out, mercurous pH value of aqueous solution was 5-9, regulated pH with the nitric acid of 1mol/L or the NaOH of hydrochloric acid and 1mol/L; Adsorption time is 0.5-1.0h; Said adsorbent is 1:1000-1500 with the g/ml ratio of water; (through measuring, the initial concentration of mercury ion is 0.02-30 μ g/ml, and absorption end of a period concentration is: if initial concentration is a lower limit, end of a period concentration is generally less than 1ng/mL, if initial concentration is the upper limit, end of a period concentration is generally less than 50ng/mL.)
A kind of renovation process of modified carbon nano tube tube material, it uses acid solution wash-out modified carbon nano tube tube material to obtain regeneration.
Above-mentioned renovation process, said acid solution are that volume ratio is the watery hydrochloric acid of 5% (v/v).
Above-mentioned renovation process, it carries out according to the following steps:
(1) modified carbon nano tube tube material and the solution after through externally-applied magnetic field adsorption reaction being finished carries out Separation of Solid and Liquid, the water-outlet body of inclining, and collection is adsorbed with the modified carbon nano tube tube material of mercury;
(2) in the modified carbon nano tube tube material, add watery hydrochloric acid;
(3) rapid stirring reaction 5min under the 300-400 r/min rotating speed;
(5) separate the adsorbent behind the wash-out through externally-applied magnetic field immediately after reaction finishes, topple over and the upper strata dilute acid soln;
(6) the modified carbon nano tube tube material after above-mentioned dilute acid soln is washed washs with deionization immediately, is neutral until cleaning solution;
(7) with the carbon nano-tube modified material of the magnetic behind the wash-out at 50 ℃ of following vacuum drying 6 h, promptly get the carbon nano-tube modified material of magnetic.
Above-mentioned renovation process, the carbon nano-tube modified material of the magnetic after the said absorption is 1:10 with the g/ml ratio of watery hydrochloric acid.
The present invention is coated on the carbon nano-tube material surface with oxides-containing iron, and the decorative material of preparation has stronger soft magnetic bodies character, under the effect of externally-applied magnetic field, is easy to realize the Separation of Solid and Liquid of adsorbent and polluted-water.And the modified carbon nano-tube material list behind the load selenium nano particles reveals higher adsorption capacity of mercury ion in the water and stronger selectivity.Under the normal temperature, the sorbing material maximum adsorption capacity is 47.5 mg/g, is 2.65 times of the activated carbon nano-tube material adsorbance of modifying without selenium.Through pickling, can be with the complete wash-out of mercury ion of absorption, and the material adsorbance of pickling does not have obvious reduction.Simultaneously; Adopt magnetic separation technique, simplified the separation process of adsorption treatment water body mercury ion process greatly, practiced thrift processing time and cost; The adsorbent that is adsorbed with poisonous element can be realized collecting more completely; Be convenient to subsequent processes, avoided secondary pollution preferably, have good economic benefits, environmental benefit and application value.
Description of drawings
Fig. 1 is loaded with nano selenium/magnetic carbon nano-tube material hysteresis curve figure;
Fig. 2 is loaded with nano selenium/magnetic carbon nano-tube material electronics flying-spot microscope (SEM) photo;
Fig. 3 is loaded with nano selenium/magnetic carbon nano-tube material electronics transmission microscopy (TEM) photo;
Fig. 4 is loaded with nano selenium/magnetic carbon nano-tube material X-ray diffraction (XRD) figure.
The specific embodiment
Below in conjunction with specific embodiment the present invention is explained further details.
Embodiment 1 CNT activation
1. get carbon nano-tube material 1.0g, place 60 ml autoclaves, adding 20 ml mass fractions is the red fuming nitric acid (RFNA) of 65-68%, airtight autoclave;
2., the autoclave that will fill above-mentioned reactant places baking oven, under 100 ℃ of conditions, keeps 10 min, is warming up to 150 ℃ then rapidly, reaction 1.0h after reacting completely, stops heating, naturally cools to room temperature;
3., in baking oven, take out and open agitated reactor, inclining the residue spent acid, is neutrality with washed with de-ionized water product to cleaning fluid;
4., with above-mentioned product at 100 ℃ of following oven dry 4 h, make the carbon nano-tube material of activation, subsequent use.
1., the magnetic modification reaction is under the condition of ultrasonic wave and nitrogen protection, to carry out, reaction temperature is 50 ℃;
2., take by weighing carbon nano-tube material 1.0 g after the activation, be suspended in 200 ml and contain 1.7g (NH
4)
2Fe (SO
4)
26H
2O and 2.5gNH
4Fe (SO
4)
212H
2In the mixed solution of O, the mass fraction of iron in the reaction system mixed liquor/(iron+CNT) is 35%, and it is carbon nano-tube modified that product is designated as 35%Fe magnetic;
3., above-mentioned system solution is placed under the ultrasonic wave condition react 10min; The ultrasonic wave condition is: supersonic frequency 40KHz, ultrasonic power 250W, heating power 400W.Dropwise add 8mol/L ammoniacal liquor in the course of reaction, the pH value of mixed liquor is remained between the 11-12;
4., after ultrasonic reaction finishes, carry out thoroughly, reaction system keeps 60min in 50 ℃ of waters bath with thermostatic control, and the constant speed of carrying out 300r/min stirs for further guaranteeing reaction;
5., after reaction accomplishes, use distilled water and absolute ethanol washing 3-4 time respectively, vacuum drying 8h under 50 ℃ of conditions makes the ferriferous oxide magnetic carbon-nano tube composite material, and is subsequent use.
Embodiment 3 selenium nano particles loads
1., get 0.0658 g Na
2SeO
3Placing internal capacity with 0.198 g glucose is in the autoclave of 60mL jar, adds deionized water 20 ml then, is stirred to dissolving; An interior jar material is a polytetrafluoroethylene (PTFE);
2., adding 0.2 g embodiment, 2 gained ferriferous oxide magnetic carbon-nano tube composite materials in the jar, builds seal cover, the autoclave stainless steel outer sleeve of screwing, sealing in PTFE;
3., above-mentioned autoclave is placed baking oven, be warming up to 140 ℃, keep 10min;
4. then, react 10h down at 180 ℃;
5. be cooled to room temperature, the brown precipitate thing filters the back water and absolute ethyl alcohol washes repeatedly, and is colourless to cleaning solution, dries 8h down at 55 ℃, makes selenium nano particles load/ferriferous oxide magnetic carbon-nano tube composite material.
Embodiment 4 selenium nano particles loads
Get 0.0658 g Na
2SeO
3Placing internal capacity with 0.198 g glucose is the autoclave liner cup of 60mL, adds deionized water 20 ml then, is stirred to dissolving; An interior jar material is a polytetrafluoroethylene (PTFE);
2. add 2 g embodiment, 2 gained ferriferous oxide magnetic carbon-nano tube composite materials in PTFE liner cup, build seal cover, the autoclave stainless steel outer sleeve of screwing, sealing;
3. above-mentioned autoclave is placed baking oven, be warming up to 140 ℃, keep 10min;
4., react 10h down at 180 ℃;
5. be cooled to room temperature, the brown precipitate thing filters the back water and absolute ethyl alcohol washes repeatedly, and is colourless to cleaning solution, dries 8h down at 55 ℃, makes selenium nano particles load/ferriferous oxide magnetic carbon-nano tube composite material.
Mercury ion in the contaminant water is removed in embodiment 5 absorption
Selenium nano particles load/ferriferous oxide magnetic carbon-nano tube composite material with embodiment 3 preparations is an adsorbent, and the Trace Mercury ion in the contaminant water is removed in absorption.Adsorption experiment carries out in the 50mL closed container at 20 ℃, and the mercury ion initial concentration is 50 μ g/mL, and pH value of solution is 7, and the adsorbent dosage is 0.02g, and the volume of contaminant water is 25mL, and adsorption time is 60 min, and maximal absorptive capacity is 47.5.
Adsorbance described in this specification is represented the quality of every gram adsorbents adsorb mercury, and unit is mg/g.
Mercury ion in the contaminant water is removed in embodiment 6 absorption
Selenium nano particles load/ferriferous oxide magnetic carbon-nano tube composite material with embodiment 4 preparations is an adsorbent, and adsorption conditions is with embodiment 5, and the maximal absorptive capacity of adsorbent is 30.0.
The comparative example 5, and visible, in the selenium nano particles loading process, the mass fraction that suitably improves selenium/(selenium+magnetic carbon nano-tube material) can improve the adsorption capacity of sorbing material to mercury ion in the water.
Embodiment 7
Selenium nano particles load/ferriferous oxide magnetic carbon-nano tube composite material with embodiment 3 preparations is an adsorbent, under 40 ℃, 60 ℃ conditions, carries out adsorption experiment respectively, and other adsorption conditions records maximal absorptive capacity and is respectively 52.6 and 59.8 with embodiment 5.
The comparative example 5, and visible, in certain temperature range, selenium nano particles load/ferriferous oxide magnetic carbon-nano tube composite material becomes big to the adsorption capacity of mercury ion in the water along with the rising of temperature.
Embodiment 8
Selenium nano particles load/ferriferous oxide magnetic carbon-nano tube composite material with embodiment 3 preparations is an adsorbent, under pH 5, pH9 condition, adsorbs respectively respectively, and other adsorption conditions records maximal absorptive capacity and is respectively 32.7 and 47.0 with embodiment 5.
The comparative example 5, and is visible, under neutral and weak basic condition, high under the absorption property weaker acid property condition of mercury ion in selenium nano particles load/ferriferous oxide magnetic carbon-nano tube composite material adsorbed water.
Embodiment 9
Selenium nano particles load/ferriferous oxide magnetic carbon-nano tube composite material with embodiment 3 preparations is an adsorbent, vibration absorption 20min, 100min, and other adsorption conditions records maximal absorptive capacity and is respectively 30.2 and 47.5 with embodiment 5.
The comparative example 5, and is visible, selenium nano particles load according to the invention/ferriferous oxide magnetic carbon-nano tube composite material to mercury ion in the water be adsorbed on 60min after reach adsorption equilibrium basically.
Selenium nano particles load/ferriferous oxide magnetic carbon-nano tube composite material with embodiment 3 preparations is an adsorbent, in the polluted-water that contains 20 ng/mL mercury ions, adds the Na of 1000 μ g/mL
+, K
+, Ca
2+, Mg
2+, Zn
2+, Mn
2+, Ni
2+, Cu
2+, Cd
2+, Al
3+And Fe
3+Ion, adsorption conditions are investigated the influence of higher concentration common metal ion to the mercury adsorption process with embodiment 5, and the result shows that common metal ion is to the not obviously influence of absorption of selenium nano particles load/ferriferous oxide magnetic carbon-nano tube composite material.It is thus clear that the applied sorbing material of the present invention has superior selectivity and antijamming capability to the absorption of mercury ion in the water.
Embodiment 11
Adsorbent behind the absorption mercury ion is carried out wash-out regeneration.Adopting 10mL5%HCl (v/v) be eluant, eluent, in the 50mL beaker, stirs 5min, removes eluent, and washing selenium nano particles load/ferriferous oxide magnetic carbon-nano tube composite material 3-4 time to cleaning solution with deionized water is neutrality.Vacuum drying 8h under 50 ℃ of conditions obtains to reclaim back selenium nano particles load/ferriferous oxide magnetic carbon-nano tube composite material.
Embodiment 12
Selenium nano particles load/ferriferous oxide the magnetic carbon-nano tube composite material that reclaims with embodiment 11 is an adsorbent; The mercury ion in the water body is removed in absorption; Adsorption conditions is with embodiment 5, and the selenium nano particles load/ferriferous oxide magnetic carbon-nano tube composite material maximal absorptive capacity that records recovery is 44.7.Measure the magnetic of selenium nano particles load/ferriferous oxide magnetic carbon-nano tube composite material that embodiment 11 reclaims, the result shows that magnetic do not have obvious reduction.
It is thus clear that it is that eluant, eluent is regenerated that described selenium nano particles load/ferriferous oxide magnetic carbon-nano tube composite material can adopt watery hydrochloric acid, regeneration still has more superior mercury ion absorption property and stronger magnetic, satisfies the requirement that recycles.
Embodiment 13
Activated carbon nano-tube material so that embodiment 1 makes is directly removed the mercury ion in the water as adsorbents adsorb under the situation of not carrying out the magnetic modification; Adsorption conditions is with embodiment 5, and recording the activated carbon nano-tube material sorbent is 17.9 to the maximal absorptive capacity of mercury ion.
Ferriferous oxide magnetic carbon-nano tube composite material so that embodiment 2 makes is removed the mercury ion in the water as adsorbent; When adsorption conditions was 4,60 ℃ of pH, adsorbent dosage 0.02g, 100min (optimal adsorption condition), the maximal absorptive capacity that records the carbon nano-tube material absorption mercury ion of magnetic modification was 27.5.
Comparative example 5 and embodiment 6, visible through can obviously improving adsorption capacity to mercury ion in magnetic carbon nano-tube area load nanometer selenium.
Claims (10)
1. a modified carbon nano tube tube material is characterized in that, said modified carbon nano tube tube material is selenium decorated nanometer particle load/ferriferous oxide magnetic carbon-nano tube composite material.
2. a modified carbon nano-tube preparation methods is characterized in that, it coats ferriferous oxide with coprecipitation method in carbon nano tube surface with solution containing iron salts with carbon nano-tube material behind the concentrated acid oxidized activating, again with contain Na
2SeO
3With the reactant aqueous solution of glucose, promptly get selenium nano particles load/ferriferous oxide magnetic carbon-nano tube composite material.
3. according to the said modified carbon nano-tube preparation methods of claim 2, it is characterized in that it carries out as follows:
A, oxidized activating:
1. take by weighing carbon nano-tube material 0.5-1.0g, place 40-60 ml autoclave, adding 10-20 ml mass fraction is the red fuming nitric acid (RFNA) of 65-68%, airtight autoclave;
The autoclave that 2. will fill above-mentioned reactant places baking oven, under 100-105 ℃ of condition, keeps 10-15 min, is warming up to 150-160 ℃ then rapidly, and reaction 1.0-1.5 h after reacting completely, stops heating, naturally cools to room temperature;
3. in baking oven, take out and the unlatching agitated reactor, inclining the residue spent acid, is neutrality with washed with de-ionized water product to cleaning fluid;
4. above-mentioned product is dried 4-6 h down at 100-110 ℃, make the carbon nano-tube material of activation, subsequent use;
B, magnetic are modified:
1., the magnetic modification reaction of carbon nano-tube material is under the condition of ultrasonic wave and nitrogen protection, to carry out, reaction temperature is 45-55 ℃;
2., take by weighing the carbon nano-tube material 0.5-1.0 g after the activation, be suspended in 100-200 ml and contain (NH
4)
2Fe (SO
4)
26H
2O and NH
4Fe (SO
4)
212H
2In the mixed solution of O, the reaction system solid-to-liquid ratio, promptly the g/ml of activated carbon nano-tube/mixed solution is 1:200; The solute mass range is in the mixed liquor: (NH
4)
2Fe (SO
4)
26H
2O is 0.36-3.2g, NH
4Fe (SO
4)
212H
2O is 0.53-4.7g; Solute (NH
4)
2Fe (SO
4)
26H
2O and NH
4Fe (SO
4)
212H
2The mass ratio of O is 1.7:2.5;
3., above-mentioned system solution is placed reaction 10-15 min under the ultrasonic wave condition; Ultrasound condition is: supersonic frequency 40KHz, ultrasonic power 250W, heating power 400W; The ammoniacal liquor that dropwise adds 8mol/L in the course of reaction remains between the 11-12 pH value of mixed liquor;
4., after ultrasonic reaction finishes, carry out thoroughly, reaction system keeps 60-70min in 45-55 ℃ of water bath with thermostatic control, and the constant speed of carrying out 300-400r/min stirs for further guaranteeing reaction;
5., after reaction accomplishes, use distilled water and absolute ethanol washing 3-4 time respectively, vacuum drying 8-10 h makes the ferriferous oxide magnetic carbon-nano tube composite material under 50 ℃ of conditions, and is subsequent use;
C, selenium nano particles load:
1., get 0.0658 g Na
2SeO
3Placing volume with 0.198 g glucose is in the autoclave of 40-60mL jar, adds deionized water 12-20 ml then, is stirred to dissolving;
2., add 0.2-2g step B gained modified carbon nano tube tube material, autoclave is airtight;
3., autoclave is placed baking oven, be warming up to 140 ℃, keep 10min;
4., then, continue reaction 10h down at 180 ℃;
5., be cooled to room temperature, the brown precipitate thing filters the back water and washes repeatedly with absolute ethyl alcohol, and is colourless to cleaning solution, dries 8h down at 55 ℃, makes the selenium decorated nanometer particle load/ferriferous oxide magnetic carbon-nano tube composite material of modification.
4. method of removing mercury ion in the water; It is characterized in that; It places pending water with the adsorbed water mercury ion as adsorbent the modifying and decorating carbon nano-tube material, and said modified carbon nano tube tube material is selenium decorated nanometer particle load/ferriferous oxide magnetic carbon-nano tube composite material.
5. according to the method for mercury ion in the said removal water of claim 4, it is characterized in that said adsorbent is that the mercury ion in the water is removed in absorption under 20-60 ℃, the condition of pH5-9 in temperature.
6. according to the method for mercury ion in the said removal water of claim 5, it is characterized in that when said absorption was carried out, the numerical value of pH was regulated for 5-9. pH adopts the nitric acid of 1mol/L or the NaOH of hydrochloric acid and 1mol/L in the water; Adsorption time is 0.5-1.0h; Said adsorbent is 1:1000-1500 with the g/ml ratio of water.
7. the renovation process of a modified carbon nano tube tube material is characterized in that, it uses acid solution wash-out modified carbon nano tube tube material to obtain regeneration.
8. according to the renovation process of the said modified carbon nano tube tube material of claim 7, it is characterized in that said acid solution is that volume ratio is the watery hydrochloric acid of 5% (v/v).
9. the renovation process of said according to Claim 8 modified carbon nano tube tube material is characterized in that, it carries out according to the following steps:
(1) modified carbon nano tube tube material and the solution after through externally-applied magnetic field adsorption reaction being finished carries out Separation of Solid and Liquid, the water-outlet body of inclining, and collection is adsorbed with the modified carbon nano tube tube material of mercury;
(2) in the modified carbon nano tube tube material, add watery hydrochloric acid;
(3) rapid stirring reaction 5min under the 300-400 r/min rotating speed;
(5) separate the adsorbent behind the wash-out through externally-applied magnetic field immediately after reaction finishes, topple over and the upper strata dilute acid soln;
(6) the modified carbon nano tube tube material after above-mentioned dilute acid soln is washed washs with deionization immediately, is neutral until cleaning solution;
(7) with the carbon nano-tube modified material of the magnetic behind the wash-out at 50 ℃ of following vacuum drying 6 h, promptly get the carbon nano-tube modified material of magnetic.
10. according to the renovation process of the said modified carbon nano tube tube material of claim 9, it is characterized in that the carbon nano-tube modified material of the magnetic after the said absorption is 1:10 with the g/ml ratio of watery hydrochloric acid.
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| CN109569551A (en) * | 2018-11-27 | 2019-04-05 | 中国科学院北京综合研究中心 | A kind of preparation method and regeneration method of the nano ceramic material loading nanometer selenium |
| CN109772275A (en) * | 2019-01-07 | 2019-05-21 | 中科京投环境科技江苏有限公司 | Mercury absorbent and preparation method thereof |
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