CN103086459A - Method for removing humic acid in water by magnetic nanometer carbon and regeneration method of magnetic nanometer carbon - Google Patents
Method for removing humic acid in water by magnetic nanometer carbon and regeneration method of magnetic nanometer carbon Download PDFInfo
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- CN103086459A CN103086459A CN2013100174155A CN201310017415A CN103086459A CN 103086459 A CN103086459 A CN 103086459A CN 2013100174155 A CN2013100174155 A CN 2013100174155A CN 201310017415 A CN201310017415 A CN 201310017415A CN 103086459 A CN103086459 A CN 103086459A
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Abstract
The invention discloses a method for removing humic acid in water by magnetic nanometer carbon and a regeneration method of the magnetic nanometer carbon, relates to the method for removing humic acid in water by magnetic nanometer carbon and the regeneration method of the magnetic nanometer carbon, and aims at solving the problems that the existing method is poor in removing effect of humic acid in water, and the used materials are expensive and cannot be recycled. The preparation method comprises the following steps of: firstly, preparing magnetic nanometer carbon; secondly, adding the magnetic nanometer carbon to a humic acid solution; and thirdly, recycling the magnetic nanometer carbon by utilizing magnets, putting the recycled magnetic nanometer carbon to a tubular furnace for carbonization, transferring the carbonized magnetic nanometer carbon to a container with 50mL of deionized water, and carrying out water-bathing and drying. The method and the regeneration method disclosed by the invention are applicable to the chemical field.
Description
Technical field
The present invention relates to the method for humic acid in magnetic Nano carbon removal water and the renovation process of magnetic nanometer carbon.
Background technology
Water pollution has become the problem of extensive concern in world wide.Humic acid is a kind of macromole natural organic matter, extensively is present in the nature water body, is the main organism in the drinking water source.There are some researches show, its content is higher, and the hygienic quality situation is poorer.As important natural ligand and carrier, humic acid is all influential to many environmental problems such as validity, toxicity and migrate attribute thereof of heavy metal in natural water body and organic pollutant.Humic acid is also the strong complexing agent of trace metal, can make underwater gold belong to ion and micronutrient levels decline, and salinity reduces.And the humic acids natural organic matter in water body and the complex reaction of heavy metal ion make heavy metal easily keep dissolved state, and easily occur with the current migration and easily absorb for Living organism.More seriously, the waterworks is in the cholorination treating processes of water, and the substance reactions such as the humic acid in chlorine and water can produce a series of chlorinated secondary products (being mainly haloform, halogen acetic acid etc.), easily cause the breeding once again of bacterium in water-carriage system.And these disinfection byproduct (DBP) are to harmful " three cause " material of HUMAN HEALTH (carcinogenic, mutagenesis, teratogenesis).Therefore, in recent years the control research of humic acids Natural Organic Pollutants in water body has been become the focus of water treatment field.
The humic acid surface comprises a large amount of active groups, makes the humic acid surface with larger electronegativity, thus may with the material generation series reaction of positively charged.And, there are differences from separating the difficulty or ease degree of the groups such as the contained carbonyl of the humic acid of different sources, phenolic hydroxyl group, this just makes the coagulation of water factory's routine, sedimentation processing technology very limited to the removal effect of humic acid.There is the scholar to find that still, Powdered Activated Carbon is expensive with the Powdered Activated Carbon removal effect of enhanced coagulation to humic acid significantly, and disposable use, is difficult to reclaim.The scholar is also arranged with humic acid in the material planar water such as gac, medical stone, metal oxide or with oxidative degradation humic acid such as ozone, photocatalysts, the common problem that exists of these methods is that used material can not reclaim, and easily water surrounding is caused secondary pollution.
Summary of the invention
The present invention will solve material expensive, the irretrievable problem that the method removal effect of humic acid in existing removal water is bad and use, and the method for humic acid in magnetic Nano carbon removal water and the renovation process of magnetic nanometer carbon are provided.
The method of humic acid in magnetic Nano carbon removal water of the present invention, carry out according to the following steps:
One, the orange skin with drying is 1 with catalyzer in mass ratio: the ratio of (0.5～3) is mixed, and dry 20～25h, then put into tube furnace, at N under the condition of 100 ℃
2600-1100 ℃ of charing 0.5～1.5h under atmosphere cleans 1.5～2.5h with the product that obtains in 80 ℃ of deionized waters, the magnetic nanometer carbon that then obtains preparing after dry 20～25h under the condition of 100 ℃; Two, the magnetic nanometer carbon with the step 1 preparation is added in humic acid solution, and regulating pH is 5～13, then at 18～25 ℃ of lower constant temperature oscillation 10～300min, namely completes the method for humic acid in magnetic Nano carbon removal water; Three, utilize magnet that the magnetic nanometer carbon in step 2 is reclaimed, then the magnetic nanometer carbon that reclaims is placed in tube furnace, at N
2300～900 ℃ of charing 20～120min under atmosphere, then move into and to be equipped with in the container of 50mL deionized water, then carry out water-bath 25～35min at the temperature of 50 ℃, stir simultaneously, then after drying, namely complete the renovation process of magnetic nanometer carbon.
The method of humic acid in magnetic Nano carbon removal water of the present invention, by controlling the preparation of magnetic nanometer carbon, the conditions such as the throwing amount of magnetic nanometer carbon, temperature of reaction, reaction times, reaction pH, can make magnetic nanometer carbon to humic acid in water, good removal ability be arranged, thereby make the applicable elimination to humic acids natural organic matter in water surrounding of magnetic nanometer carbon.
The renovation process of magnetic nanometer carbon of the present invention is undertaken by following steps: utilize magnet that the magnetic nanometer carbon that has adsorbed humic acid is reclaimed, then the magnetic nanometer carbon that reclaims is placed in tube furnace, at N
2300～900 ℃ of charing 20～120min under atmosphere, then move into and to be equipped with in the container of 50mL deionized water, then carry out water-bath 25～35min at the temperature of 50 ℃, stir simultaneously, then after drying, namely complete the renovation process of magnetic nanometer carbon.
Magnetic nanometer carbon renovation process of the present invention, very simple, environmental protection can realize the cycling and reutilization of resource, have avoided to greatest extent secondary pollution.Simultaneously, save treatment time and cost, had potential using value aspect the environmental pollutant removal.
Description of drawings
Fig. 1 is the X-ray diffraction spectrogram of the magnetic nanometer carbon of test 1 step 1 preparation;
Fig. 2 is the X-ray diffraction spectrogram of testing the magnetic nanometer carbon of regenerating in 1 step 3;
Fig. 3 is the adsorption test figure as a result of test 2 step 2;
Fig. 4 is the adsorption test figure as a result of test 3 step 2.
Embodiment
Embodiment one: the method for humic acid in the magnetic Nano carbon removal water of present embodiment, carry out according to the following steps:
One, the orange skin with drying is 1 with catalyzer in mass ratio: the ratio of (0.5～3) is mixed, and dry 20～25h, then put into tube furnace, at N under the condition of 100 ℃
2600-1100 ℃ of charing 0.5～1.5h under atmosphere cleans 1.5～2.5h with the product that obtains in 80 ℃ of deionized waters, the magnetic nanometer carbon that then obtains preparing after dry 20～25h under the condition of 100 ℃; Two, the magnetic nanometer carbon with the step 1 preparation is added in humic acid solution, and regulating pH is 5～13, then at 18～25 ℃ of lower constant temperature oscillation 10～300min, namely completes the method for humic acid in magnetic Nano carbon removal water; Three, utilize magnet that the magnetic nanometer carbon in step 2 is reclaimed, then the magnetic nanometer carbon that reclaims is placed in tube furnace, at N
2300～900 ℃ of charing 20～120min under atmosphere, then move into and to be equipped with in the container of 50mL deionized water, then carry out water-bath 25～35min at the temperature of 50 ℃, stir simultaneously, then after drying, namely complete the renovation process of magnetic nanometer carbon.
The method of humic acid in the magnetic Nano carbon removal water of present embodiment, by controlling the preparation of magnetic nanometer carbon, the conditions such as the throwing amount of magnetic nanometer carbon, temperature of reaction, reaction times, reaction pH, can make magnetic nanometer carbon to humic acid in water, good removal ability be arranged, thereby make the applicable elimination to humic acids natural organic matter in water surrounding of magnetic nanometer carbon.And the magnetic nanometer carbon renovation process of present embodiment, very simple, environmental protection can realize the cycling and reutilization of resource, have avoided to greatest extent secondary pollution.Simultaneously, save treatment time and cost, had potential using value aspect the environmental pollutant removal.
Embodiment two: what present embodiment was different from embodiment one is: the catalyzer in step 1 is that one or more in iron(ic) chloride, iron protochloride, ferric sulfate, ferrous sulfate, iron nitrate or Iron nitrate are mixed by any ratio.Other is identical with embodiment one.
Embodiment three: what present embodiment was different from embodiment one or two is: in step 1, dry orange skin and catalyzer are that the ratio of 1: 1 is mixed in mass ratio.Other is identical with embodiment one or two.
Embodiment four: what present embodiment was different from one of embodiment one to three is: in step 1 under the condition of 100 ℃ dry 24h.Other is identical with one of embodiment one to three.
Embodiment five: what present embodiment was different from one of embodiment one to four is: N in step 1
2Flow be 100mL/min.Other is identical with one of embodiment one to four.
Embodiment six: what present embodiment was different from one of embodiment one to five is: be 100 according to magnetic nanometer carbon and humic acid mass ratio in step 2: the ratio of (1～10) adds magnetic nanometer carbon.Other is identical with one of embodiment one to five.
Embodiment seven: what present embodiment was different from one of embodiment one to six is: adopt hydrochloric acid or sodium hydroxide to regulate pH in step 2.Other is identical with one of embodiment one to six.
Embodiment eight: the renovation process of the magnetic nanometer carbon of present embodiment, undertaken by following steps: utilize magnet that the magnetic nanometer carbon that has adsorbed humic acid is reclaimed, then the magnetic nanometer carbon that reclaims is placed in tube furnace, at N
2300～900 ℃ of charing 20～120min under atmosphere, then move into and to be equipped with in the container of 50mL deionized water, then carry out water-bath 25～35min at the temperature of 50 ℃, stir simultaneously, then after drying, namely complete the renovation process of magnetic nanometer carbon.
Embodiment nine: what present embodiment was different from embodiment eight is: N
2Flow be 100mL/min.Other is identical with embodiment eight.
Embodiment ten: what present embodiment was different from embodiment eight or nine is: dry in temperature being dry 24h in the air dry oven of 50 ℃.Other is identical with embodiment eight or nine.
By following verification experimental verification beneficial effect of the present invention:
The method of humic acid and the renovation process of magnetic nanometer carbon in test 1, this test magnetic Nano carbon removal water, undertaken by following steps: after one, the orange epidermis face impurity of drying being cleaned out, taking 100g orange skin and iron(ic) chloride and be in mass ratio 1: 1 mixes, put into tube furnace after 100 ℃ of dry 24h, at N
2(100mL/min) 900 ℃ of charing 1h under atmosphere; The product that obtains is cleaned 2h, the magnetic nanometer carbon that then obtains preparing after 100 ℃ of dry 24h in 80 ℃ of deionized waters; Two, take the 1g magnetic nanometer carbon and add (adjusting pH value is in 9 left and right) in the solution that is dissolved with the 50mg humic acid, then at 20 ℃ of lower constant temperature oscillation 30min; Three, utilize magnet that the magnetic nanometer carbon in step 2 is reclaimed, then the magnetic nanometer carbon that reclaims is placed in tube furnace, at N
2The lower 500 ℃ of charing 30min of atmosphere, then move into and to be equipped with in the container of 50mL deionized water, then carry out water-bath 30min at the temperature of 50 ℃, stir simultaneously, then after drying, namely complete the renovation process of magnetic nanometer carbon.This test adopts hydrochloric acid or sodium hydroxide to regulate pH.
The X-ray diffraction spectrogram of the magnetic nanometer carbon of this testing sequence one preparation as shown in Figure 1, main diffraction peak and Fe in spectrogram
3O
4The peak position of (JCPDS card No.75-1609) is consistent, and the Fe on carbon material is described
3O
4Be face-centred cubic structure.Fig. 2 is the X-ray diffraction spectrogram of the magnetic nanometer carbon of regeneration in this testing sequence three, can find out main crystalline phase or the Fe of reconstituted product
3O
4, basically identical with all peak positions of untapped magnetic Nano carbon products in Fig. 1.
The method of humic acid and the renovation process of magnetic nanometer carbon in test 2, this test magnetic Nano carbon removal water, undertaken by following steps: after one, the orange epidermis face impurity of drying being cleaned out, taking 100g orange skin and iron(ic) chloride and be in mass ratio 1: 1 mixes, put into tube furnace after 100 ℃ of dry 24h, at N
2(100mL/min) 900 ℃ of charing 1h under atmosphere; The product that obtains is cleaned 2h, the magnetic nanometer carbon that then obtains preparing after 100 ℃ of dry 24h in 80 ℃ of deionized waters; Two, in being the solution of humic acid of 10mg/L, 20mg/L, 40mg/L, 60mg/L, 80mg/L, 100mg/L, 120mg/L and 150mg/L, concentration adds 1g magnetic nanometer carbon (regulating the pH value in 9 left and right) respectively, then at 20 ℃ of lower constant temperature oscillation 30min; Three, utilize magnet that the magnetic nanometer carbon in step 2 is reclaimed, then the magnetic nanometer carbon that reclaims is placed in tube furnace, at N
2The lower 500 ℃ of charing 30min of atmosphere, then move into and to be equipped with in the container of 50mL deionized water, then carry out water-bath 30min at the temperature of 50 ℃, stir simultaneously, then after drying, namely complete the renovation process of magnetic nanometer carbon.This test adopts hydrochloric acid or sodium hydroxide to regulate pH.
The adsorption test result of this testing sequence two as shown in Figure 3, as shown in Figure 3, along with the increase of humic acid concentration used, product increases gradually to the adsorptive capacity of humic acid, until substantially near the maximum adsorption ability.This is to have the multi-stage porous gap structure of macropore, mesopore and micropore due to magnetic nanometer carbon, forms the relatively surfaces externally and internally of expansion, makes the magnetic Nano carbon material to the adsorption effect preferably that has of humic acid.
The method of humic acid and the renovation process of magnetic nanometer carbon in test 3, this test magnetic Nano carbon removal water, undertaken by following steps: after one, the orange epidermis face impurity of drying being cleaned out, taking 100g orange skin and iron(ic) chloride and be in mass ratio 1: 1 mixes, put into tube furnace after 100 ℃ of dry 24h, at N
2(100mL/min) 900 ℃ of charing 1h under atmosphere; The product that obtains is cleaned 2h, the magnetic nanometer carbon that then obtains preparing after 100 ℃ of dry 24h in 80 ℃ of deionized waters; Two, take the 1g magnetic nanometer carbon and add (adjusting pH value is in 9 left and right) in the solution that is dissolved with the 50mg humic acid, then at 20 ℃ of lower constant temperature oscillation 10～300min; Three, utilize magnet that the magnetic nanometer carbon in step 2 is reclaimed, then the magnetic nanometer carbon that reclaims is placed in tube furnace, at N
2The lower 500 ℃ of charing 30min of atmosphere, then move into and to be equipped with in the container of 50mL deionized water, then carry out water-bath 30min at the temperature of 50 ℃, stir simultaneously, then after drying, namely complete the renovation process of magnetic nanometer carbon.This test adopts hydrochloric acid or sodium hydroxide to regulate pH.
The adsorption test result of this testing sequence two as shown in Figure 4, as shown in Figure 4, the magnetic Nano carbon material is a comparatively faster process to the absorption of humic acid, just can reach the adsorptive capacity of 30mg/g within 5min,, and the reaction times when 45min, the magnetic carbon material reaches the maximum adsorption ability substantially, along with the prolongation in reaction times, the magnetic carbon material remains unchanged substantially to the adsorptive power of humic acid.
Claims (10)
1. the method for humic acid in magnetic Nano carbon removal water, the method that it is characterized in that humic acid in magnetic Nano carbon removal water is undertaken by following steps: one, the orange skin with drying is 1 with catalyzer in mass ratio: the ratio of (0.5～3) is mixed, dry 20～25h under the condition of 100 ℃, then put into tube furnace, at N
2600-1100 ℃ of charing 0.5～1.5h under atmosphere cleans 1.5～2.5h with the product that obtains in 80 ℃ of deionized waters, the magnetic nanometer carbon that then obtains preparing after dry 20～25h under the condition of 100 ℃; Two, the magnetic nanometer carbon with the step 1 preparation is added in humic acid solution, regulating pH is 5～13, then at 18～25 ℃ of lower constant temperature oscillation 10～300min, obtain adsorbing the magnetic nanometer carbon of humic acid, namely completed the method for humic acid in magnetic Nano carbon removal water.
2. the method for humic acid in magnetic Nano carbon removal water according to claim 1 is characterized in that catalyzer in step 1 is that one or more in iron(ic) chloride, iron protochloride, ferric sulfate, ferrous sulfate, iron nitrate or Iron nitrate are mixed by any ratio.
3. the method for humic acid in magnetic Nano carbon removal water according to claim 1 is characterized in that orange skin dry in step 1 and catalyzer are that the ratio of 1: 1 is mixed in mass ratio.
4. the method for humic acid in magnetic Nano carbon removal water according to claim 1 is characterized in that in step 1 dry 24h under the condition of 100 ℃.
5. the method for humic acid in magnetic Nano carbon removal water according to claim 1, is characterized in that N in step 1
2Flow be 100mL/min.
6. the method for humic acid in magnetic Nano carbon removal water according to claim 1, it is characterized in that in step 2 being 100 according to magnetic nanometer carbon and humic acid mass ratio: the ratio of (1～10) adds magnetic nanometer carbon.
7. the method for humic acid in magnetic Nano carbon removal water according to claim 1, is characterized in that adopting in step 2 hydrochloric acid or sodium hydroxide to regulate pH.
8. the renovation process of magnetic nanometer carbon as claimed in claim 1, the renovation process that it is characterized in that magnetic nanometer carbon is undertaken by following steps: utilize magnet that the magnetic nanometer carbon that has adsorbed humic acid is reclaimed, then the magnetic nanometer carbon that reclaims is placed in tube furnace, at N
2Then 300～900 ℃ of charing 20～120min under atmosphere, then move into and to be equipped with in the container of 50mL deionized water carry out water-bath 25～35min at the temperature of 50 ℃, stir simultaneously, drier, namely complete the renovation process of magnetic nanometer carbon.
9. the renovation process of magnetic nanometer carbon according to claim 8, is characterized in that N
2Flow be 100mL/min.
10. the renovation process of magnetic nanometer carbon according to claim 8 is characterized in that dry in temperature being dry 24h in the air dry oven of 50 ℃.
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Cited By (4)
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| CN103480331A (en) * | 2013-09-10 | 2014-01-01 | 兰州大学 | Biomass magnetic carbon material for degrading organic dye |
| CN105056887A (en) * | 2015-08-06 | 2015-11-18 | 广东工业大学 | Ca-supported magnetic carbon nanotube composite material and preparation method and application thereof |
| CN106040167A (en) * | 2016-05-26 | 2016-10-26 | 江苏大学 | Preparation method and application of magnetic hierarchical porous carbon material |
| CN111514868A (en) * | 2020-04-09 | 2020-08-11 | 华东师范大学 | Magnetic nano carbon, preparation method thereof and application thereof in removing micro plastic in water |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103480331A (en) * | 2013-09-10 | 2014-01-01 | 兰州大学 | Biomass magnetic carbon material for degrading organic dye |
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| CN105056887A (en) * | 2015-08-06 | 2015-11-18 | 广东工业大学 | Ca-supported magnetic carbon nanotube composite material and preparation method and application thereof |
| CN105056887B (en) * | 2015-08-06 | 2018-06-29 | 广东工业大学 | A kind of magnetic carbon-nano tube composite material of negative Ca and preparation method and application |
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| CN111514868A (en) * | 2020-04-09 | 2020-08-11 | 华东师范大学 | Magnetic nano carbon, preparation method thereof and application thereof in removing micro plastic in water |
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