CN108178152A - It is a kind of can efficient absorption heavy metal ion graphite oxide aerogel preparation method - Google Patents
It is a kind of can efficient absorption heavy metal ion graphite oxide aerogel preparation method Download PDFInfo
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- CN108178152A CN108178152A CN201810170368.0A CN201810170368A CN108178152A CN 108178152 A CN108178152 A CN 108178152A CN 201810170368 A CN201810170368 A CN 201810170368A CN 108178152 A CN108178152 A CN 108178152A
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- metal ion
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- sodium alginate
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
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Abstract
The present invention relates to it is a kind of can efficient absorption heavy metal ion graphite oxide aerogel preparation method, it is made of sodium alginate, graphene oxide, glucolactone, thioacetic acid, graphene aerogel produced by the present invention has higher porosity, specific surface area and mechanical strength, and the thioacetic acid being attached on graphene aerogel and the porosity of the material cause it to Cu2+、Cd2+、Pb2+Wait metal ions that there is stronger adsorption capacity, the adsorption effect for heavy metal ion is not only greatly improved in the addition of sulphur, while eliminates the influence for adsorption effect such as pH temperature.
Description
Technical field
The invention belongs to aeroge fields, and in particular to it is a kind of can efficient absorption heavy metal ion graphene oxide airsetting
The preparation method of glue.
Background technology
Graphene be one kind by carbon atom with sp2Hydridization connects the monoatomic layer two-dimensional structure nano material to be formed, and carbon is former
Cuckoo entire row is listed in honeycomb lattice structural unit, has high-specific surface area and excellent electricity calorifics optics and mechanical characteristic
Deng.The monoatomic layer two-dimensional structure of graphene makes it show unique advantage, high-ratio surface in terms of absorption and separation material
Product makes its absorption surface far above conventional adsorbent, can quick adsorption various pollutants, such as heavy metal ion, dyestuff and organic
Pollutant etc..
The preparation of three-dimensional grapheme aeroge is typically by the use of graphene oxide as presoma, by graphene oxide in water
Stable dispersion in solution since graphene is the two-dimensional structure of both sexes conjugated polymers polyelectrolyte, has hydrophobic bottom surface
With a large amount of hydrophilic oxygen-containing group, such as carboxyl, hydroxyl, epoxy group, Van der Waals force between layers and electrostatic repulsion it is flat
Weighing apparatus makes it be stabilized in disperse system, when carrying out physical operations or adding chemical substance thereto, it will usually reduction-oxidation
Part hydrophilic radical in graphene and partial aromatic structure is restored, the hydrophilic radical at bottom surface and edge is reduced, and material is dredged
Aqueous enhancing, graphene oxide layer, which is tended to detach with solution between simultaneous oxidation graphene sheet layer, to be stacked and Van der Waals force
Effect makes to re-assembly to form new structure between lamella, also just prepares various three-dimensional graphene composite materials；By
In containing a large amount of oxygen-containing group on the edge of graphene oxide layer and basal plane, these groups are provided for graphene aerogel
Decorating site, such as the inorganic elements such as doping nitrogen phosphorus are combined with other carbon materials or are introduced metal and its oxide wherein, this
A little modifications can further improve the performance of graphene aerogel.
Invention content
The purpose of the present invention is to provide it is a kind of can efficient absorption heavy metal ion graphite oxide aerogel preparation
Method.
The technical solution adopted by the present invention to solve the technical problems is：It is a kind of can efficient absorption heavy metal ion oxidation
The preparation method of graphene aerogel, includes the following steps：
1）Sodium alginate is taken to be dissolved in deionized water, is configured to the sodium alginate aqueous solution that mass concentration is 5-7%；
2）The graphene oxide solution that mass concentration is 2-5% is prepared, by step 1）In sodium alginate aqueous solution add in oxidation stone
In black alkene solution, then magnetic agitation 1-2 hours adds in glucolactone, is warming up to 40-50 DEG C of stirring and obtains for 30-50 minutes
Mixed liquor A；
3）To step 2）Mixed liquor A in add in thioacetic acid, be warming up to 70-80 DEG C react 2-4 hours；
4）After reaction, ultrasonic 20min, is washed with deionized water, and repeats ultrasound, water-washing step 3 times；
5）It is placed in freeze drier and obtains graphite oxide aerogel within 36-48 hours in -20 DEG C of freeze-dryings.
Specifically, the mass ratio of the sodium alginate and graphene oxide is 1:8-1:15.
Specifically, the addition of the glucolactone is the 0.5-2% of graphene oxide quality.
Specifically, the addition of the thioacetic acid is the 3-10% of graphene oxide quality.
The invention has the advantages that：Graphene aerogel produced by the present invention has higher porosity, compares table
The porosity of area and mechanical strength, the thioacetic acid being attached on graphene aerogel and the material causes it to Cu2+、Cd2 +、Pb2+Wait metal ions that there is stronger adsorption capacity, the suction for heavy metal ion is not only greatly improved in the addition of sulphur
Attached effect, while eliminate the influence for adsorption effect such as pH temperature.
Specific embodiment
The following is specific embodiments of the present invention, and technical scheme of the present invention is described further, but the present invention
Protection domain is not limited to these embodiments.It is every to be included in the present invention without departing substantially from the change of present inventive concept or equivalent substitute
Protection domain within.
Embodiment 1
Sodium alginate is taken to be dissolved in deionized water, is configured to the sodium alginate aqueous solution that mass concentration is 7%；
According to sodium alginate and graphene oxide 1:10 mass ratio prepares the graphene oxide solution that mass concentration is 2%, will be extra large
Alginic acid sodium water solution is added in graphene oxide solution, magnetic agitation 2 hours, is then added in and is accounted for graphene oxide quality 0.5%
Glucolactone is warming up to 45 DEG C of stirrings and obtains mixed liquor A in 50 minutes；
The thioacetic acid for accounting for graphene oxide quality 5% is added in into mixed liquor A, 80 DEG C is warming up to and reacts 3 hours；
After reaction, ultrasonic 20min, is washed with deionized water, and repeats ultrasound, water-washing step 3 times；
It is placed in freeze drier and obtains graphite oxide aerogel within 36 hours in -20 DEG C of freeze-dryings.
Embodiment 2
Sodium alginate is taken to be dissolved in deionized water, is configured to the sodium alginate aqueous solution that mass concentration is 5%；
According to sodium alginate and graphene oxide 1:8 mass ratio prepares the graphene oxide solution that mass concentration is 5%, will be extra large
Alginic acid sodium water solution is added in graphene oxide solution, magnetic agitation 1 hour, is then added in and is accounted for graphene oxide quality 1.5%
Glucolactone is warming up to 50 DEG C of stirrings and obtains mixed liquor A in 30 minutes；
The thioacetic acid for accounting for graphene oxide quality 3% is added in into mixed liquor A, 70 DEG C is warming up to and reacts 4 hours；
After reaction, ultrasonic 20min, is washed with deionized water, and repeats ultrasound, water-washing step 3 times；
It is placed in freeze drier and obtains graphite oxide aerogel within 42 hours in -20 DEG C of freeze-dryings.
Embodiment 3
Sodium alginate is taken to be dissolved in deionized water, is configured to the sodium alginate aqueous solution that mass concentration is 6%；
According to sodium alginate and graphene oxide 1:15 mass ratio prepares the graphene oxide solution that mass concentration is 3%, will be extra large
Alginic acid sodium water solution is added in graphene oxide solution, magnetic agitation 1.5 hours, is then added in and is accounted for graphene oxide quality 2%
Glucolactone is warming up to 40 DEG C of stirrings and obtains mixed liquor A in 35 minutes；
The thioacetic acid for accounting for graphene oxide quality 10% is added in into mixed liquor A, 75 DEG C is warming up to and reacts 2 hours；
After reaction, ultrasonic 20min, is washed with deionized water, and repeats ultrasound, water-washing step 3 times；
It is placed in freeze drier and obtains graphite oxide aerogel within 48 hours in -20 DEG C of freeze-dryings.
Embodiment 4
Sodium alginate is taken to be dissolved in deionized water, is configured to the sodium alginate aqueous solution that mass concentration is 7%；
According to sodium alginate and graphene oxide 1:12 mass ratio prepares the graphene oxide solution that mass concentration is 4%, will be extra large
Alginic acid sodium water solution is added in graphene oxide solution, magnetic agitation 2 hours, then adds in the Portugal for accounting for graphene oxide quality 1%
Grape saccharic acid lactone is warming up to 50 DEG C of stirrings and obtains mixed liquor A in 40 minutes；
The thioacetic acid for accounting for graphene oxide quality 8% is added in into mixed liquor A, 70 DEG C is warming up to and reacts 4 hours；
After reaction, ultrasonic 20min, is washed with deionized water, and repeats ultrasound, water-washing step 3 times；
It is placed in freeze drier and obtains graphite oxide aerogel within 42 hours in -20 DEG C of freeze-dryings.
Claims (4)
1. it is a kind of can efficient absorption heavy metal ion graphite oxide aerogel preparation method, which is characterized in that including with
Lower step：
1) sodium alginate is taken to be dissolved in deionized water, is configured to the sodium alginate aqueous solution that mass concentration is 5-7%；
2) graphene oxide solution that mass concentration is 2-5% is prepared, the sodium alginate aqueous solution in step 1) is added in into oxidation
In graphene solution, then magnetic agitation 1-2 hours adds in glucolactone, is warming up to 40-50 DEG C and stirs 30-50 minutes
Obtain mixed liquor A；
3) thioacetic acid is added in into the mixed liquor A of step 2), is warming up to 70-80 DEG C and reacts 2-4 hours；
4) after reaction, ultrasonic 20min, is washed with deionized water, and repeats ultrasound, water-washing step 3 times；
5) it is placed in freeze drier and obtains graphite oxide aerogel within 36-48 hours in -20 DEG C of freeze-dryings.
2. as described in claim 1 can efficient absorption heavy metal ion graphite oxide aerogel preparation method, it is special
Sign is that the mass ratio of the sodium alginate and graphene oxide is 1:8-1:15.
3. as described in claim 1 can efficient absorption heavy metal ion graphite oxide aerogel preparation method, it is special
Sign is that the addition of the glucolactone is the 0.5-2% of graphene oxide quality.
4. as described in claim 1 can efficient absorption heavy metal ion graphite oxide aerogel preparation method, it is special
Sign is that the addition of the thioacetic acid is the 3-10% of graphene oxide quality.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108686633A (en) * | 2018-07-10 | 2018-10-23 | 济南开发区星火科学技术研究院 | A kind of attapulgite modified water purification agent of graphene oxide compound |
| CN109054111A (en) * | 2018-07-12 | 2018-12-21 | 信阳师范学院 | A kind of graphene oxide/sodium alginate composite hydrogel preparation method through modification |
| CN109607885A (en) * | 2019-02-19 | 2019-04-12 | 北京林业大学 | A kind of water treatment technology generated based on graphene-based material absorption/catalysis oxidation step coupling control bromate |
| CN110817849A (en) * | 2019-11-29 | 2020-02-21 | 无锡市惠山区川大石墨烯应用研究中心 | Sulfhydrylation graphene aerogel and preparation method and application thereof |
| CN110975834A (en) * | 2019-12-19 | 2020-04-10 | 浙江工业大学 | Ultra-light floatable material and preparation method and application thereof |
| CN111014275A (en) * | 2019-12-19 | 2020-04-17 | 江苏华东新能源勘探有限公司（江苏省有色金属华东地质勘查局八一三队） | Heavy metal soil remediation agent and application thereof |
| CN111495324A (en) * | 2020-05-25 | 2020-08-07 | 海泰纺织（苏州）有限公司 | Preparation method of porous aerogel composite material and porous aerogel composite material |
| CN115212868A (en) * | 2022-08-31 | 2022-10-21 | 四川大学 | Nano metal particle loaded reduced graphene oxide aerogel and preparation method thereof |
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| CN104069815A (en) * | 2014-07-22 | 2014-10-01 | 西南民族大学 | Sulfur doped grapheme foam, preparation method thereof and sewage treatment method employing same |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108686633A (en) * | 2018-07-10 | 2018-10-23 | 济南开发区星火科学技术研究院 | A kind of attapulgite modified water purification agent of graphene oxide compound |
| CN109054111A (en) * | 2018-07-12 | 2018-12-21 | 信阳师范学院 | A kind of graphene oxide/sodium alginate composite hydrogel preparation method through modification |
| CN109607885A (en) * | 2019-02-19 | 2019-04-12 | 北京林业大学 | A kind of water treatment technology generated based on graphene-based material absorption/catalysis oxidation step coupling control bromate |
| CN110817849A (en) * | 2019-11-29 | 2020-02-21 | 无锡市惠山区川大石墨烯应用研究中心 | Sulfhydrylation graphene aerogel and preparation method and application thereof |
| CN110975834A (en) * | 2019-12-19 | 2020-04-10 | 浙江工业大学 | Ultra-light floatable material and preparation method and application thereof |
| CN111014275A (en) * | 2019-12-19 | 2020-04-17 | 江苏华东新能源勘探有限公司（江苏省有色金属华东地质勘查局八一三队） | Heavy metal soil remediation agent and application thereof |
| CN111014275B (en) * | 2019-12-19 | 2021-07-02 | 江苏华东新能源勘探有限公司（江苏省有色金属华东地质勘查局八一三队） | Heavy metal soil remediation agent and application thereof |
| CN110975834B (en) * | 2019-12-19 | 2022-03-25 | 浙江工业大学 | Ultra-light floatable material and preparation method and application thereof |
| CN111495324A (en) * | 2020-05-25 | 2020-08-07 | 海泰纺织（苏州）有限公司 | Preparation method of porous aerogel composite material and porous aerogel composite material |
| CN115212868A (en) * | 2022-08-31 | 2022-10-21 | 四川大学 | Nano metal particle loaded reduced graphene oxide aerogel and preparation method thereof |
| CN115212868B (en) * | 2022-08-31 | 2023-08-18 | 四川大学 | Nano metal particle loaded reduced graphene oxide aerogel and preparation method thereof |
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