CN107570118A - A kind of preparation method and applications of sulfur doping graphene aerogel - Google Patents
A kind of preparation method and applications of sulfur doping graphene aerogel Download PDFInfo
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- CN107570118A CN107570118A CN201711082862.3A CN201711082862A CN107570118A CN 107570118 A CN107570118 A CN 107570118A CN 201711082862 A CN201711082862 A CN 201711082862A CN 107570118 A CN107570118 A CN 107570118A
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Abstract
The present invention is more particularly directed to a kind of preparation method and applications of sulfur doping graphene aerogel, the waste water of complex state heavy metal ion is contained especially suitable for advanced treating.Sulfide of the present invention grafting with sequestering power, heavy metal can produce chelating suction-operated, effective to provide heavy metal complexing power.Beneficial effect of the present invention：Sulfur doping graphene aerogel specific surface area is big, high mechanical strength, can carry out depth absorption to complexation heavy metal ion.
Description
Technical field
The present invention is more particularly directed to a kind of preparation method and applications of sulfur doping graphene aerogel, especially suitable for depth
Handle the waste water containing complex state heavy metal ion.
Background technology
Heavy metal is a great problem handled in waste water, and waste water caused by a variety of industries contains heavy metal ion, such as
Plating, electronics, petrochemical industry, smelting, non-ferrous metals processing etc..In heavy metal containing wastewater treatment, heavy metal ion shows as two kinds of shapes
State, a kind of free state, a kind of complex state.The heavy metal ion of free state can be by adding sodium hydroxide or vulcanized sodium and its
Reaction generation sediment, is thoroughly removed from waste water.And for the heavy metal ion of complex state, particularly with amino or sulfydryl
The heavy metal ion of complexing can not effectively be removed using the above method from waste water.The advanced treating of complex state heavy metal ion
It is the development trend that heavy metal wastewater thereby is administered.
As increasing enterprise and regional requirements perform GB21900-2008《Electroplate pollutant emission standard》Middle table
Three standards, this standard heavy metal have higher requirement.For example it is less than 0.1mg/L for Ni requirements, require low for Cd
In 0.01mg/L.The index of this kind of heavy metal has gone the limit of removing heavy metals far below addition medicament.For complex state
Ni, adding chemical agent sometimes can not all cause Ni to be less than 0.5mg/L.
For extremely low heavy metal concentration, it usually needs add excessive several times, or even the medicament of decades of times to ensure reaction
Forward direction is carried out.To ensure the heavy metal ion of extremely low concentration, crash response can be carried out with remover in waste water.Based on this
One principle, the mode of the removal fixed bed for heavy metal often react more effective than adding medicine into waste water.Also not simultaneously
The problem of medicament can be caused excessively to introduce new pollutant in waste water too much.Another can be exactly to improve material in an improved way
The specific surface area of material, in same volume, the surface area of carrier is bigger, and the functional group being grafted is more, for heavy metal
Adsorption capacity is stronger.
The present invention utilizes the extra specific surface area of graphene aerogel, and the surface functional group of graphene aerogel is carried out
Modified, sulfide of the grafting with sequestering power, heavy metal can produce chelating suction-operated, the effective network for improving heavy metal
Conjunction ability, so as to realize the removal of the depth of heavy metal.Compared to traditional resin material, graphene aerogel has bigger
Specific surface area, the problem of higher mechanical strength is not in material efflorescence.This technology is particularly complexed weight for heavy metal
The removal of metal ion has remarkable result.
The content of the invention
For many deficiencies of the prior art, it is an object of the invention to provide a kind of sulfur doping graphene aerogel
Preparation method, the technical scheme that it is used are as follows：A kind of sulfur doping graphene aerogel, it is characterised in that：
1. a kind of preparation method for mixing sulfur graphite alkene aeroge, it is characterised in that comprise the following steps
Step a. takes 1-20g graphene oxide to be scattered in 1000ml deionized waters, ultrasonic 4-24 hours；
Step b. is measured in 100-600ml alcoholic solution steps for importing a graphene oxide solution, stirs 1-5 hours；
Step c. adds 20-60ml sulphur solution, and be gradually added 30-80ml liquid caustic soda after step b mixed liquor is completely dispersed
Solution, stir 0.5-5 hours；
Solution obtained by step c is transferred to reactor by step d., and constant temperature continues to react 2-8 hours under conditions of 50-150 DEG C,
After question response kettle temperature degree is cooled to room temperature, after solution is filtered, filter cake is washed with deionized three times, then washs one with alcohol
Time, obtain mixing sulfur graphite alkene aeroge.
Alcoholic solution described in described step b and step d is absolute ethyl alcohol or isopropanol.
Sulphur solution described in described step c is carbon disulfide or dithiothreitol (DTT).
The beneficial effects of the invention are as follows：
The sulfur graphite alkene aeroge of mixing of the present invention has that specific surface area is big, and total grafted functional group quantity is more, takes fixed bed
Form heavy metal ion is adsorbed, and there is heavy metal ion very big probability to be reacted with functional groups, so as to
Realize that the depth of heavy metal ion removes.The hydrochloric acid solution backwash mixed sulfur graphite alkene aeroge and use 5% of absorption heavy metal,
And regenerated using 8% sodium hydroxide solution, the waste water after regeneration is based on the chloride of heavy metal, using sodium hydroxide
Heavy metals removal in regeneration liquid waste can be returned directly to regulating reservoir and be handled, it is outer without being entrusted as hazardous waste
Processing.
It is big that prepared by the processing method mix sulfur graphite alkene aeroge specific surface area, and the absorption of complexation heavy metal ion depth is gone
Removing solid capacity is strong, and total heavy metal adsorption capacity is big.
Embodiment
With reference to embodiments, the present invention is elaborated, but protection scope of the present invention is not limited to following embodiments,
The simple equivalent changes and modifications made in every case with scope of the present invention patent and description, all still belong to the present invention
Within covering scope.
Embodiment 1：
Nickel and complexing copper waste water are complexed, former technique is using ferrous sulfate+vulcanized sodium processing, the ton day of water 500, former water outlet nickel
0.53mg/L, copper 0.36mg/L, after being handled using graphene aerogel, the ton day of water 500, reveal water nickel 0.03mg/L, water outlet
Copper does not detect.
Embodiment 2：
Chemical nickel plating rinse water, former technique are handled using heavy metal chelating agent, the ton day of water 20, former water outlet nickel 0.3mg/L, adopted
After being handled with graphene aerogel, the ton day of water 20, reveal water nickel 0.02mg/L.
Embodiment 3：
Electroplating washing water, former technique are handled using vulcanized sodium, the ton day of water 800, former water outlet cadmium 0.05mg/L, using graphene
After aeroge processing, the ton day of water 800, reveal water cadmium 0.004mg/L.
Embodiment 4：
Percolate, former technique are handled using vulcanized sodium, the ton day of water 60, former water outlet mercury 0.02mg/L, using graphene gas
After Gel Treatment, the ton day of water 60, reveal water and do not detect.
Embodiment 5：
Steel stainless steel acid cleaning waste water, former technique are handled using vulcanized sodium, the ton day of water 2500, former water outlet nickel 0.3mg/L, adopted
After being handled with graphene aerogel, the ton day of water 2500, reveal water nickel 0.002mg/L.
Claims (3)
1. a kind of preparation method for mixing sulfur graphite alkene aeroge, it is characterised in that comprise the following steps：
A. 1-20g graphene oxide is taken to be scattered in 1000ml deionized waters, ultrasonic 4-24 hours；
B. in the graphene oxide solution for measuring 100-600ml alcoholic solution steps for importing a, 1-5 hours are stirred；
C. after step b mixed liquor is completely dispersed, 20-60ml sulphur solution is added, and is gradually added 30-80ml liquid caustic soda solution,
Stir 0.5-5 hours；
D. the solution obtained by step c is transferred to reactor, constant temperature continues to react 2-8 hours under conditions of 50-150 DEG C, treats anti-
After answering kettle temperature degree to be cooled to room temperature, after solution is filtered, filter residue is washed with deionized three times, is then washed one time, obtained with alcohol
To mixing sulfur graphite alkene aeroge.
2. the preparation method for mixing sulfur graphite alkene aeroge according to claim 1, it is characterised in that the step b and
Alcoholic solution described in step d is absolute ethyl alcohol or isopropanol.
3. the preparation method for mixing sulfur graphite alkene aeroge according to claim 1, it is characterised in that institute in the step c
The sulphur solution stated is carbon disulfide or dithiothreitol (DTT).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201711082862.3A CN107570118A (en) | 2017-11-07 | 2017-11-07 | A kind of preparation method and applications of sulfur doping graphene aerogel |
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| CN201711082862.3A CN107570118A (en) | 2017-11-07 | 2017-11-07 | A kind of preparation method and applications of sulfur doping graphene aerogel |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108585104A (en) * | 2018-05-22 | 2018-09-28 | 武汉材料保护研究所有限公司 | A kind of processing method of the waste water containing Ni |
| CN110280218A (en) * | 2019-06-27 | 2019-09-27 | 济南大学 | A kind of preparation method of dithiothreitol (DTT) modified magnetic biological adsorption agent |
| CN110711565A (en) * | 2019-09-30 | 2020-01-21 | 北京石墨烯技术研究院有限公司 | Vulcanized graphene sponge composite material and preparation method and application thereof |
| CN112877117A (en) * | 2021-01-21 | 2021-06-01 | 徐州振峰新材料科技有限公司 | Efficient low-price nano-copper/sulfur-doped graphene modified lubricating oil |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108585104A (en) * | 2018-05-22 | 2018-09-28 | 武汉材料保护研究所有限公司 | A kind of processing method of the waste water containing Ni |
| CN110280218A (en) * | 2019-06-27 | 2019-09-27 | 济南大学 | A kind of preparation method of dithiothreitol (DTT) modified magnetic biological adsorption agent |
| CN110711565A (en) * | 2019-09-30 | 2020-01-21 | 北京石墨烯技术研究院有限公司 | Vulcanized graphene sponge composite material and preparation method and application thereof |
| CN110711565B (en) * | 2019-09-30 | 2020-10-30 | 北京石墨烯技术研究院有限公司 | Vulcanized graphene sponge composite material and preparation method and application thereof |
| CN112877117A (en) * | 2021-01-21 | 2021-06-01 | 徐州振峰新材料科技有限公司 | Efficient low-price nano-copper/sulfur-doped graphene modified lubricating oil |
| CN112877117B (en) * | 2021-01-21 | 2022-09-09 | 徐州振峰新材料科技有限公司 | Efficient low-price nano-copper/sulfur-doped graphene modified lubricating oil |
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Application publication date: 20180112 |