CN109513422A - A kind of graphene oxide modified activated carbon and preparation method thereof - Google Patents
A kind of graphene oxide modified activated carbon and preparation method thereof Download PDFInfo
- Publication number
- CN109513422A CN109513422A CN201811396279.4A CN201811396279A CN109513422A CN 109513422 A CN109513422 A CN 109513422A CN 201811396279 A CN201811396279 A CN 201811396279A CN 109513422 A CN109513422 A CN 109513422A
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- Prior art keywords
- graphene oxide
- activated carbon
- agent
- modified activated
- oxide modified
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- 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
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/283—Treatment of water, waste water, or sewage by sorption using coal, charred products, or inorganic mixtures containing them
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
Abstract
The invention discloses a kind of graphene oxide modified activated carbons and preparation method thereof.The water body dispersion liquid of graphene oxide is made after first mixing graphene oxide, auxiliary agent, coupling agent and water；Then water body dispersion liquid that granular activated carbon is immersed to the graphene oxide is reacted by high-speed stirred and heating and graphene oxide modified activated carbon is made；It is by action of coupling agents that graphene oxide is immobilized in the hollow of active carbon, macroporous structure using thermosetting method after filtering by graphene oxide modified activated carbon obtained, clean, dry.The graphene oxide modified activated carbon prepared in this approach remains the conventional absorbtion efficiency of active carbon, while improving it and filtering out efficiency to heavy metal ion, polar organic matter；In addition, graphene oxide is immobilized on the porous structure of active carbon, it is not likely to produce the risk of leakage, there is very high safety, can be widely applied in all kinds of Water warfare products.
Description
Technical field
The present invention relates to Water warfare fields more particularly to a kind of graphene oxide modified activated carbon and preparation method thereof.
Background technique
In recent years, heavy metal pollution event takes place frequently, and according to environmental protection administration's data, Environmental Protection in China department in 2009 is informed of a case with much money
Category, metalloid contamination accident 12 rise, and cause 4035 people's blood leads exceeded, 182 people's cadmiums are exceeded, cause 32 social events.Hair recently
Raw Guangxi Longjiang river cadmium pollution event, pollution level is unprecedented, and heavy metal pollution problem is pushed into forward position.Heavy metal refers mainly to
Lead, mercury, arsenic, chromium etc., bio-toxicity is significant, does great harm to human body, calomel poisoning can cause headache, dizziness, insomnia, amnesia,
The symptoms such as amentia, arthralgia, severe intoxication is by carcinogenic teratogenesis.Currently, in all parts of the country is even more numerous cancer villages occur,
Heavy metal pollution problem is extremely serious, and government department pays much attention to this, and the prevention and treatment of heavy metal pollution is imperative.At these water
Reason technology includes desalination, all kinds of trace toxic heavy metals and purification of all kinds of organic pollutants of seawater or salt lake saline etc..With
The continuous improvement of living standard, Drinking Water health and safety have been to be concerned by more and more people and pay attention to, China's water purification row
Industry rapidly develops, and possesses potential hundred billion grades of market scale, all kinds of water purification products arise therewith.
Active carbon is the common filtrate in Water warfare field, has and decolourizes, de-tastes, except the multiple efficacies of chlorine residue, but right
Heavy metal to filter out efficiency bad.
Graphene oxide is the oxide of graphene, and it is a kind of nano particle, under normal conditions with one that color, which is brown color,
The loose micron powder morphology of kind reunion exists, and surface has numerous epoxy groups, hydroxyl and carboxyl, has stronger absorption
Property, the micropollutants such as adsorbable a large amount of organic matter, heavy metal ion, but powdered graphene oxide is in water purification product
It can not accomplish commercialization in, cannot be efficiently used.
Summary of the invention
Problem to be solved by this invention is aiming at the problems and shortcomings existing in the prior art, to provide a kind of oxidation stone
Black alkene modified activated carbon will using functional groups such as porous structure and the activated carbon surface hydroxyl abundant of active carbon, carbonyls
Graphene oxide powder material and coupling agent carry out the pre-dispersed water body dispersion liquid that graphene oxide is made, and pass through agitating and heating
Mode, by graphene oxide particle insertion active carbon porous structure in；Again by graphene oxide modified activated carbon obtained
It filtered, dried, under heating conditions, by action of coupling agents by the immobilized mesoporous in active carbon of graphene oxide, big
In pore structure.
To achieve the above object, the present invention is the following technical schemes are provided: a kind of graphene oxide modified activated carbon, feature
It is, graphene oxide is embedded into and immobilized in the mesoporous, macroporous structure of active carbon by action of coupling agents.
Further, a kind of graphene oxide modified activated carbon preparation method the following steps are included:
(1) it prepares the water body dispersion liquid of graphene oxide: graphene oxide, auxiliary agent, coupling agent and water is mixed to prepare oxygen
The water body dispersion liquid of graphite alkene；
(2) it prepares graphene oxide modified activated carbon: granular activated carbon is immersed into graphite oxide made from the step (1)
In the water body dispersion liquid of alkene, high-speed stirred, heating reaction are carried out under the conditions of 60-150 DEG C of temperature, the time is 2-48 hours；
(3) immobilized graphene oxide modified activated carbon: graphene oxide modified activated carbon obtained in step (2) is carried out
After filtering, clean, drying, pass through action of coupling agents for the immobilized mesoporous in active carbon of graphene oxide, macropore using thermosetting method
In structure, the heating temperature of the thermosetting method is 60-150 DEG C, and heating time is 30min to for 24 hours.
It is further limited as of the invention, in the preparation method step (1), prepares the dispersion of graphene oxide water body
The dispersing method of liquid includes ultrasonic wave, high-speed stirred, ball grinding stirring, heating etc..
It is further limited as of the invention, the auxiliary agent is surfactant, defoaming agent, dispersing agent, chelating agent and increasing
At least one of thick dose；
It is further limited as of the invention, the surfactant is dodecyl sodium sulfate, lauryl sulfosuccinate
At least one of acid monoester disodium, stearic acid and fatty glyceride；
It is further limited as of the invention, the defoaming agent is glycerol trihydroxy polyethers, dimethyl silicone polymer, spiceleaf
At least one of alkene and firpene；
It is further limited as of the invention, the dispersing agent is calgon, sodium polyphosphate, white oil and methylene
At least one of sodium naphthalene sulfonate；
It is further limited as of the invention, the chelating agent is citric acid, tartaric acid, fumaric acid, polymethylacrylic acid
At least one of with polyacrylic acid；
It is further limited as of the invention, the thickener is that sodium carboxymethylcellulose, sodium alginate and ethoxy are fine
Tie up at least one of element.
It is further limited as of the invention, the coupling agent includes silane coupling agent, titanate coupling agent, Aluminate idol
Join at least one of agent, bimetallic coupling agent, lignin coupling agent and tin coupling agent；Preferably, the coupling agent is silane
Coupling agent and/or titanate coupling agent.
Compared with prior art, the beneficial effects of the present invention are:
A kind of graphene oxide modified activated carbon of the present invention and preparation method thereof, because of graphene oxide powder material
First pass through in advance it is fully dispersed, and by way of high-speed stirred, heating, by stannic oxide/graphene nano particle insertion active carbon
In mesoporous, macroporous structure, and it is using the effect of coupling agent that graphene oxide is immobilized in the mesoporous, macroporous structure of active carbon,
Fixed graphene oxide is not easy to fall off from active carbon, ensures that the security performance of modified activated carbon, effectively solves
The safety issue of graphene oxide leakage.In addition, graphene oxide is embedded into, the immobilized mesoporous in active carbon, macropore knot
In structure, it in this way can greatly improve active carbon and efficiency is filtered out to heavy metal, organic matter.
Detailed description of the invention
Fig. 1 is the preparation technology flow chart of graphene oxide modified activated carbon of the invention.
Specific embodiment
In order to facilitate the understanding of those skilled in the art, below in conjunction with accompanying drawings and embodiments to technical solution of the present invention make into
One step understands, detailed complete describes, it is clear that described embodiment is served only for that the present invention is further illustrated, cannot
It is interpreted as limiting the scope of the invention.Based on the embodiments of the present invention, those skilled in the art is according to above-mentioned hair
Bright content makes some nonessential changes and adjustment, all belongs to the scope of protection of the present invention.
Embodiment 1
The preparation of graphene oxide water body dispersion liquid
After graphene oxide, auxiliary agent, coupling agent and water are mixed, pass through strength ultrasound and high-speed stirred preparation at 80 DEG C
10 liters fresh of graphene oxide water body dispersion liquid, wherein the auxiliary agent is dodecyl sodium sulfate, and coupling agent is (3- amino
Propyl) dimethylethoxysilane；The average grain diameter of graphene oxide powder in the graphene oxide water body dispersion liquid is
0.1 micron, the content of graphene oxide is 5mM, and dodecyl sodium sulfate content is 1.0mM, (3- aminopropyl) dimethyl second
Oxysilane content is 10.0mM.The graphene oxide water body dispersion liquid prepared with this is stood 72 hours and deposited phenomenon does not occur
Occur.
Embodiment 2
The preparation of graphene oxide modified activated carbon
30-70 mesh granular activated carbon 2kg (active carbon iodine number 1050) is taken, graphene oxide prepared by embodiment 1 is immersed
In water body dispersion liquid, high-speed stirred, reaction 5 hours at 80 DEG C are filtered, clean, drying and is (modified after standing cooling
Active carbon moisture content is less than 30%), then the baking oven high temperature placed it at 180 DEG C solidifies 12 hours, can be obtained graphite oxide
Alkene modified activated carbon.
Embodiment 3
Regular activated filtration core A1 and graphene oxide modified active filtration core B1 dechlorination efficiency evaluation and test
200 grams of granular activated carbons (30-70 mesh), graphene oxide modified activated carbon (30-70 mesh) are taken to be packaged in greatly respectively
In T33, the challenge water that configuration contents of residual chlorine is 2.0ppm tests regular activated filtration core A1 and oxidation under 0.2bar pressure
The chlorine residue of graphene modified active filtration core B1 removes efficiency, and survey water inventory is 3000L.Test experiments result such as the following table 1:
Table 1:A1 and B1 chlorine residue removal rate experimental data
| It surveys water flow (L) | The chlorine residue removal rate (%) of A1 | The chlorine residue removal rate (%) of B1 |
| 5 | 99 | 99 |
| 500 | 97 | 97 |
| 1000 | 90 | 92 |
| 2000 | 75 | 80 |
| 3000 | 60 | 68 |
It can be seen that regular activated filtration core A1 and graphite oxide modified active filtration core B1 all from 1 experimental data of table
Efficiency is removed with good chlorine residue, the chlorine residue of the more regular activated filtration core A1 of graphene oxide active carbon filter core B1 removes effect
It can slightly be promoted.
Embodiment 4
The lead ion removal efficiency evaluation and test of regular activated filtration core A1 and graphene oxide modified active filtration core B1
The challenge water (note: lead is limited to 10ppb in national drinking water standard) that lead content is 100ppb is configured,
Under 0.2bar pressure, the lead ion removal effect of regular activated filtration core A1 and graphene oxide modified active filtration core B1 is tested
Can, survey water inventory is 3000L.Test experiments result such as the following table 2:
Table 2:A1 and B1 lead ion removal rate experimental data
| It surveys water flow (L) | The lead ion removal rate (%) of A1 | The lead ion removal rate (%) of B1 |
| 5 | 15 | 99 |
| 500 | 5 | 97 |
| 1000 | 0 | 95 |
| 2000 | 68 | 92 |
| 3000 | 33 | 87 |
Terminal is imitated by the filter of filter core of 90% lead ion removal rate in the embodiment of the present invention 4, it can from 2 experimental data of table
To find out, regular activated filtration core A1 cannot remove lead ion substantially, and when reaching efficient endpoint, graphene oxide is modified to live
Property filtration core B1 it is very good to the removal efficiency of lead ion, to lead content be 100ppb challenge water the amount of filtering out up to 3000L.
It although an embodiment of the present invention has been shown and described, for the ordinary skill in the art, can be with
Understand without departing from the principles and spirit of the present invention can to the present embodiment carry out it is a variety of variation, modification, replacement and
Modification, the scope of the present invention is defined by the appended.
Claims (5)
1. a kind of graphene oxide modified activated carbon, which is characterized in that graphene oxide is by action of coupling agents by immobilized in work
In the mesoporous of property charcoal, macroporous structure.
2. a kind of preparation method of graphene oxide modified activated carbon described in claim 1, which is characterized in that including following step
It is rapid:
(1) it prepares the water body dispersion liquid of graphene oxide: graphene oxide, auxiliary agent, coupling agent and water is mixed to prepare oxidation stone
The water body dispersion liquid of black alkene；
(2) it prepares graphene oxide modified activated carbon: granular activated carbon is immersed into graphene oxide made from the step (1)
In water body dispersion liquid, high-speed stirred, heating reaction are carried out under the conditions of 60-150 DEG C of temperature, the time is 2-48 hours；
(3) immobilized graphene oxide modified activated carbon: graphene oxide modified activated carbon obtained in step (2) is taken out
After filtering, clean, drying, pass through action of coupling agents for the immobilized mesoporous in active carbon of graphene oxide, macropore knot using thermosetting method
In structure, the heating temperature of the thermosetting method is 60-150 DEG C, and heating time is 30min to for 24 hours.
3. a kind of preparation method of graphene oxide modified activated carbon according to claim 2, which is characterized in that prepare oxygen
The dispersing method of the water body dispersion liquid of graphite alkene includes ultrasonic wave, high-speed stirred, ball grinding stirring, heating etc..
4. a kind of preparation method of graphene oxide modified activated carbon according to claim 2, which is characterized in that described to help
Agent is at least one of surfactant, defoaming agent, dispersing agent, chelating agent and thickener；
The surfactant is that dodecyl sodium sulfate, lauryl sulfosuccinic acid monoester disodium, stearic acid and fatty acid are sweet
At least one of grease；
The defoaming agent is at least one of glycerol trihydroxy polyethers, dimethyl silicone polymer, myrcene and firpene；
The dispersing agent is at least one of calgon, sodium polyphosphate, white oil and methanonaphthalene sodium sulfonate；
The chelating agent is at least one of citric acid, tartaric acid, fumaric acid, polymethylacrylic acid and polyacrylic acid；
The thickener is at least one of sodium carboxymethylcellulose, sodium alginate and hydroxyethyl cellulose.
5. a kind of preparation method of graphene oxide modified activated carbon according to claim 2, which is characterized in that the idol
Connection agent includes that silane coupling agent, titanate coupling agent, aluminate coupling agent, bimetallic coupling agent, lignin coupling agent and tin are even
Join at least one of agent；Preferably, the coupling agent is silane coupling agent and/or titanate coupling agent.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201811396279.4A CN109513422A (en) | 2018-11-19 | 2018-11-19 | A kind of graphene oxide modified activated carbon and preparation method thereof |
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| CN201811396279.4A CN109513422A (en) | 2018-11-19 | 2018-11-19 | A kind of graphene oxide modified activated carbon and preparation method thereof |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110127697A (en) * | 2019-05-23 | 2019-08-16 | 东南大学 | A method of can be prepared on a large scale modified activated carbon |
| CN110339670A (en) * | 2019-07-15 | 2019-10-18 | 北京绿能嘉业新能源有限公司 | A kind of graphene composite material and preparation method thereof containing negative oxygen ion |
| CN110496449A (en) * | 2019-09-24 | 2019-11-26 | 广州康滤净化科技有限公司 | A kind of graphene scale inhibition composite filter element and preparation method thereof |
| CN111170307A (en) * | 2020-01-14 | 2020-05-19 | 中国科学院苏州纳米技术与纳米仿生研究所南昌研究院 | Nano-carbon modified hollow activated carbon micro-tube and preparation method and application thereof |
| CN113000023A (en) * | 2021-03-04 | 2021-06-22 | 上海晶宇环境工程股份有限公司 | Graphene oxide modified activated carbon, preparation method thereof and water treatment method |
| CN113769716A (en) * | 2021-07-05 | 2021-12-10 | 昆明理工大学 | Preparation method and application of novel rubber seed shell-based composite material |
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2018
- 2018-11-19 CN CN201811396279.4A patent/CN109513422A/en active Pending
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110127697A (en) * | 2019-05-23 | 2019-08-16 | 东南大学 | A method of can be prepared on a large scale modified activated carbon |
| CN110127697B (en) * | 2019-05-23 | 2022-10-14 | 东南大学 | Method for preparing modified activated carbon in large scale |
| CN110339670A (en) * | 2019-07-15 | 2019-10-18 | 北京绿能嘉业新能源有限公司 | A kind of graphene composite material and preparation method thereof containing negative oxygen ion |
| CN110496449A (en) * | 2019-09-24 | 2019-11-26 | 广州康滤净化科技有限公司 | A kind of graphene scale inhibition composite filter element and preparation method thereof |
| CN111170307A (en) * | 2020-01-14 | 2020-05-19 | 中国科学院苏州纳米技术与纳米仿生研究所南昌研究院 | Nano-carbon modified hollow activated carbon micro-tube and preparation method and application thereof |
| CN111170307B (en) * | 2020-01-14 | 2023-04-28 | 江西省纳米技术研究院 | Nanocarbon modified hollow activated carbon microtube and preparation method and application thereof |
| CN113000023A (en) * | 2021-03-04 | 2021-06-22 | 上海晶宇环境工程股份有限公司 | Graphene oxide modified activated carbon, preparation method thereof and water treatment method |
| CN113769716A (en) * | 2021-07-05 | 2021-12-10 | 昆明理工大学 | Preparation method and application of novel rubber seed shell-based composite material |
| CN113769716B (en) * | 2021-07-05 | 2023-11-10 | 昆明理工大学 | Preparation method and application of novel rubber seed shell-based composite material |
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Application publication date: 20190326 |