CN108479736A - A kind of magnetic oxygenated graphene adsorbent and the preparation method and application thereof that second diene triamine is modified - Google Patents
A kind of magnetic oxygenated graphene adsorbent and the preparation method and application thereof that second diene triamine is modified Download PDFInfo
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28002—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their physical properties
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- B01J2/02—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic by dividing the liquid material into drops, e.g. by spraying, and solidifying the drops
- B01J2/06—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic by dividing the liquid material into drops, e.g. by spraying, and solidifying the drops in a liquid medium
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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Abstract
The invention discloses the magnetic oxygenated graphene adsorbents and the preparation method and application thereof that a kind of second diene triamine is modified.The preparation method introduces the ferroso-ferric oxide prepared by coprecipitation first on graphene oxide, the epoxy group or carboxyl of amino and surface of graphene oxide on second diene triamine is recycled to react, make the amino grafting and modifying graphene oxide on second diene triamine, the magnetic oxygenated graphene adsorbent of second diene triamine modification is prepared.The magnetic oxygenated graphene adsorbent that the second diene triamine of the present invention is modified is to have high adsorption capacity to heavy metal ion and be easy to the composite material separated and recovered from waste water, is had a good application prospect in the treatment of waste water to the Adsorption of heavy metal ion.
Description
Technical field
The present invention relates to the preparation metal fields of graphene composite modification material, and in particular to a kind of second diene triamine modification
Magnetic oxygenated graphene adsorbent and the preparation method and application thereof.
Background technology
Since the industrial revolution, industrialization is fast-developing, and heavy metal is excessively lost in, and is constituted to ecological environment and human health straight
Connect threat.Such as cadmium, it is one of maximum heavy metal element of toxicity, because it has mutagenicity and teratogenesis to organism
Property.Once excessive cadmium ion enters human body, main overstock will be in liver, kidney, in diarrhea and thyroid gland, leads to organ injury
And influence the normal life of the mankind.Due to cost-effectiveness and easily operated, absorption is considered as that heavy metal is removed from aqueous solution
Attractive method.Common adsorbent such as activated carbon, modified mesoporous silicon oxide, there is suctions for montmorillonite and kaolin
The shortcomings of attached ability is not high, and separation is uneven.Therefore, a kind of new fertile absorber is explored to reduce heavy metal ion in biology
Harm be highly desirable to concern.
There is graphite oxide two-dimensional framework, graphene oxide can be prepared by removing graphite oxide.In its graphite master
There are a large amount of oxygen-containing functional groups in chain:Carboxyl at sheet edge(-COOH)And carbonyl(-C = O)Group, the ring on basal plane
Oxygroup(COC)And hydroxyl(-OH), hydrophily is made it have, can be dispersed in water to form stable suspension.Therefore, it aoxidizes
Graphene(GO)Potentiality with removal heavy metal ions in wastewater.However, since adsorption group depends primarily on carboxyl and hydroxyl
Base, absorbability are restricted.Surface Oxygen functional group is easy since interaction of hydrogen bond is occupied in further adsorption process
Reunite.In addition, being difficult to detach and recycle from solution, it is easy to cause secondary pollution.These disadvantages hinder it in a removal huge sum of money
Application in terms of category.
Second diene triamine (DLTA), can be to metal due to containing a large amount of amino and imido grpup functional group in its molecule
Ion forms effective complexing, therefore has ion exchanging function, can adsorb heavy metal ion.Utilize the epoxy of amino and the surfaces GO
Base or carboxyl react and it are made to modify in succession, can increase activated adoption site, enhance its absorption property.If will
Suitable magnetic Fe3O4It is further introduced into compound system, then compound system will be easy to detach with aqueous environments.Meanwhile Fe3O4
Insertion in GO can be effectively prevented the accumulation between the graphene layer of oxidation.Therefore it prepares amino modified magnetic oxygenated
Graphene has absorption property height, and can well be detached from aqueous solution.
Invention content
In view of the above-mentioned deficiencies in the prior art, it is an object of the present invention to provide a kind of second diene triamine be modified it is magnetic oxygenated
Graphene adsorbent(DLTA-mGO).The magnetic oxygenated graphene adsorbent that the second diene triamine is modified is to have to heavy metal ion
There is high adsorption capacity and be easy to the composite material separated and recovered from waste water, in the treatment of waste water to the Adsorption of heavy metal ion
It has a good application prospect.
The present invention also aims to provide the magnetic oxygenated graphene suction for preparing a kind of second diene triamine and being modified
Attached dose of method.The preparation method is cross-linking modified to graphene oxide progress by second diene triamine, introduces amino, introduces simultaneously
Fe 3 O 4 magnetic ion, so as to get composite material have to heavy metal ion and high adsorption capacity and be easy to detach from waste water
Recycling.
Another object of the present invention, which also resides in, provides the magnetic oxygenated graphene suction that a kind of second diene triamine is modified
Attached dose of application.
The purpose of the present invention is achieved through the following technical solutions.
A kind of preparation method for the magnetic oxygenated graphene adsorbent that second diene triamine is modified, first on graphene oxide
Introduce the ferroso-ferric oxide prepared by coprecipitation(Fe3O4), recycle the amino and graphite oxide on second diene triamine (DLTA)
Alkene(GO)The epoxy group or carboxyl on surface react, and make the amino grafting and modifying graphene oxide on second diene triamine, system
It is standby to obtain the magnetic oxygenated graphene composite material of second diene triamine modification;
Specifically comprise the following steps:
(1)It adds graphene oxide into deionized water, ultrasonic disperse is uniform, obtains solution A;
(2)By FeCl under stirring2·4H2O and FeCl3·6H2O is dissolved in deionized water, obtains solution B;
(3)Solution B is slowly added to be uniformly mixed in solution A under stirring, then NH is added dropwise3·H2After O adjusts pH value, in 70~90
It DEG C persistently stirs 3~5 hours, obtains modified graphene oxide(mGO)Solution;
(4)By step(3)Second diene triamine is added in obtained modified graphene oxide solution(DLTA)In, it is held then at 50~70 DEG C
After continuous stirring 6~12 hours, wash, it is dry, obtain the magnetic oxygenated graphene adsorbent that the second diene triamine is modified
(DLTA-mGO).
Preferably, step(1)In, the mass ratio of the graphene oxide and deionized water is 0.3~0.5:100~200.
Preferably, step(2)In, the FeCl2·4H2O and FeCl3·6H2The total amount of O and the mass ratio of deionized water
It is 1:20~105.
Preferably, step(2)In, the FeCl2·4H2O and FeCl3·6H2The molar ratio of O is 1:1~2.
Preferably, step(3)In, the mixed proportion of the solution A and solution B presses graphene oxide and FeCl2·4H2O and
FeCl3·6H2The mass ratio of the total amount of O is 0.1~0.52:1 is mixed.
Preferably, step(3)In, the adjusting pH value is that adjusting pH value is 9~11.
Preferably, step(4)In, the modified graphene oxide be added the amount in second diene triamine by second diene triamine with
The liquid ratio of graphene oxide is 5~10:0.3~0.5 ml/g is added.
Preferably, step(4)In, the washing is to be washed successively with methanol and deionized water.
Preferably, step(4)In, the drying is dried in vacuo 8~24 hours at 50~70 DEG C.
A kind of magnetic oxygenated graphene suction that second diene triamine is modified made from preparation method described in any one of the above embodiments
Attached dose.
The application for the magnetic oxygenated graphene adsorbent that a kind of second diene triamine is modified, including be applied at waste water
To the Adsorption of heavy metal ion in reason.
Compared with prior art, the invention has the advantages that and advantageous effect:
(1)The magnetic oxygenated graphene adsorbent that the second diene triamine of the present invention is modified is by the way that second diene triamine to be effectively grafted to
On graphene oxide, more chemisorption sites are introduced, take full advantage of the dual suction of graphene oxide and second diene triamine
Attached ability makes the absorption property of composite material be obviously improved, and has high adsorbance to heavy metal ion, wherein to cadmium ion
Absorbance maximum reaches 108.06 mg/g;
(2)The Fe 3 O 4 magnetic particle introduced in the magnetic oxygenated graphene adsorbent that the second diene triamine of the present invention is modified
Stable dispersion has good to enable composite material that there is stable ferromagnetism, saturation magnetization to reach 28.5 emu/g
Magnetic separation separating property, solve the problems, such as sorbing material difficulty separation, easily cause secondary pollution, have environmental-friendly characteristic;
(3)The preparation method of the present invention is simple for process, and energy consumption is small, and raw material is easy to get, and is advantageously implemented industrialized production.
Description of the drawings
Fig. 1 is the preparation principle and its application original for the magnetic oxygenated graphene adsorbent that the second diene triamine of the present invention is modified
Manage schematic diagram;
Fig. 2 a and Fig. 2 b are respectively that the second diene triamine of the graphene oxide and modified preparation in embodiment 3 before modified is modified
The TEM of magnetic oxygenated graphene adsorbent schemes.
Specific implementation mode
Technical scheme of the present invention is described in further detail below in conjunction with specific embodiment and attached drawing, but the present invention
Protection domain and embodiment it is without being limited thereto.
In specific embodiment, the preparation principle of the magnetic oxygenated graphene of second diene triamine of the invention modification and its application
Principle schematic is as shown in Figure 1;
In preparation process, the ferroso-ferric oxide 2 prepared by coprecipitation is introduced first on graphene oxide 1(Fe3O4), obtain
Magnetic oxygenated graphene 3;Recycle the epoxy group or carboxylic of the amino and surface of graphene oxide on second diene triamine 4 (DLTA)
Base reacts, and makes the amino grafting and modifying graphene oxide on second diene triamine, and the magnetic of second diene triamine modification is prepared
Property graphene oxide adsorbent 5(DLTA-mGO);
Wherein, the Grafting mechanism that second diene triamine is grafted to magnetic oxygenated graphene is amino and magnetic oxygen on second diene triamine
The epoxy group or carboxyl on graphite alkene surface connect.
In application process, the magnetic oxygenated graphene adsorbent that second diene triamine is modified puts into giving up containing heavy metal ion
Absorption heavy metal ion is carried out in water, after the completion of absorption, is inhaled using the magnetic oxygenated graphene that second diene triamine is modified by magnet 6
Attached dose separates and recovers from waste water.
Embodiment 1
The preparation for the magnetic oxygenated graphene adsorbent that second diene triamine is modified, is as follows:
(1)0.3 g GO are gradually added into 100g deionized waters, is then ultrasonically treated 1 hour, obtains solution A;
(2)Under stirring, by FeCl2·4H2O (0.257g) and FeCl3·6H2O (0.699g) is dissolved in the deionized water of 100mL
In, obtain mixed solution B;
(3)Then solution B is slowly added into solution A, NH is then added dropwise3·H2O by pH to be adjusted to 9, by mixed solution
It is maintained at 70 DEG C and continues stirring 5 hours, obtain mGO solution;
(4)By step(3)Second diene triamine is added in obtained mGO solution(5mL)In, it is stirred continuously 12 hours in 50 DEG C, then
It is washed with methanol and deionized water, is dried in vacuo 24 hours at 50 DEG C successively, obtain the magnetic oxygenated of second diene triamine modification
Graphene adsorbent(DLTA-mGO).
The magnetic oxygenated graphene adsorbent absorption input concentration of cadmium ions that the second diene triamine of preparation is modified is 50mg/
In the waste water of L, adsorbed 3 hours under the conditions of pH=5, adsorbance 86.7mg/g;After absorption, using magnet to adsorbent
It is separated and recovered, intensity of magnetization 28.5emu/g.
Embodiment 2
The preparation for the magnetic oxygenated graphene that second diene triamine is modified, is as follows:
(1)0.4 g GO are gradually added into 150g deionized waters, is then ultrasonically treated 1 hour, obtains solution A;
(2)Under stiring, by FeCl2·4H2O (0.257g) and FeCl3·6H2O (0.699g) is dissolved in the deionization of 100mL
In water, mixed solution B is obtained;
(3)Then solution B is slowly added into solution A, NH is then added dropwise3·H2O by pH to be adjusted to 10, by mixed solution
It is maintained at 80 DEG C and continues stirring 4 hours, obtain mGO solution;
(4)By step(3)Second diene triamine is added in obtained mGO solution(8mL)In, be stirred continuously 8 hours in 60 DEG C, then according to
It is secondary to be washed with methanol and deionized water, it is dried in vacuo 24 hours at 50 DEG C, obtains the magnetic oxygenated stone of second diene triamine modification
Black alkene adsorbent(DLTA-mGO).
The magnetic oxygenated graphene adsorbent absorption input concentration of cadmium ions that the second diene triamine of preparation is modified is 50mg/
In the waste water of L, adsorbed 3 hours under the conditions of pH=5, adsorbance 94.3mg/g;After absorption, using magnet to adsorbent
It is separated and recovered, intensity of magnetization 22.6emu/g.
Embodiment 3
The preparation for the magnetic oxygenated graphene that second diene triamine is modified, is as follows:
(1)0.5 g GO are gradually added into 200g deionized waters, is then ultrasonically treated 1 hour, obtains solution A;
(2)Under stiring, by FeCl2·4H2O (0.257g) and FeCl3·6H2O (0.699g) is dissolved in the deionization of 100mL
In water, mixed solution B is obtained;
(3)Then solution B is slowly added into solution A, NH is then added dropwise3·H2O by pH to be adjusted to 11, by mixed solution
It is maintained at 90 DEG C and continues stirring 3 hours, obtain mGO solution;
(4)By step(3)Second diene triamine is added in obtained mGO solution(10mL)In, it is stirred continuously 6 hours in 70 DEG C, then
It is washed with methanol and deionized water, is dried in vacuo 24 hours at 50 DEG C successively, obtain the magnetic oxygenated of second diene triamine modification
Graphene adsorbent(DLTA-mGO).
The TEM figures of graphene oxide before unmodified are as shown in Figure 2 a, the magnetic of the second diene triamine modification of modified preparation
Property graphene oxide adsorbent TEM figures it is as shown in Figure 2 b, by Fig. 2 a and Fig. 2 b it is found that ferroso-ferric oxide particle deposition is to aoxidizing
It on graphene and is uniformly dispersed, it is in accordion that simultaneous oxidation graphene is modified through second diene triamine.
The magnetic oxygenated graphene adsorbent absorption input concentration of cadmium ions that the second diene triamine of preparation is modified is 50mg/
In the waste water of L, adsorbed 3 hours under the conditions of pH=5, adsorbance 108.6mg/g;After absorption, using magnet to adsorbent
It is separated and recovered, intensity of magnetization 19.4emu/g.
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, it is other it is any without departing from the spirit and principles of the present invention made by changes, modifications, substitutions, combinations, simplifications,
Equivalent substitute mode is should be, is included within the scope of the present invention.
Claims (10)
1. a kind of preparation method for the magnetic oxygenated graphene adsorbent that second diene triamine is modified, which is characterized in that including as follows
Step:
(1)It adds graphene oxide into deionized water, ultrasonic disperse is uniform, obtains solution A;
(2)By FeCl under stirring2·4H2O and FeCl3·6H2O is dissolved in deionized water, obtains solution B;
(3)Solution B is slowly added to be uniformly mixed in solution A under stirring, then NH is added dropwise3·H2After O adjusts pH value, in 70~90
It DEG C persistently stirs 3~5 hours, obtains modified graphene oxide solution;
(4)By step(3)Obtained modified graphene oxide solution is added in second diene triamine, then at 50~70 DEG C of lasting stirrings
After 6~12 hours, wash, it is dry, obtain the magnetic oxygenated graphene adsorbent that the second diene triamine is modified.
2. preparation method according to claim 1, which is characterized in that step(1)In, the graphene oxide and deionization
The mass ratio of water is 0.3~0.5:100~200.
3. preparation method according to claim 1, which is characterized in that step(2)In, the FeCl2·4H2O and
FeCl3·6H2The total amount of O and the mass ratio of deionized water are 1:20~105.
4. preparation method according to claim 1, which is characterized in that step(2)In, the FeCl2·4H2O and
FeCl3·6H2The molar ratio of O is 1:1~2.
5. preparation method according to claim 1, which is characterized in that step(3)In, the mixing of the solution A and solution B
Ratio presses graphene oxide and FeCl2·4H2O and FeCl3·6H2The mass ratio of the total amount of O is 0.1~0.52:1 is mixed.
6. preparation method according to claim 1, which is characterized in that step(3)In, the adjusting pH value is to adjust pH value
It is 9~11.
7. preparation method according to claim 1, which is characterized in that step(4)In, the modified graphene oxide solution
The amount being added in second diene triamine is 5~10 by the liquid ratio of second diene triamine and graphene oxide:0.3~0.5 ml/g is carried out
Addition.
8. preparation method according to claim 1, which is characterized in that step(4)In, it is described washing be successively use methanol and
Deionized water is washed;The drying is dried in vacuo 8~24 hours at 50~70 DEG C.
9. a kind of magnetic oxygenated stone that second diene triamine is modified made from claim 1~8 any one of them preparation method
Black alkene adsorbent.
10. the application for the magnetic oxygenated graphene adsorbent that a kind of second diene triamine described in claim 9 is modified, feature exist
In being applied in wastewater treatment to the Adsorption of heavy metal ion.
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
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CN111346610A (en) * | 2020-03-03 | 2020-06-30 | 邢台学院 | Graphite oxide/ferrite composite material and preparation method and application thereof |
CN113617339A (en) * | 2021-08-16 | 2021-11-09 | 成都理工大学 | GOC/PEI composite adsorbent and preparation method and application thereof |
CN114700050A (en) * | 2022-03-18 | 2022-07-05 | 华南理工大学 | Polyethyleneimine functionalized magnetic graphene oxide adsorbent and preparation method and application thereof |
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CN104043396A (en) * | 2014-07-10 | 2014-09-17 | 湖南大学 | Preparation method and application of magnetic aminated graphene oxide |
CN104709902A (en) * | 2015-02-12 | 2015-06-17 | 宁波市疾病预防控制中心 | Preparation method of magnetic graphene ternary composite material based on click chemistry |
CN106111064A (en) * | 2016-06-24 | 2016-11-16 | 湖南大学 | The preparation method of a kind of diethylene triamine pentacetic acid modified magnetic oxygenated graphene composite material and purposes |
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CN104043396A (en) * | 2014-07-10 | 2014-09-17 | 湖南大学 | Preparation method and application of magnetic aminated graphene oxide |
CN104709902A (en) * | 2015-02-12 | 2015-06-17 | 宁波市疾病预防控制中心 | Preparation method of magnetic graphene ternary composite material based on click chemistry |
CN106111064A (en) * | 2016-06-24 | 2016-11-16 | 湖南大学 | The preparation method of a kind of diethylene triamine pentacetic acid modified magnetic oxygenated graphene composite material and purposes |
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
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CN111346610A (en) * | 2020-03-03 | 2020-06-30 | 邢台学院 | Graphite oxide/ferrite composite material and preparation method and application thereof |
CN113617339A (en) * | 2021-08-16 | 2021-11-09 | 成都理工大学 | GOC/PEI composite adsorbent and preparation method and application thereof |
CN114700050A (en) * | 2022-03-18 | 2022-07-05 | 华南理工大学 | Polyethyleneimine functionalized magnetic graphene oxide adsorbent and preparation method and application thereof |
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