CN105170095B - A kind of In bases organic backbone graphene oxide composite material and its preparation method and application - Google Patents
A kind of In bases organic backbone graphene oxide composite material and its preparation method and application Download PDFInfo
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Abstract
The invention belongs to metal-organic framework materials technical field, a kind of In bases organic backbone graphene oxide composite material and its preparation method and application is disclosed, preparation method is：Graphene oxide powder is scattered in N, N ' dimethylformamides and carries out ultrasonically treated, dispersion liquid is obtained；Soluble indium salts and 2 amino terephthalic acid (TPA)s are added in above-mentioned dispersion liquid, uniform stirring is simultaneously ultrasonically treated, obtains reaction solution, are reacted under the conditions of temperature programming, obtain rough composite；Rough composite is successively used into N, N ' dimethylformamides and methanol solvate rinse immersion, and activation finally obtains purpose composite.Material prepared by the present invention is bigger than surface, with flourishing micropore structure, there is high adsorption capacity to the rhdamine B molecule of low concentration in water, under equal conditions, it is 2.24 times, 20.1 times of the molecular sieves of ZSM 5 of activated carbon to the adsorbance of rhodamine B.
Description
Technical field
The present invention relates to dye molecule rhodamine B sorbing material in water, more particularly to a kind of In bases organic backbone-oxidation stone
Black alkene composite and preparation method thereof.
Background technology
Dyestuff is widely used in the various industry such as printing and dyeing, papermaking, paint, timber preservative.In some developing countries, by
The wastewater flow rate of textile industry discharge has more than ten hundred million tons every year according to estimates.The waste water from dyestuff of high chroma has a strong impact on water quality, and can be to life
Object produces toxic action even " three cause " effect.In view of the toxicity of dye molecule and its spy such as complicated, biodegradability is poor
Point, for the effective and safe Adsorption of dyes molecule, has important section for solving water body environment safety problem
Learn meaning and realistic meaning.
For the treatment technology of water body middle and high concentration waste water from dyestuff, existing method include coagulation, biodegradation, precipitation and
Chemical oxidization method.But, after even being handled using the above method, water body fails to decolourize completely, is still remained in water low dense
The soluble ion dyestuff of degree.The characteristics of adsorption technology is because of its feasibility height and good cost benefit, is widely used in processing big
The industrial wastewater of scale.Traditional material such as activated carbon, natural minerals and industrial residue etc., height is shown to the waste water of high concentration
Adsorption capacity, but adsorption efficiency is not then good when the processing applied to low concentration waste water from dyestuff.Therefore, research and develop to water
The novel absorption material that middle low concentration dye molecule has high Adsorption efficiency is very important.
In recent years, metal-organic framework compound (metal organic frameworks, MOFs) is because of its specific surface area
The advantages of huge, physicochemical property is adjustable, easy functionalization and synthesis strategy are diversified shows very well in fields such as adsorbing separations
Potential application foreground.Wherein, MIL-68 (In)-NH2Be a kind of good hydrothermal stability and with high-ratio surface MOFs materials,
And the free amino group group of its band is towards pore passage structure center, and because the confinement in duct is acted on, large-sized substrate is not
Duct can be entered, small size substrate, which can then enter, to react in duct and be adsorbed with amino active sites.So, MIL-68
(In)-NH2Metal-organic framework materials possess good adsorption selectivity.
The content of the invention
In order to overcome the shortcomings and deficiencies of the prior art described above, primary and foremost purpose of the invention is to provide a kind of In bases organic
The preparation method of skeleton-graphene oxide composite material.By modified with functional group, be combined with the means such as fabricated in situ, it is real
Now to the high adsorption capacity of low concentration dye molecule rhodamine B in water.
The purpose of the present invention is achieved through the following technical solutions：
A kind of preparation method of In bases organic backbone-graphene oxide composite material, comprises the following steps：
(1) by graphene oxide powder be scattered in N, N '-dimethylformamide and carry out it is ultrasonically treated, obtain aoxidize stone
The dispersion liquid of black alkene；
(2) soluble indium salts and 2- amino terephthalic acid (TPA)s are added in the graphene oxide dispersion of step (1),
Even stirring is simultaneously ultrasonically treated, obtains reaction solution, is reacted under the conditions of temperature programming, obtain rough In bases organic backbone-oxidation stone
Black alkene composite；
(3) the rough In bases organic backbone for obtaining step (2)-graphene oxide composite material successively uses N, N '-two
NMF and methanol solvate rinse immersion, and activation finally obtains In bases organic backbone-graphene oxide composite wood of purifying
Material.
The amount of graphene oxide used is the 2~7% of soluble indium salts and 2- amino terephthalic acid (TPA) gross masses.
Soluble indium salts are indium nitrate described in step (2).
Solubility indium salts used in step (2) and the mol ratio of 2- amino terephthalic acid (TPA)s are (2~4)：1.
Concentration of the soluble indium salts in N, N '-dimethylformamide is 0.093~0.120g/mL.
Temperature programming is described in step (2)：The temperature of reaction solution is risen to by 150- with 5~10 DEG C/h programming rate
170 DEG C, after 5~6h of constant temperature, naturally cool to room temperature.
Step (3) activation is that 8~12h is kept under 100~150 DEG C of vacuum conditions.
In bases organic backbone-graphene oxide composite material prepared by above method dye molecule rhodamine in absorption water
Application in B.
Graphene is by carbon atom with alveolate texture (similar benzene ring structure) the tightly packed two-dimensional material constituted, and it has
There are the specific surface area and hydrophobic property of superelevation, it is designed with MOFs Material claddings, while also using the fine and close carbon of graphene
Atomic surface can be between reinforcing material and guest molecule dispersion force the characteristics of the absorption property of MOFs composites is obtained significantly
Improve, and its mechanical property is also improved.
Compared with prior art, the present invention has advantages below and beneficial effect：
(1) present invention is by adding graphene oxide, the abundant oxygen-containing functional group having using graphene oxide with
Unsatuated metal site In in MOFs units3+It is bonded, accelerates the crystal growth and pore structure of metal-organic framework materials
Formation；Simultaneously as the introducing of graphene oxide so that material have higher atomic density, and can MOFs units with
Dispersion force is produced on the interface of graphene oxide, so as to assign material excellent absorption property.
(2) compared with existing sorbing material, In bases organic backbone-graphene oxide composite material pair that the present invention is obtained
The rhdamine B molecule of low concentration has higher adsorption capacity in water.Under equal conditions, the organic bone of In bases of the invention
Frame-graphene oxide composite material is to 2.24 times that the adsorbance of the rhdamine B molecule of low concentration is activated carbon, ZSM-5
20.1 times of molecular sieve.
(3) In bases organic backbone-graphene oxide composite material that the present invention is obtained remains original In bases organic material
Skeleton structure, and be successfully introduced into graphene oxide.Meanwhile, In bases organic backbone-graphene oxide that the present invention is obtained is multiple
Condensation material has middle micro-diplopore structure.
Brief description of the drawings
Fig. 1 is MIL-68 (In)-NH prepared by embodiment 2,3,42The MIL-68 that@GO composites are prepared with embodiment 1
(In)-NH2Material powder X-ray RD spectrograms contrast, and graphene oxide XRD spectra.
Fig. 2 is MIL-68 (In)-NH prepared by embodiment 22MIL-68 prepared by@GO-1 composites and embodiment 1
(In)-NH2The N of material2Adsorption isotherm is contrasted.
Fig. 3 is MIL-68 (In)-NH prepared by embodiment 12MIL-68 (In)-NH prepared by material (a) and embodiment 22@
The SEM comparison diagrams of GO-1 composites (b).
Fig. 4 is MIL-68 (In)-NH prepared by embodiment 2,3,42The MIL-68 that@GO composites are prepared with embodiment 1
(In)-NH2Material, activated carbon and ZSM-5 molecular sieve are contrasted to the adsorption effect of low concentration rhodamine B.
Embodiment
With reference to embodiment and accompanying drawing, the invention will be further described, but the implementation not limited to this of the present invention, change
Implement to be included in the technical scope of the present invention.
Embodiment 1：Comparative example
1.49g indium nitrates and 0.230g2- amino terephthalic acid (TPA)s are dissolved in 12.4mLN, N '-dimethylformamide,
Even stirring is simultaneously ultrasonically treated, and obtained reaction solution rises to 150 DEG C with 10 DEG C/h speed from room temperature, and constant temperature 5h is naturally cooled to
Room temperature.Filtered product first uses N, N '-dimethylformamide to rinse 3 times, then soaks in methyl alcohol after 3 days, exists through tube furnace
N2The lower 200 DEG C of roastings 5h of atmosphere, in activating 12h under 150 DEG C of vacuum conditions, it is MIL-68 (In)-NH to mark this sample2。
Embodiment 2：The preparation of In bases organic backbone-graphene oxide composite material
By 0.0965g graphene oxide powders be scattered in 11.0mLN, N '-dimethylformamide and carry out it is ultrasonically treated,
Obtain the dispersion liquid of graphene oxide；1.148g indium nitrates and 0.230g2- amino terephthalic acid (TPA)s are added to above-mentioned oxidation stone
In black alkene dispersion liquid, stir and ultrasonically treated, obtained reaction solution rises to 160 DEG C, constant temperature with 5 DEG C/h speed from room temperature
6h, naturally cools to room temperature.Filtered product first uses N, and N '-dimethylformamide is rinsed 3 times, then is soaked 3 days in methyl alcohol
Afterwards, through tube furnace in N2The lower 180 DEG C of roastings 5h of atmosphere, in activating 12h under 130 DEG C of vacuum conditions, it is MIL-68 to mark this sample
(In)-NH2@GO-1。
Embodiment 3：The preparation of In bases organic backbone-graphene oxide composite material
By 0.0722g graphene oxide powders be scattered in 10.1mLN, N '-dimethylformamide and carry out it is ultrasonically treated,
Obtain the dispersion liquid of graphene oxide；1.207g indium nitrates and 0.237g2- amino terephthalic acid (TPA)s are added to above-mentioned oxidation stone
In black alkene dispersion liquid, uniform stirring is simultaneously ultrasonically treated, and obtained reaction solution rises to 170 DEG C, constant temperature with 8 DEG C/h speed from room temperature
5h, naturally cools to room temperature.Filtered product first uses N, and N '-dimethylformamide is rinsed 3 times, then is soaked 3 days in methyl alcohol
Afterwards, through tube furnace in N2The lower 150 DEG C of roastings 5h of atmosphere, in activating 12h under 100 DEG C of vacuum conditions, it is MIL-68 to mark this sample
(In)-NH2@GO-2。
Embodiment 4：The preparation of In bases organic backbone-graphene oxide composite material
By 0.0340g graphene oxide powders be scattered in 12.4mLN, N '-dimethylformamide and carry out it is ultrasonically treated,
Obtain the dispersion liquid of graphene oxide；1.49g indium nitrates and 0.230g2- amino terephthalic acid (TPA)s are added to above-mentioned oxidation stone
In black alkene dispersion liquid, uniform stirring is simultaneously ultrasonically treated, and obtained reaction solution rises to 150 DEG C, perseverance with 10 DEG C/h speed from room temperature
Warm 6h, naturally cools to room temperature.Filtered product first uses N, N '-dimethylformamide to rinse 3 times, then soaks in methyl alcohol 3
After it, through tube furnace in N2The lower 200 DEG C of roastings 5h of atmosphere, in activating 12h under 150 DEG C of vacuum conditions, it is MIL- to mark this sample
68(In)-NH2@GO-3。
Material obtained by embodiments of the invention 1 and embodiment 2, its characterization result and absorption rhodamine B performance are as follows：
(1) XRD phenetic analysis
The sharp shadow X-ray diffractometers of Empyrean produced using Dutch PANalytical company are prepared to the embodiment of the present invention 1 and 2
The crystal structure of obtained porous material is characterized, and graphene oxide (GO) is as blank, as shown in figure 1, wherein grasping
It is as condition：Copper target, 40KV, 40mA, 0.0131 degree of step-length, 9.664 seconds/step of sweep speed.
It will be seen from figure 1 that MIL-68 (In)-NH prepared by embodiment 2,3,42@GO composites show and implemented
MIL-68 (In)-NH prepared by example 12The consistent characteristic peak of material, peak intensity and sharp shows that it has good MIL-68
(In)-NH2Crystal framework structure.
(2) pore structure is characterized
Test prepared by embodiment 1 and embodiment 2 using ASAP2020 specific surface areas and distribution of pores structural test machines
The material that in the pore structure of material, Fig. 2 prepared by two embodiments is respectively labeled as MIL-68 (In)-NH2With MIL-68 (In)-
NH2@GO-1.Test result is as shown in table 1.
Table 1
The pore volume and aperture parameters of the porous material of table 2
As seen from Figure 2, MIL-68 (In)-NH that prepared by embodiment 22The N of@GO-1 composites2Adsorption isotherm belongs to
In Ι class thermoisopleths, show that it has microcellular structure.As shown in Table 1, MIL-68 (In)-NH that prepared by embodiment 22@GO-1 are combined
The ratio surface of material is 493.1m2/ g, MIL-68 (the In)-NH prepared less than embodiment 12Material 579.6m2/ g, this shows oxygen
The addition of graphite alkene has a certain impact to the specific surface area of composite.Table 2 shows, In bases organic backbone-graphite oxide
Alkene composite has middle micro-diplopore structure, and micro-porous adsorption gesture and its absorption pore volume have important to the adsorption of composite
Influence, meso-hole structure is then conducive to quick diffusion of the adsorption molecule in hole.
(3) SEM phenetic analysis
The surface topography of sample is entered using MERLIN field emission scanning electron microscopes (Carl Zeiss companies, Germany)
Row is characterized.As a result as shown in figure 3, bar-shaped crystal structure, and MIL-68 (In)-NH prepared by embodiment 2 is presented in sample2@
The crystalline size of GO composites is significantly greater than MIL-68 (In)-NH of the preparation of embodiment 12The crystalline size of material, shows oxygen
The addition of graphite alkene has a certain impact to the crystal growing process of composite.
(4) rhodamine B absorption property is determined
The model DR5000 ultraviolet specrophotometers produced using HACH companies of the U.S. determine absorption property.Fig. 4 is
Under 298K, MIL-68 (In)-NH prepared by embodiment 12MIL-68 (In)-NH prepared by material and embodiment 2,3,42@GO are combined
Material, and activated carbon, the absorption property curve map of ZSM-5 molecular sieve adsorption of Low Concentration rhodamine B, exist sample before test
Vacuum activating 12h under the conditions of 150 DEG C.
As shown in Figure 4, MIL-68 (In)-NH2@GO composites, in 55mg/g or so, are higher than to the adsorbance of rhodamine B
MIL-68(In)-NH240.7mg/g of the material under equal experiment condition.This shows, due to the introducing of graphene oxide, fully
Using functional group thereon, contribute to the raising of absorption property；Meanwhile, on the individual layer interface of MOF units and graphene oxide
The dispersion force of generation, is also increased on the unsatuated metal adsorption site and organic ligand in rhodamine B molecule and MOF skeletons
Interaction force between functional group, so as to improve In bases organic backbone-graphene oxide composite material to low concentration Luo Dan
The absorption property of bright B molecules.
Table 3 is desorption balance data of the rhodamine B on different sorbing materials.As can be seen from the table, testing on an equal basis
Under the conditions of, MIL-68 (In)-NH2@GO composites are about MIL-68 (In)-NH to the equilibrium adsorption capacity of low concentration rhodamine B2
1.37 times, 2.24 times of activated carbon, 20.1 times of ZSM-5 molecular sieve.
Table 3
Claims (7)
1. a kind of preparation method of In bases organic backbone-graphene oxide composite material, it is characterised in that comprise the following steps：
(1) graphene oxide powder is scattered in N, N '-dimethylformamide and carries out ultrasonically treated, obtain graphene oxide
Dispersion liquid；
(2) soluble indium salts and 2- amino terephthalic acid (TPA)s are added in the graphene oxide dispersion of step (1), uniformly stirred
Mix and ultrasonically treated, obtain reaction solution, reacted under the conditions of temperature programming, obtain rough In bases organic backbone-graphene oxide
Composite；Wherein, the temperature of reaction solution is risen to after 150-170 DEG C, 5~6h of constant temperature with 5~10 DEG C/h programming rate, from
So it is cooled to room temperature；
(3) the rough In bases organic backbone for obtaining step (2)-graphene oxide composite material successively uses N, N '-dimethyl
Formamide and methanol solvate rinse immersion, and activation finally obtains In bases organic backbone-graphene oxide composite material of purifying；
Wherein, activate to keep 8~12h under 100~150 DEG C of vacuum conditions.
2. preparation method according to claim 1, it is characterised in that the amount of graphene oxide used be soluble indium salts and
The 2~7% of 2- amino terephthalic acid (TPA) gross masses.
3. preparation method according to claim 1, it is characterised in that soluble indium salts are indium nitrate described in step (2).
4. preparation method according to claim 1, it is characterised in that solubility indium salts used and 2- amino in step (2)
The mol ratio of terephthalic acid (TPA) is (2~4)：1.
5. preparation method according to claim 1, it is characterised in that the soluble indium salts are in N, N '-dimethyl formyl
Concentration in amine is 0.093~0.120g/mL.
6. In bases organic backbone-graphene oxide composite material prepared by any one of Claims 1 to 5 method.
7. the dye molecule rhodamine B in absorption water of In bases organic backbone-graphene oxide composite material described in claim 6
In application.
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| CN112457499B (en) * | 2020-11-30 | 2022-03-25 | 华南理工大学 | Rare earth-based metal organic framework fluorescent nano material and preparation method and application thereof |
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Address after: 510640 Tianhe District, Guangdong, No. five road, No. 381, Co-patentee after: Guangzhou Chao Hui Biological Technology Co., Ltd. Patentee after: South China University of Technology Address before: 510640 Tianhe District, Guangdong, No. five road, No. 381, Co-patentee before: Guangzhou Chaohui Chemical Technology Co., Ltd. Patentee before: South China University of Technology |