CN109663573A - A kind of imidazoles zeolite framework nanocomposite, preparation method and applications - Google Patents
A kind of imidazoles zeolite framework nanocomposite, preparation method and applications Download PDFInfo
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Abstract
The present invention relates to a kind of imidazoles zeolite framework nanocomposites, preparation method and applications, it includes hollow Nano carbon balls and the zeolite imidazole ester frame structure material being formed in the hollow Nano carbon balls, and the metal center of the zeolite imidazole ester frame structure material is Co2+And crosslinking ligand is alkyl imidazole.It is Co by filling metal center in hollow Nano carbon balls2+And crosslinking ligand is the zeolite imidazole ester frame structure material of alkyl imidazole, the advantages of not only there is excellent light-weight, mechanical performance, thermodynamic stability and corrosion resistant advantage, also show microporous properties, suitable for the large-scale application carbon dioxide capture.
Description
Technical field
The invention belongs to field of nanometer material technology, and in particular to a kind of imidazoles zeolite framework nanocomposite, preparation method
And its application.
Background technique
With the continuous development of human society, the greenhouse effects as caused by carbon dioxide excess emissions cause global climate
Greatly destroy.The rising of gas concentration lwevel improves the temperature on average in the whole world, leads to south poles Melting Glacierss, sea level
Constantly rising, serious harm coastal state and Part Wild animal inhabit.In addition, the increase of gas concentration lwevel will lead to ground
The temperature of ball surface is higher and higher, increases global extreme climate phenomenon odds.Therefore, carbon dioxide in atmosphere is reduced
Concentration have become a task too impatient to wait.
In order to inhibit the concentration of carbon dioxide in atmosphere, porous material absorption carbon dioxide is selected to be undoubtedly one of solution
Certainly scheme.Imidazoles zeolite framework material receives much attention due to extra specific surface area and pore volume；And imidazoles zeolite framework
Material itself is prepared simply, cheap, can adsorb several times of sole mass of carbon dioxide.In order to play high hole to the maximum extent
The advantage of gap rate imidazoles zeolite framework material, this material is constantly by nanosizing, Composite in the hope of being optimal performance.
Summary of the invention
A kind of imidazoles zeolite framework nanocomposite is provided the invention aims to overcome the deficiencies in the prior art.
In order to achieve the above objectives, the technical solution adopted by the present invention is that: a kind of imidazoles zeolite framework nanocomposite, it
Including hollow Nano carbon balls and the zeolite imidazole ester frame structure material being formed in the hollow Nano carbon balls, the zeolite
The metal center of imidazate frame structure material is Co2+And crosslinking ligand is alkyl imidazole.
Optimally, the hollow Nano carbon balls are meso-porous nano ball, and carbon thickness of the shell is 10~50nm.
Optimally, the size of the hollow Nano carbon balls is 100~500nm.
Optimally, the mass content of the zeolite imidazole ester frame structure material is 40~60%.
Another object of the present invention is to provide a kind of preparation method of above-mentioned imidazoles zeolite framework nanocomposite, it
The following steps are included:
(a) hollow Nano carbon balls are made using template；
(b) it penetrates into the alkyl imidazole of melting in the hollow Nano carbon balls, then alkyl imidazole is made to react shape with cobalt salt
At zeolite imidazole ester frame structure material.
Optimally, step (a) specifically: polystyrene nanospheres mother liquor, pyrrole monomer are distributed in deionized water, dripped
Ammonium persulfate solution is added to be reacted；It filters, is dry that polypyrrole coats polystyrene nanospheres；Polypyrrole cladding is poly-
Styrene nanosphere is carbonized in nitrogen atmosphere, collects to obtain hollow Nano carbon balls.
A further object of the present invention is to provide a kind of applications of above-mentioned imidazoles zeolite framework nanocomposite, it is used for
Adsorb carbon dioxide.
Due to the above technical solutions, the present invention has the following advantages over the prior art: imidazoles zeolite of the present invention
Frame nanocomposite is Co by filling metal center in hollow Nano carbon balls2+And crosslinking ligand is alkyl imidazole
Zeolite imidazole ester frame structure material not only has excellent light-weight, mechanical performance, thermodynamic stability and corrosion resistant excellent
Point, the advantages of also showing microporous properties, suitable for the large-scale application carbon dioxide capture.
Detailed description of the invention
Fig. 1 prepares schematic diagram for imidazoles zeolite framework nanocomposite of the present invention: (a) imidazoles zeolite framework nanometer is multiple
The preparation flow figure of condensation material, the transmission electron microscope picture of (b, c) polystyrene nanospheres, (d, e) polypyrrole cladding polystyrene are received
The transmission electron microscope picture of rice ball, (f, g) hollow Nano carbon balls, (h, i) load the transmission electricity of the hollow Nano carbon balls of 2-methylimidazole
Mirror figure, the transmission electron microscope picture of (j, k) imidazoles zeolite framework nanocomposite；
Fig. 2 is hollow Nano carbon balls structural characterization figure obtained in embodiment 1: (a) X-ray diffracting spectrum, (b) Raman
Spectrum, (c) x-ray photoelectron spectroscopy, (d) transmission electron microscope figure；
Fig. 3 is the transmission electron microscope figure of hollow Nano carbon balls in embodiment 1: before (a) loading 2-methylimidazole, (b)
After loading 2-methylimidazole；
Fig. 4 is the structural characterization of imidazoles zeolite framework nanocomposite prepared by embodiment 1: (a) x-ray diffraction pattern
Spectrum, (b) infrared spectroscopy, (c) with 5 DEG C of min-1Thermogravimetric curve of the heating rate in nitrogen atmosphere, (d) in the N of 77K measurement2
Adsorption desorption curve；
Fig. 5 is the structural characterization of imidazoles zeolite framework nanocomposite prepared by embodiment 1: (a, b) pore size distribution
Figure, (c, d) is with 5 DEG C of min-1Thermogravimetric curve of the heating rate in nitrogen atmosphere；
Fig. 6 is the adsorption experiment figure of the imidazoles zeolite framework nanocomposite prepared in embodiment 1- embodiment 3: (a,
B) CO of 273K measurement2Adsorption curve, (c) 273,293 and 333K measurement CO2Adsorption curve, (d) CO2And N2Absorption it is bent
Line, (e) CO under 273 and 293K2To N2Selective calculated curve, (f) CO under 273K2Sorption cycle curve；
Fig. 7 is the CO of the imidazoles zeolite framework nanocomposite prepared in embodiment 12Adsorption test curve: circulation 2
It is secondary；Circulation 5 times；Circulation 8 times；Circulation 10 times.
Specific embodiment
Imidazoles zeolite framework nanocomposite of the present invention, it includes hollow Nano carbon balls and is formed in the hollow carbon
Zeolite imidazole ester frame structure material in nanosphere, the metal center of the zeolite imidazole ester frame structure material are Co2+And
Crosslinking ligand is that (alkyl imidazole is those of routine to alkyl imidazole, such as 2-methylimidazole, 2- ethyl imidazol(e), 2- propyl imidazole, 2-
Butyl imidazole etc., general formula can indicate are as follows:The integer that n is 1~6 in formula).By being filled out in hollow Nano carbon balls
Filling metal center is Co2+And crosslinking ligand is the zeolite imidazole ester frame structure material of alkyl imidazole, not only has excellent weight
The advantages of amount is light, mechanical performance, thermodynamic stability and corrosion resistant advantage, also shows microporous properties, is suitable in dioxy
Change the large-scale application in carbon capture.The hollow Nano carbon balls are meso-porous nano ball, and carbon thickness of the shell is 10~50nm.It is described
The size of hollow Nano carbon balls is 100~500nm.The mass content of the zeolite imidazole ester frame structure material be 40~
60%.
The preparation method of above-mentioned imidazoles zeolite framework nanocomposite, it is the following steps are included: (a) uses template legal system
Obtain hollow Nano carbon balls；(b) it penetrates into the alkyl imidazole of melting in the hollow Nano carbon balls, then makes alkyl imidazole and cobalt salt
Reaction forms zeolite imidazole ester frame structure material.Step (a) specifically: by polystyrene nanospheres mother liquor, pyrrole monomer point
It is scattered in deionized water, ammonium persulfate solution is added dropwise and is reacted；It filters, is dry that polypyrrole coats polystyrene nanospheres；
Polypyrrole cladding polystyrene nanospheres are carbonized in nitrogen atmosphere, collect to obtain hollow Nano carbon balls.Above-mentioned imidazoles boiling
The application of stone frame nanocomposite, it is for adsorbing carbon dioxide.
Below in conjunction with embodiment, invention is further explained.
Embodiment 1
The present embodiment provides a kind of preparation methods of imidazoles zeolite framework nanocomposite, as shown in Figure 1, specifically such as
Under:
(a) synthetic polystyrene nanosphere: by Na2CO3(0.1g, 0.94mmol) and lauryl sodium sulfate (0.2g,
It 0.69mmol) is dissolved in 300mL deionized water, drum nitrogen 30 minutes；30mL styrene is added and (successively uses 5wt% using preceding
NaOH solution, deionized water washing to remove polymerization inhibitor), 60 DEG C heating stirring 30 minutes；Potassium persulfate solution is added dropwise
(15ml, 0.23mol/L) and 75 DEG C are warming up to, reaction 20h is cooled to room temperature；With the revolving speed centrifugation of 12000rpm, use deionization
Water washing is distributed in 100mL deionized water afterwards in triplicate and obtains polystyrene nanospheres mother liquor；
Synthesis polypyrrole coats polystyrene nanospheres: taking polystyrene nanospheres mother liquor 2mL (about 0.1g mL-1)、
0.6mL pyrrole monomer is distributed in 100mL deionized water and stirs 10 minutes, is added dropwise ammonium persulfate solution (100mL, 1.7mmol)
React 6h, filtration washing, in 60 DEG C of vacuum drying 12h；
It prepares hollow Nano carbon balls: polypyrrole cladding polystyrene nanospheres (0.2g) being placed in silica crucible, with 5
℃min-1Heating rate 800 DEG C are heated in nitrogen atmosphere, collected after cooled to room temperature to obtain hollow Nano carbon balls (letter
Claim HCSs)；It characterizes such as Fig. 2.
(b) it synthesizes the ZIF-67 composite material of hollow Nano carbon balls cladding: taking hollow Nano carbon balls 20mg and 2- methyl miaow
Azoles 300mg is fully ground mixing and is placed in silica crucible；In nitrogen atmosphere, with 5 DEG C of min-1Rate from room temperature to
145 DEG C, keep the temperature 20h；Then it is dispersed back into methanol, is added dissolved with cobalt nitrate after mixing material being washed one time with methanol
The 4mL methanol of (0.05g) is stirred to react for 24 hours to form zeolite imidazole ester frame structure material；So that filtration drying product obtains
(abbreviation ZIF-67@HCSs-40,40 finger zeolite imidazole ester frame structure materials are averaged imidazoles zeolite framework nanocomposite
Size, nm), test performance (is compared) as shown in Fig. 3-Fig. 5 with commercially available ZIF-67, HCSs.
Embodiment 2
The present embodiment provides a kind of preparation method of imidazoles zeolite framework nanocomposite, it and answering in embodiment 1
Condensation material is almost the same, unlike: in step (b), take hollow Nano carbon balls 20mg and 2-methylimidazole 250mg, finally plus
The cobalt nitrate entered is 0.05g, final to obtain ZIF-67@HCSs-50.
Embodiment 3
The present embodiment provides a kind of preparation method of imidazoles zeolite framework nanocomposite, it and answering in embodiment 1
Condensation material is almost the same, unlike: in step (b), take hollow Nano carbon balls 20mg and 2-methylimidazole 180mg, finally plus
The cobalt nitrate entered is 0.05g, final to obtain ZIF-67@HCSs-60.
Embodiment 4
The present embodiment provides a kind of preparation method of imidazoles zeolite framework nanocomposite, it and answering in embodiment 1
Condensation material is almost the same, unlike: in step (b), use 2- ethyl imidazol(e).
Embodiment 5
The present embodiment provides a kind of preparation method of imidazoles zeolite framework nanocomposite, it and answering in embodiment 1
Condensation material is almost the same, unlike, in step (b), use 2- propyl imidazole.
Embodiment 6
The present embodiment provides a kind of preparation method of imidazoles zeolite framework nanocomposite, it and answering in embodiment 1
Condensation material is almost the same, unlike, in step (b), use 2- butyl imidazole.
Embodiment 7
The present embodiment provides a kind of preparation method of imidazoles zeolite framework nanocomposite, it and answering in embodiment 1
Condensation material is almost the same, unlike, in step (b), use 2- hexyl imidazolium.
Comparative example 1
The present embodiment provides a kind of preparation methods of composite material, it is substantially consistent with the composite material in embodiment 1, no
It is same, in step (b), 1- methylimidazole is used, does not obtain imidazoles zeolite framework nanocomposite finally.
By the imidazoles zeolite framework nanocomposite applications obtained in embodiment 1-7 in the absorption of carbon dioxide and nitrogen
Test, specifically: it weighs imidazoles zeolite framework composite material (40mg) and is placed in gas absorption instrument test specimens quality control, at 120 DEG C
Degasification activation 3h then measures N at 273K, 293K and 333K2And CO2Adsorption curve, finally carry out data processing and point
Analysis；Other contrast samples such as ZIF-67, HCSs carry out absorption test for comparing under similarity condition；The result is shown in Fig. 6 and figure
7.ZIF-67@HCSs-40 illustrates maximum CO2Absorption property and biggish CO2To N2Selectivity.As a result it is also shown that
ZIF-67@HCSs composite material has higher CO than single ZIF-67 and HCSs2Adsorbance and selectivity, and adsorbance and
Selectivity increases with the reduction of ZIF-67 average-size, i.e. ZIF-67@HCSs-40 has best CO2Absorption property.
The above embodiments merely illustrate the technical concept and features of the present invention, and its object is to allow person skilled in the art
Scholar cans understand the content of the present invention and implement it accordingly, and it is not intended to limit the scope of the present invention.It is all according to the present invention
Equivalent change or modification made by Spirit Essence, should be covered by the protection scope of the present invention.
Claims (7)
1. a kind of imidazoles zeolite framework nanocomposite, it is characterised in that: it includes hollow Nano carbon balls and is formed in institute
State the zeolite imidazole ester frame structure material in hollow Nano carbon balls, the metal center of the zeolite imidazole ester frame structure material
For Co2+And crosslinking ligand is alkyl imidazole.
2. imidazoles zeolite framework nanocomposite according to claim 1, it is characterised in that: the hollow Nano carbon balls
For meso-porous nano ball, carbon thickness of the shell is 10 ~ 50nm.
3. imidazoles zeolite framework nanocomposite according to claim 1, it is characterised in that: the hollow Nano carbon balls
Size be 100 ~ 500nm.
4. imidazoles zeolite framework nanocomposite according to claim 1, it is characterised in that: the zeolite imidazole ester bone
The mass content of frame structural material is 40 ~ 60 %.
5. the preparation method of any imidazoles zeolite framework nanocomposite in Claims 1-4, which is characterized in that it
The following steps are included:
(a) hollow Nano carbon balls are made using template；
(b) it penetrates into the alkyl imidazole of melting in the hollow Nano carbon balls, alkyl imidazole is then made to react to form boiling with cobalt salt
Stone imidazate frame structure material.
6. the preparation method of imidazoles zeolite framework nanocomposite according to claim 5, which is characterized in that step (a)
Specifically: polystyrene nanospheres mother liquor, pyrrole monomer are distributed in deionized water, ammonium persulfate solution is added dropwise and carries out instead
It answers；It filters, is dry that polypyrrole coats polystyrene nanospheres；By polypyrrole cladding polystyrene nanospheres in nitrogen gas
It is carbonized in atmosphere, collects to obtain hollow Nano carbon balls.
7. the application of any imidazoles zeolite framework nanocomposite in Claims 1-4, it is characterised in that: it is used for
Adsorb carbon dioxide.
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| CN113042105A (en) * | 2021-04-12 | 2021-06-29 | 西北师范大学 | Preparation method of hydroxyapatite nanowire combined cobalt MOFs beaded catalyst |
| CN113801538A (en) * | 2021-09-16 | 2021-12-17 | 中山大学 | Metal organic framework/epoxy coating and preparation method and application thereof |
| CN114957681A (en) * | 2022-04-18 | 2022-08-30 | 苏州大学 | Neutron shielding material based on metal boron-imidazole framework and preparation method thereof |
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