CN109894085A - Monodisperse bakelite resin nano stick is embedded in the simple universality preparation method of MOF composite material in situ - Google Patents
Monodisperse bakelite resin nano stick is embedded in the simple universality preparation method of MOF composite material in situ Download PDFInfo
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- CN109894085A CN109894085A CN201910221887.XA CN201910221887A CN109894085A CN 109894085 A CN109894085 A CN 109894085A CN 201910221887 A CN201910221887 A CN 201910221887A CN 109894085 A CN109894085 A CN 109894085A
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Abstract
The present invention relates to the simple universality preparation methods that a kind of monodisperse bakelite resin nano stick is embedded in MOF composite material in situ, it include following steps: monodisperse bakelite resin nano stick is evenly dispersed in the solution, metal salt is added to be stirred, ultrasound, it is eventually adding the solution that a certain concentration contains organic ligand, reaction obtains monodisperse bakelite resin nano stick insertion MOF composite material in situ after centrifugation, washing, drying.Compared with prior art, the present invention have the advantage that synthesis technology is simple, it is low in cost；N doping in situ can effectively improve the electric conductivity and chemical property of material；The partial size of MOF is adjustable, can consolidate insertion or intert into monodisperse resin nanorod structure, overall structure is stablized；Monodimension nano stick to be utilized effectively inside big partial size MOF, shortens the transmission path of electronics and reduces the diffusional resistance of electronics.
Description
Technical field
The invention belongs to technical field of material chemistry, and in particular to a kind of monodisperse bakelite resin nano stick original position insertion MOF is multiple
The simple universality preparation method of condensation material.
Background technique
MOF material is since it has many advantages, such as that high thermal stability and chemical stability and hole are abundant, extensively at present
Applied to fields such as gas absorption separation, ion exchanges.When being used as electrode material, the biggish gap of MOF nanocrystal and envelope
Structure is closed for storing electronics and ion and buffer volumes expansion；Porous or hollow carbon frame has high local conductivity and whole
Body electric conductivity helps speed up ion or electron-transport speed, improves its chemical property.
For the partial size of MOF material mostly in 1 microns, biggish partial size makes its internal electron transmission path and resistance at present
Power becomes larger, and is difficult to realize the raising of its chemical property and further applies.Big partial size MOF material is got through in the form in " tunnel "
Its inner utilization space will be greatly increased.It is obtained from current literature survey, only researcher interts carbon nanotube into MOF material
In material, but intert inefficient.In addition, if carbon nanotube wants adsorbing metal to need to carry out its surface nitric acid or sulfuric acid
Pretreatment is to increase organo-functional group, and this considerably increases its practical application costs.Chen et al. (J.Am.Chem.Soc.,
2017,139,12710) devise the structure that a kind of carbon nanotube interts ZIF-67, considerably increase its inner utilization efficiency and
Electron-transport speed.But there is still a need for sulfuric acid and nitric acid to be handled for its carbon nanotube, higher cost, it is difficult to business metaplasia
It produces.Therefore it synthesizes a kind of simple one-dimentional structure and interts big partial size MOF composite material in situ and play a significant role for practical application.
Summary of the invention
The purpose of the present invention is to provide a kind of simple process, mild condition, the monodisperse phenol that cheap, universality is strong
Urea formaldehyde nanometer rods are embedded in the simple universality preparation method of MOF composite material in situ.
The present invention solves scheme used by above-mentioned technical problem: monodisperse bakelite resin nano stick is embedded in MOF in situ
The simple universality preparation method of composite material, includes following steps: monodisperse bakelite resin nano stick is dispersed in
In solution, metal salt being added and is stirred, ultrasound is eventually adding the solution that a certain concentration contains organic ligand, it reacts, centrifugation,
Monodisperse bakelite resin nano stick insertion MOF composite material in situ is obtained after washing, drying.
According to the above scheme, selected metal salt is zinc nitrate hexahydrate, cabaltous nitrate hexahydrate, ferric trichloride or four hydrations
Nickel acetate.
According to the above scheme, the zinc nitrate hexahydrate concentration is 15~30mg/mL；Cabaltous nitrate hexahydrate concentration be 10~
200mg/mL；Ferric trichloride concentration is 20-40mg/mL；Nickel acetate tetrahydrate concentration is 5-20mg/mL.
According to the above scheme, the organic ligand is methylimidazole, terephthalic acid (TPA) or polyvinylpyrrolidone.
According to the above scheme, the methylimidazole solution concentration is 10~40mg/mL；Terephthalic acid solution's concentration is
10-20mg/mL；Polyvinylpyrrolidonesolution solution concentration is 10~50mg/mL.
According to the above scheme, the reaction temperature is 20~40 DEG C, and mixing time is 6~18h.
Reaction mechanism of the present invention: monodisperse bakelite resin nano stick surface has oxygen-containing functional group abundant, can be effective
Ground adsorbing metal ions.When immersing in metallic solution, metal ion is adsorbed to the surface of resin nano stick and interior in large quantities
Portion；Start to form ligand with metal and in resin nano stick surface nucleation after organic ligand is added；The concentration of organic ligand for
Nucleation number it is most important.When concentration is lower, nucleation is less, is gradually grown to big partial size with the extension of reaction time
MOF；When concentration is higher, nucleation increases, and obtains small particle MOF first, more due to being nucleated, and the quantity of metal ion has
Limit, it is nanocrystalline to finally obtain the lesser MOF of partial size.Since MOF is growth in situ on resin nano stick, nanometer rods are finally obtained
The interspersed rock-steady structure into MOF.
Compared with prior art, the present invention having the advantage that
1) synthesis technology is simple, low in cost；
2) N doping in original position can effectively improve the electric conductivity and chemical property of material；
3) partial size of MOF is adjustable, can consolidate insertion or intert into monodisperse resin nanorod structure, overall structure is stablized；
4) monodimension nano stick to be utilized effectively inside big partial size MOF, shortens the transmission path and reduction of electronics
The diffusional resistance of electronics；
5) the synthetic method universality is strong, and the interspersed insertion in situ of bakelite resin nano stick can be made according to the synthetic route
Big partial size ZIF-8, ZIF-67, Zn/Co-ZIF, Fe-Mil-88 and Ni base MOFs material.
Detailed description of the invention
Fig. 1 is the XRD that 1 gained monodisperse bakelite resin nano stick of embodiment is embedded in big partial size ZIF-8 composite material in situ
Map, microstructure schematic diagram and SEM figure；
Fig. 2 is the SEM that 2 gained small particle ZIF-8 of embodiment is embedded in monodisperse bakelite resin nano rod composite material in situ
Figure；
Fig. 3 is the XRD that 3 gained monodisperse bakelite resin nano stick of embodiment is embedded in big partial size ZIF-67 composite material in situ
Map, microstructure schematic diagram and SEM figure；
Fig. 4 is that 4 gained monodisperse bakelite resin nano stick of embodiment is embedded in big partial size Zn/Co-ZIF composite material in situ
XRD spectrum, microstructure schematic diagram and SEM figure；
Fig. 5 is that 5 gained monodisperse bakelite resin nano stick of embodiment is embedded in big partial size Fe-MIL-88 composite material in situ
XRD spectrum, microstructure schematic diagram and SEM figure；
Fig. 6 is the XRD that 6 gained monodisperse bakelite resin nano stick of embodiment is embedded in big partial size Ni-MOF composite material in situ
Map, microstructure schematic diagram and SEM figure.
Specific embodiment
Technical solution of the present invention is further illustrated below with reference to embodiment, but not as the limit to the scope of the present invention
System.
Embodiment 1
200mg monodisperse bakelite resin nano stick and 508mg zinc nitrate hexahydrate are dispersed in the methanol solution of 25mL,
Then pass through ultrasonic disperse uniform adsorption metal zinc ion, add the 25mL methanol solution dissolved with 330mg methylimidazole, 25
12h is stirred to react at DEG C, centrifuge washing, drying, obtaining monodisperse bakelite resin nano stick, the big partial size ZIF-8 of insertion is compound in situ
Material (RNR/L-ZIF-8).
By taking the resulting monodisperse bakelite resin nano stick of the present embodiment is embedded in big partial size ZIF-8 composite material in situ as an example.
Monodisperse bakelite resin nano stick surface has oxygen-containing functional group abundant, being capable of effective adsorbing metal ions.When immersion metal
When in solution, metal ion is adsorbed to the surface and inside of resin nano stick in large quantities；Be added methylimidazole after start with
Metal ion forms ligand and in resin nano stick surface nucleation；This embodiment methylimidazole concentration is lower, and nucleation is less, with
The extension in reaction time be gradually grown to big partial size ZIF-8.It can be obtained by X-ray diffractogram spectrum analysis shown in attached drawing 1a,
RNR/L-ZIF-8 crystallinity is very high；Bakelite resin nano stick shown in attached drawing 1b~d interts the micro- of ZIF-8 composite material in situ
Structural schematic diagram and SEM figure are seen, shows that monodisperse bakelite resin nano stick successfully interts and enters in ZIF-8 crystal, ZIF-8
Crystal is positive dodecahedron structure, and average grain diameter is in 700nm or so, this demonstrate that synthesis mechanism has reasonability.
The inner utilization space that bulky grain ZIF-8 will be effectively increased after material carbonization, improves its electron-transport efficiency, increases
Add electric conductivity.Its excellent one-dimentional structure will be connected between ZIF-8 simultaneously, and electron-transport efficiency is further promoted.In addition
In conjunction with the higher specific surface area of the material, it will in gas absorption, separation and energy storage (lithium electricity, sodium electricity etc.), conversion field
Practical application value with higher.
Embodiment 2
200mg monodisperse bakelite resin nano stick and 508mg zinc nitrate hexahydrate are dispersed in the methanol solution of 25mL,
Then pass through ultrasonic disperse uniform adsorption metal zinc ion, add the 25mL methanol solution dissolved with 990mg methylimidazole, 25
At DEG C, it is stirred to react 12h, centrifuge washing, drying, obtaining small particle ZIF-8, insertion monodisperse bakelite resin nano stick is multiple in situ
Condensation material (S-ZIF-8/RNR).
As shown in attached drawing 2SEM image, small particle ZIF-8 is successfully embedded in monodisperse bakelite resin nano stick structure in situ
In, the average grain diameter of ZIF-8 is in 110nm or so.The reunion that the presence of monodimension nano stick structure avoids small particle ZIF-8 is existing
As.
Embodiment 3
40mg monodisperse bakelite resin nano stick and 2.5g cabaltous nitrate hexahydrate are dispersed in the methanol solution of 15mL, so
Afterwards by ultrasonic disperse uniform adsorption metal cobalt ions, the methanol solution of the 15mL dissolved with 1.3g methylimidazole is added,
At room temperature, it is stirred to react 12h, centrifuge washing, drying obtain monodisperse bakelite resin nano stick insertion ZIF-67 composite wood in situ
Expect (RNR/L-ZIF-67).
As depicted in figure 3 a, the crystallinity by the available RNR/L-ZIF-67 of XRD analysis is very high.Attached drawing 3b~d is
The microstructure schematic diagram of the interspersed big partial size ZIF-67 composite material of insertion and SEM scheme monodisperse bakelite resin nano stick in situ,
Showing that monodisperse bakelite resin nano stick is successfully embedded into ZIF-67 crystal in situ, ZIF-67 crystal is regular dodecahedron,
Average grain diameter is in 600nm or so.
Embodiment 4
1) by 150mg monodisperse bakelite resin nano stick, 385mg cabaltous nitrate hexahydrate and the dispersion of 60mg zinc nitrate hexahydrate
In the methanol solution of 25mL, by ultrasonic disperse uniform adsorption metal cobalt ions and zinc ion, add dissolved with 990mg diformazan
The methanol solution of the 25mL of base imidazoles is stirred to react 12h at room temperature, and centrifuge washing, drying obtain monodisperse phenolic resin
Nanometer rods insertion Zn/Co-ZIF composite material (RNR/L-Zn/Co-ZIF) in situ.
As shown in attached drawing 4a, the crystallinity by the available RNR/L-Zn/Co-ZIF of XRD analysis is very high.Attached drawing 4b~d
For monodisperse bakelite resin nano stick, the microstructure schematic diagram of insertion Zn/Co-ZIF composite material and SEM scheme in situ, show list
Successfully insertion is punctured into big partial size Zn/Co-ZIF crystal dispersed phenolic resin nanometer rods in situ, and Zn/Co-ZIF crystal is positive
Dodecahedron, average grain diameter is in 600nm or so.
Embodiment 5
By 200mg monodisperse bakelite resin nano stick, 300mg ferric trichloride and 200mg terephthalic acid (TPA) are dispersed in 12mL
N,N-Dimethylformamide solution in, by ultrasonic disperse uniform adsorption metal iron ion, then the poly- second of 0.5mL is added dropwise
Alkene pyrrolidone (PVP) solution (the n,N-Dimethylformamide solution that 8g PVP is dissolved in 12mL), under conditions of 145 DEG C,
It is condensed back, is stirred to react 1.5h, last centrifuge washing, drying obtain monodisperse bakelite resin nano stick and be embedded in big grain in situ
Diameter Fe-MIL-88 composite material (RNR/L-Fe-MIL-88).
As shown in attached drawing 5a, the crystallinity by the available RNR/L-Fe-MIL-88 of XRD analysis is very high.Attached drawing 5b~d
It is embedded in the microstructure schematic diagram and SEM figure of big partial size Fe-MIL-88 composite material in situ for monodisperse bakelite resin nano stick,
Show that monodisperse bakelite resin nano stick is successfully embedded into Fe-MIL-88 crystal in situ, Fe-MIL-88 crystal is six prisms
Type.
Embodiment 6
150mg monodisperse bakelite resin nano stick and 350mg nickel acetate tetrahydrate are dispersed in the ethanol solution of 50mL,
Add 0.75g PVP；After ultrasonic disperse uniform adsorption metallic nickel ions, under conditions of 90 DEG C, it is condensed back, stirring
React 10h；Last centrifuge washing, drying obtain monodisperse bakelite resin nano stick and are embedded in big partial size Ni-MOF composite wood in situ
Expect (RNR/L-Ni-MOF)；
As shown in fig. 6, the crystallinity by the available RNR/L-Ni-MOF of XRD analysis is very high.Attached drawing 6b~d is
The microstructure schematic diagram of insertion Ni-MOF composite material and SEM scheme monodisperse bakelite resin nano stick in situ, show monodisperse
Bakelite resin nano stick is successfully embedded into Ni-MOF crystal in situ, and Ni-MOF crystal is cubic type.
Claims (6)
- It include following 1. monodisperse bakelite resin nano stick is embedded in the simple universality preparation method of MOF composite material in situ Step: bakelite resin nano stick is evenly dispersed in the solution, metal salt is added and is stirred, ultrasound is eventually adding certain dense The solution containing organic ligand is spent, reaction obtains monodisperse bakelite resin nano stick insertion MOF in situ after centrifugation, washing, drying Composite material.
- 2. the simple universality that monodisperse bakelite resin nano stick according to claim 1 is embedded in MOF composite material in situ Preparation method, it is characterised in that selected metal salt is zinc nitrate hexahydrate, cabaltous nitrate hexahydrate, ferric trichloride or four hydrations Nickel acetate.
- 3. the simple universality that monodisperse bakelite resin nano stick according to claim 2 is embedded in MOF composite material in situ Preparation method, it is characterised in that the zinc nitrate hexahydrate concentration is 15~30mg/mL；Cabaltous nitrate hexahydrate concentration be 10~ 200mg/mL；Ferric trichloride concentration is 20~40mg/mL；Nickel acetate tetrahydrate concentration is 5~20mg/mL.
- 4. the simple universality that monodisperse bakelite resin nano stick according to claim 1 is embedded in MOF composite material in situ Preparation method, it is characterised in that the organic ligand is methylimidazole, terephthalic acid (TPA) or polyvinylpyrrolidone.
- 5. the simple universality that monodisperse bakelite resin nano stick according to claim 4 is embedded in MOF composite material in situ Preparation method, it is characterised in that the methylimidazole solution concentration is 10~40mg/mL；Terephthalic acid solution's concentration is 10~20mg/mL；Polyvinylpyrrolidonesolution solution concentration is 10~50mg/mL.
- 6. the simple universality that monodisperse bakelite resin nano stick according to claim 1 is embedded in MOF composite material in situ Preparation method, it is characterised in that the reaction temperature is 20~40 DEG C, and mixing time is 6~18h.
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| CN113600153A (en) * | 2021-08-27 | 2021-11-05 | 西安理工大学 | Preparation method and application of nickel-based metal organic framework loaded phenolic resin material |
| CN113753883A (en) * | 2021-08-31 | 2021-12-07 | 青岛海洋科学与技术国家实验室发展中心 | Low-interface-resistance carbon microsphere material, and preparation method and application thereof |
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