CN105837509A - Preparation method of 2-methylimidazole and zinc complex with hierarchical porous structure - Google Patents
Preparation method of 2-methylimidazole and zinc complex with hierarchical porous structure Download PDFInfo
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- B01J20/28057—Surface area, e.g. B.E.T specific surface area
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Abstract
A preparation method of a 2-methylimidazole and zinc complex with a hierarchical porous structure comprises the following steps: 1, mixing arranged soluble polystyrene microspheres adopted as a template with methanol and 2-methylimidazole, and stirring to obtain a solution a; and 2, dissolving zinc nitrate hydrate in methanol to obtain a solution b, adding the solution b to the solution a in a dropwise manner 5min later, stirring the solution a and the solution b at room temperature for 24h, centrifuging the obtained solution mixture, washing the obtained material to obtain a white solid, and removing the arranged soluble polystyrene microsphere template at 80DEG C by using N,N-dimethyl formamide or toluene to obtain the 2-methylimidazole and zinc complex with a hierarchical porous structure. The preparation method has the advantages of simplicity, wide sources of raw materials, low cost and easy industrial amplified production; and the above material finally prepared through the method has the advantages of high specific surface area, facilitation of enhancement of the hydrophobicity and diffusion of organic solvents due to macro-pores, meso-pores and micro-pores, large adsorption quantity of the organic solvents, and certain hydrophobicity.
Description
Technical field
The present invention relates to hydrophobic organic solvent adsorbing material, be specifically related to a kind of 2-with hierarchical porous structure
The preparation method and applications of Methylimidazole. Zn complex.
Background technology
Metal-organic framework materials (MOFs), due to its composition and the controllability in hole, is widely used in catalysis,
Fluorescence, the field such as gas absorption, but the hole that most MOFs has is less than 2nm, limits bigger molecule
Enter inside its duct, and then limit its related application.
The MOFs under synthesis meso-scale with hierarchy makes it have macropore simultaneously, and mesoporous, micropore is permissible
Improve the connectivity of MOFs so that it is expose more surface activity site, and then improve its catalysis, absorption etc.
Performance.But, the MOFs of most hierarchies only has unordered macropore, mesoporous, and this kind of material should
Narrower by scope, focus mostly in catalysis, absorbing dye.
Summary of the invention
The present invention purpose be for above-mentioned existing problems, it is provided that a kind of 2-methyl miaow with hierarchical porous structure
The preparation method and applications of azoles Zn complex, prepared by the method has the 2-methylimidazole zinc of hierarchical porous structure
Coordination compound is big to organic solvent adsorbance, has certain hydrophobicity；Preparation method is simple, and raw material sources are extensive,
Low cost, it is easy to industrial amplification production.
Technical scheme:
The preparation method of a kind of 2-methylimidazole Zn complex with hierarchical porous structure, comprises the following steps:
1) with the solvable polystyrene microsphere of arrangement as template, and methanol, 2-methylimidazole mix and blend,
To solution a, the amount ratio that solvable polystyrene microsphere is template, methanol and 2-methylimidazole of arrangement is 0.2g:
58mL:1.311g；
2) zinc nitrate hydrate being dissolved in methanol, zinc nitrate hydrate is 0.298g:2mL with the amount ratio of methanol,
Obtain solution b, after 5 minutes, solution b is added dropwise in solution a, under room temperature, stir 24h, centrifugal second
Alcohol washing obtains white solid, then removes arrangement at 80 DEG C with DMF or toluene
Solvable polystyrene microsphere template, obtains the 2-methylimidazole Zn complex with hierarchy.
The synthetic method of the solvable polystyrene microsphere template of described arrangement, comprises the steps:
1) by styrene, methacrylic acid and H2O is mix homogeneously at 80 DEG C, obtains solution c, styrene,
Methacrylic acid and H2The amount ratio of O is 54mL:6mL:450mL；
Potassium peroxydisulfate is dissolved in H by 2}2Obtained solution d in O, potassium peroxydisulfate and 30mLH2The amount ratio of O is
0.6g:30mL；
3) solution d is added in solution c, continuously stirred 24h, white solid will be obtained after being centrifuged and use respectively
Water and ethanol respectively wash three times, are then the H of 1:1 by volume ratio2O and the mixed liquor dispersing solid of ethanol, shape
Become suspension, after being centrifuged off supernatant under 4000r/min, solid is dried, obtain containing intermingle with of arrangement
Phenylethylene micro ball template.
The application of a kind of prepared 2-methylimidazole Zn complex with hierarchical porous structure, is used for adsorbing first
Alcohol, ethanol, normal hexane, pentane, toluene, benzene, dichloromethane, petroleum ether, methyl-silicone oil, N, N-
Dimethylformamide or vegetable oil.
The invention have the advantage that this preparation method is simple, raw material sources are extensive, low cost, it is easy to industrialization is put
Big production；Material prepared by the method has high specific surface area, has macropore simultaneously, mesoporous, and micropore has
It is beneficial to strengthen hydrophobicity and the diffusion of organic solvent, big to organic solvent adsorbance, there is certain hydrophobicity.
Accompanying drawing explanation
Fig. 1 is the X-ray powder diffraction figure of the 2-methylimidazole Zn complex with hierarchy.
Fig. 2 is the 77K isothermal nitrogen adsorption desorption data of the 2-methylimidazole Zn complex with hierarchy,
Illustration is graph of pore diameter distribution.
Fig. 3 is the adsorpting data figure to different organic solvents of the 2-methylimidazole Zn complex with hierarchy.
Fig. 4 is that the 2-methylimidazole Zn complex with hierarchy is to Ethanol Adsorption loop-around data figure.
Detailed description of the invention
In order to introduce this patent the most meticulously, now enumerate a specific embodiment for explanation, Dian Xingshi
Execute example and be directed to reference when being embodied as, and be not suitable for limiting the present invention.
Embodiment:
A kind of preparation method of the 2-methylimidazole Zn complex with hierarchical porous structure, step is as follows:
1) preparation of the solvable polystyrene microsphere template arranged
By 54mL styrene, 6mL methacrylic acid and 450mL H2O is mix homogeneously at 80 DEG C, obtains
Solution c；0.6g potassium peroxydisulfate is dissolved in 30mL H2Obtained solution d in O；Solution d is added in solution c,
Continuously stirred 24h, will obtain white solid after being centrifuged and respectively wash three times with water and ethanol respectively, then use volume
Than the H for 1:12O and the mixed liquor dispersing solid of ethanol, form suspension, be centrifuged and remove under 4000r/min
After removing supernatant, solid is dried, obtains the solvable polystyrene microsphere template of arrangement.
2) with 0.2g arrangement solvable polystyrene microsphere as template, with 8mL methanol, 1.311g 2-methyl miaow
Azoles mix and blend, obtains solution a；
3) 0.298g zinc nitrate hydrate is dissolved in 2mL methanol and obtains solution b, after 5 minutes by solution b by
Being added dropwise in solution a, stir 24h under room temperature, centrifugal washing with alcohol obtains white solid, then with N,
Dinethylformamide removes the solvable polystyrene microsphere template of arrangement at 80 DEG C, obtains having classification knot
The 2-methylimidazole Zn complex of structure.
Fig. 1 is the X-ray powder diffraction figure of the 2-methylimidazole Zn complex with hierarchy, shows it
There is preferable crystallinity.
Fig. 2 is the 77K isothermal nitrogen adsorption desorption data of the 2-methylimidazole Zn complex with hierarchy,
Illustration is graph of pore diameter distribution.Figure can be seen that the micropore mainly containing about 1nm on material, about 50nm
Mesoporous, adsorption desorption data can be seen that the specific surface area at material is 1058 square metres every gram, and has big
Hole.
The prepared 2-methylimidazole Zn complex with hierarchical porous structure is for adsorbing ethanol, and method is as follows:
Take bottle one and weigh the quality (M of empty bottleEmpty), weigh that 0.1g prepares has hierarchy
2-methylimidazole Zn complex (MSample) add in bottle, it is subsequently adding 1mL ethanol and is sufficiently mixed, 5min
Ethanol that rear sucking-off is unnecessary also weighs the gross mass (M of bottle and inner sampleAlways), then utilize formula (MAlways—MEmpty—MSample)/MSampleCalculate this sample adsorbance to ethanol.
According to above-mentioned identical method, the prepared 2-methylimidazole Zn complex with hierarchical porous structure is divided
It is not used for adsorbing methanol, ethanol, normal hexane, pentane, toluene, benzene, dichloromethane, petroleum ether, methyl
Silicone oil, vegetable oil.
Fig. 3 is the adsorpting data figure to different organic solvents of the 2-methylimidazole Zn complex with hierarchy.
Result show this material to methanol, ethanol, normal hexane, pentane, toluene, benzene, dichloromethane, petroleum ether,
Methyl-silicone oil, vegetable oil organic solvent averagely has the adsorbance of more than 200%.
Fig. 4 is that the 2-methylimidazole Zn complex with hierarchy is to Ethanol Adsorption loop-around data figure.Result shows
After showing this material circulation 10 times, adsorbance the most significantly reduces.
More than for attempting a preferred embodiment, do not constitute the restriction that patent content is realized, any substantial equivalence
Substitute and the change of the optimization of operation, condition is revised and merges, all in scope of patent protection.Describing and saying
Employing a small amount of necessary term time bright, it is also not construed as limiting the present invention.
Claims (3)
1. the preparation method of a 2-methylimidazole Zn complex with hierarchical porous structure, it is characterised in that include
Following steps:
1) with the solvable polystyrene microsphere of arrangement as template, and methanol, 2-methylimidazole mix and blend,
To solution a, the amount ratio that solvable polystyrene microsphere is template, methanol and 2-methylimidazole of arrangement is 0.2g:
58mL:1.311g；
2) zinc nitrate hydrate being dissolved in methanol, zinc nitrate hydrate is 0.298g:2mL with the amount ratio of methanol,
Obtain solution b, after 5 minutes, solution b is added dropwise in solution a, under room temperature, stir 24h, centrifugal second
Alcohol washing obtains white solid, then removes arrangement at 80 DEG C with DMF or toluene
Solvable polystyrene microsphere template, obtains the 2-methylimidazole Zn complex with hierarchy.
The most according to claim 1, there is the preparation method of the 2-methylimidazole Zn complex of hierarchical porous structure,
It is characterized in that: the synthetic method of the solvable polystyrene microsphere template of described arrangement, comprise the steps:
1) by styrene, methacrylic acid and H2O is mix homogeneously at 80 DEG C, obtains solution c, styrene,
Methacrylic acid and H2The amount ratio of O is 54mL:6mL:450mL；
Potassium peroxydisulfate is dissolved in H by 2}2Obtained solution d in O, potassium peroxydisulfate and 30mLH2The amount ratio of O is
0.6g:30mL；
3) solution d is added in solution c, continuously stirred 24h, white solid will be obtained after being centrifuged and use respectively
Water and ethanol respectively wash three times, are then the H of 1:1 by volume ratio2O and the mixed liquor dispersing solid of ethanol, shape
Become suspension, after being centrifuged off supernatant under 4000r/min, solid is dried, obtain containing intermingle with of arrangement
Phenylethylene micro ball template.
3. an application for the 2-methylimidazole Zn complex with hierarchical porous structure prepared by claim 1,
It is characterized in that: be used for adsorbing methanol, ethanol, normal hexane, pentane, toluene, benzene, dichloromethane, stone
Oil ether, methyl-silicone oil, DMF or vegetable oil.
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Cited By (4)
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| CN106540707A (en) * | 2016-11-03 | 2017-03-29 | 重庆工商大学 | A kind of preparation method of polymolecularity Cu bases cerium oxide composite catalyst |
| CN106861637A (en) * | 2017-03-30 | 2017-06-20 | 丽水学院 | A kind of method that use Zn-ef ficiency doping improves the water stabilities of ZIF 67 |
| CN109433238A (en) * | 2018-10-10 | 2019-03-08 | 北京化工大学 | Iron-nitrogen doped oxygen reduction carbon catalyst with ordered hierarchical pores and preparation method thereof |
| CN110305331A (en) * | 2019-07-02 | 2019-10-08 | 南开大学 | The method that ligand selection reservation method constructs multi-stage porous MOF |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106540707A (en) * | 2016-11-03 | 2017-03-29 | 重庆工商大学 | A kind of preparation method of polymolecularity Cu bases cerium oxide composite catalyst |
| CN106861637A (en) * | 2017-03-30 | 2017-06-20 | 丽水学院 | A kind of method that use Zn-ef ficiency doping improves the water stabilities of ZIF 67 |
| CN109433238A (en) * | 2018-10-10 | 2019-03-08 | 北京化工大学 | Iron-nitrogen doped oxygen reduction carbon catalyst with ordered hierarchical pores and preparation method thereof |
| CN110305331A (en) * | 2019-07-02 | 2019-10-08 | 南开大学 | The method that ligand selection reservation method constructs multi-stage porous MOF |
| CN110305331B (en) * | 2019-07-02 | 2021-09-28 | 南开大学 | Method for constructing hierarchical porous MOF (metal organic framework) by ligand selective retention method |
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