CN105646901A - Green chemical preparation method for nano zeolitic imidazolate framework material - Google Patents
Green chemical preparation method for nano zeolitic imidazolate framework material Download PDFInfo
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Abstract
The invention belongs to the technical field of preparation of a nano zeolitic imidazolate framework material and discloses a green chemical preparation method for the nano zeolitic imidazolate framework material. In order to improve a preparation technique and overcome defects of existing preparation methods, the energy-saving green chemical method is provided for preparing the nano zeolitic imidazolate framework material simply, quickly and massively at the room temperature. The method has the advantages of quickness and simplicity in operation, energy saving, environment friendliness, complete embodiment of a 'green chemistry' purpose and realization of rapid preparation of the uniform nano zeolitic imidazolate framework material nano-JUC-160 at the room temperature. In addition, products prepared according to the method are uniform in particle distribution and about 200nm in particle size and show excellent thermal stability.
Description
Technical field
The invention belongs to nano zeolite imidazate framework material preparing technical field, be specifically related under a kind of room temperature, simple and quick, prepare " Green Chemistry " method of nano zeolite imidazate framework material in a large number.
Background technology
Sharp increase along with population in the world, the level of consumption of people improves constantly, economic acceleration globalizes, each big industry fast development, chemical industry and relevant speciality develop rapidly especially as one of pillar industry in national economy, global environment is also caused, while bringing more material facility and making tremendous economic contribution, the threat that should not be underestimated by this high speed development. Economic development fast but along with the weight of environmental pollution, therebetween contradiction develop further sharp-pointed when, " Green Chemistry " this concept is suggested. " Green Chemistry ", also known as environmentally friendly chemistry or cleaning chemistry, core is in that " Atom economy ": the atomic energy of reactant all transfers desired end product to, it is achieved " zero-emission ", makes full use of resource, energy-conservation environmental protection again. The proposition of " Green Chemistry " makes people while constantly pursuing development of chemical industry, more focuses on the protection to environment.
Nano material is little because of its size, specific surface is big and shows small-size effect, surface and interfacial effect, quantum size effect etc., therefore it has the new features being different from Conventional solid: the character such as optics, electrochemistry, catalysis, chemical reaction, and above characteristic makes nano material in field extensive application such as photoelectron material, battery electrode material, solar cell material, effective catalyst, sensing elements.
Zeolitic imidazolate framework material (ZeoliticImidazolateFrameworks, ZIFs), is a kind of common and particularly important metal-organic framework materials (Metal-OrganicFrameworks, MOFs), is usually by Zn2+��Co2+And Cd2+Form Deng metal ion and the common coordination of one or more glyoxaline ligands. Compare to other class MOFs, ZIFs and not only show more excellent temperature capacity and chemical stability, and there is higher porosity, be therefore widely used in the technical field such as efficient catalytic and separation.
Qiu Shi synthetic fibre seminar once reported a kind of ZIF mixing glyoxaline ligand for 2014, called after JUC-160 (list of references: L.Huang, M.Xue, Q.S.Song, S.R.Chen, Y.Pan, S.L.Qiu, Inorg.Chem.Commun.46 (2014) 9-12), reported ZIF selects Zn2+As coordination center, benzimidazole that two kinds of volumes are bigger and 2-tolimidazole are as part, select DMF (N, dinethylformamide) as solvent, at 180 DEG C, the common coordination of solvent thermal reaction 3 angel three, obtains a kind of novel micron order zeolitic imidazolate framework material.But, there is high temperature and consume energy the defects such as length big, consuming time, Product size be uncontrollable in the method.
Summary of the invention
The preparation method using for reference above-mentioned JUC-160, it is an object of the invention to improve technology of preparing, overcome the defect existing for above-mentioned preparation method, it is provided that under a kind of room temperature, simple and quick, prepare " Green Chemistry " energy-saving method of nano zeolite imidazate framework material in a large number. The method quickly easily operates, energy-conservation and environmental protection, fully demonstrate " Green Chemistry " objective, achieve the quick preparation of even size zeolites imidazate framework material nano-JUC-160 under room temperature condition, product particle obtained by this method is evenly distributed, size is at about 200nm, and shows the heat stability of excellence.
The main preparation process of the present invention is as follows:
1)Zn2+The preparation of coordination center solution
1.5��3g bis-water zinc acetate is joined in 120mLDMF, is stirred at room temperature 10��20 minutes to being completely dissolved after uniformly, obtains solution A;
2) preparation of mixed ligand solution
1��2g benzimidazole is joined in 160mLDMF, is stirred at room temperature 5��10 minutes to after being uniformly dissolved, adding the 2-tolimidazole of 0.8��1.6g, continue stirring 10��20 minutes to complete uniform dissolution, obtain solution B;
3) solution hybrid reaction
Under stirring condition, solution A is slowly added in solution B, makes the two mix homogeneously, and under room temperature, within continuously stirred 10��15 hours, obtain milky white solution;
4) centrifugal
By step 3) gained milky white liquid when 10000��15000r/min centrifugal 10��20 minutes, abandoning supernatant obtains white precipitate;
5) washing, dry
By step 4) gained white precipitate DMF ultrasonic dissolution, and remove supernatant with DMF washing, centrifugal hypsokinesis; Repeated washing, centrifugation step 3��5 times, finally dry gained white precipitate under 60��80 DEG C of conditions;
6) grind
By step 5) dried product is ground to Powdered, can obtain nano zeolite imidazate framework material nano-JUC-160 of the present invention.
Accompanying drawing explanation
Fig. 1: the powder X-ray RD diffraction spectrogram of embodiment 1 sample;
Fig. 2: transmission electron microscope (TEM) photo of embodiment 1 sample;
Fig. 3: the thermogravimetric analysis figure of embodiment 1 sample;
Detailed description of the invention
Embodiment 1: prepare nano zeolite imidazate framework material JUC-160
1.98g bis-water zinc acetate is added in 120mLDMF, is stirred at room temperature 15 minutes to being completely dissolved uniformly, obtains Zn2+Coordination center solution A;
1.18g benzimidazole is added in 160mLDMF, is stirred at room temperature 8 minutes to after being uniformly dissolved, adding the 2-tolimidazole of 1.06g, continue stirring 15 minutes to complete uniform dissolution, obtain mixed ligand solution B;
Under stirring condition, by Zn2+Coordination center solution A is slowly added in mixed ligand solution B, makes the two mix homogeneously, and under room temperature, within continuously stirred 12 hours, obtains milky white solution;
On average being added by this milky white liquid in multiple centrifuge tube, under 12000r/min speed conditions, centrifugal 10min, inclines and manages interior supernatant, can obtain white precipitate;
Gained white precipitate DMF solution is ultrasonic makes it dissolve, and wash with DMF solution, centrifugal, incline supernatant, repeat more than this step 3 time, finally by gained white precipitate in 60 DEG C of oven dryings 12 hours, take out desciccate, be ground to Powdered, nano zeolite imidazate framework material JUC-160 of the present invention.The each yield of product prepared by the present invention is 1.5g, and product grain is uniformly dispersed each other, and size is about 200nm.
Its simulation powder XRD pattern spectrum and products obtained therefrom powder X-ray RD diffraction spectrogram comparison are as shown in Figure 1, a () is the powder X-ray RD diffraction curve of simulation, b powder X-ray RD diffraction curve that () is prepared product, visible analogue spectrums and product spectrogram are identical, it was demonstrated that prepared zeolitic imidazolate framework material JUC-160.
Embodiment 2: embodiment 1 products therefrom carries out transmission electron microscope (Transmissionelectronmicroscope) and analyzes
Products therefrom transmission electron microscope scanned photograph such as Fig. 2, it is seen that prepared product morphology is complete, Granular composite is uniform, and size is all at about 200nm, and therefore prepared zeolitic imidazolate framework material JUC-160 is nanosized product.
Embodiment 3: embodiment 1 products therefrom carries out thermal stability analysis
Prepare product and carry out thermogravimetric analysis, result is Fig. 3 such as, this product visible weightlessness 5.8% between 100��200 DEG C in figure, quality that this temperature range causes runs off the weightlessness being just the evaporation of its surface object hydrone and disengaging and cause, 200��500 DEG C of intervals present a platform area, illustrate that this temperature range product does not have the loss of quality, also illustrate that product can keep the complete of original skeleton in this temperature range, structure collapse phenomenon does not occur. After 500 DEG C, product begins with obvious weightlessness, and this part weightlessness is owing to the structure collapse of product causes, and illustrates that product is heated after 500 DEG C and just starts to decompose, and skeleton just starts to cave in. Thermal gravimetric analysis results demonstrates prepared product good heat stability.
Claims (3)
1. " Green Chemistry " preparation method of nano zeolite imidazate framework material nano-JUC-160, its step is as follows:
1)Zn2+The preparation of coordination center solution
1.5��3g bis-water zinc acetate is joined in 120mLDMF, is stirred at room temperature 10��20 minutes to being completely dissolved after uniformly, obtains solution A;
2) preparation of mixed ligand solution
1��2g benzimidazole is joined in 160mLDMF, is stirred at room temperature 5��10 minutes to after being uniformly dissolved, adding the 2-tolimidazole of 0.8��1.6g, continue stirring 10��20 minutes to complete uniform dissolution, obtain solution B;
3) solution hybrid reaction
Under stirring condition, solution A is slowly added in solution B, makes the two mix homogeneously, and under room temperature, within continuously stirred 10��15 hours, obtain milky white solution;
4) centrifugal
By step 3) gained milky white liquid be centrifuged, abandoning supernatant obtains white precipitate;
5) washing, dry
By step 4) gained white precipitate DMF ultrasonic dissolution, and remove supernatant with DMF washing, centrifugal hypsokinesis; Repeated washing, centrifugation step 3��5 times, finally dry gained white precipitate;
6) grind
By step 5) dried product is ground to Powdered, namely obtains nano zeolite imidazate framework material nano-JUC-160.
2. " Green Chemistry " preparation method of a kind of nano zeolite imidazate framework material nano-JUC-160 as claimed in claim 1, it is characterised in that: step 4) described in centrifugal be when 10000��15000r/min centrifugal 10��20 minutes.
3. " Green Chemistry " preparation method of a kind of nano zeolite imidazate framework material nano-JUC-160 as claimed in claim 1, it is characterised in that: step 5) described in baking temperature be 60��80 DEG C.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108219158A (en) * | 2018-02-01 | 2018-06-29 | 吉林大学 | Covalent organic framework material and preparation method thereof |
| CN108807998A (en) * | 2018-05-30 | 2018-11-13 | 武汉理工大学 | A kind of vanadium base ZIF porous materials and preparation method thereof applied to cathode of lithium battery |
| CN109529933A (en) * | 2018-12-06 | 2019-03-29 | 怀化学院 | ZIF loaded catalyst and the preparation method and application thereof |
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| US20100270239A1 (en) * | 2009-04-24 | 2010-10-28 | Headwaters Technology Innovation, Llc | Zeolite membrane and methods of making and using same for water desalination |
| CN102898448A (en) * | 2012-10-17 | 2013-01-30 | 南京林业大学 | Room temperature water-phase synthesis method for zeolite imidazole ester framework material |
| CN103951684A (en) * | 2014-04-10 | 2014-07-30 | 吉林大学 | Mixed ligand zeolitic imidazole framework, preparation method and application to carbon dioxide selective adsorption |
| CN104817577A (en) * | 2015-04-08 | 2015-08-05 | 广东工业大学 | Preparation method and catalysis applications of efficient and simple zeolite imidazole framework ZIF-8 crystals with different morphologies |
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2016
- 2016-03-28 CN CN201610183606.2A patent/CN105646901A/en active Pending
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| US20100270239A1 (en) * | 2009-04-24 | 2010-10-28 | Headwaters Technology Innovation, Llc | Zeolite membrane and methods of making and using same for water desalination |
| CN102898448A (en) * | 2012-10-17 | 2013-01-30 | 南京林业大学 | Room temperature water-phase synthesis method for zeolite imidazole ester framework material |
| CN103951684A (en) * | 2014-04-10 | 2014-07-30 | 吉林大学 | Mixed ligand zeolitic imidazole framework, preparation method and application to carbon dioxide selective adsorption |
| CN104817577A (en) * | 2015-04-08 | 2015-08-05 | 广东工业大学 | Preparation method and catalysis applications of efficient and simple zeolite imidazole framework ZIF-8 crystals with different morphologies |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108219158A (en) * | 2018-02-01 | 2018-06-29 | 吉林大学 | Covalent organic framework material and preparation method thereof |
| CN108807998A (en) * | 2018-05-30 | 2018-11-13 | 武汉理工大学 | A kind of vanadium base ZIF porous materials and preparation method thereof applied to cathode of lithium battery |
| CN109529933A (en) * | 2018-12-06 | 2019-03-29 | 怀化学院 | ZIF loaded catalyst and the preparation method and application thereof |
| CN109529933B (en) * | 2018-12-06 | 2021-10-22 | 怀化学院 | ZIF supported catalyst and preparation method and application thereof |
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Application publication date: 20160608 |