CN105032489B - A kind of degradating organic dye CuMOFs method for preparing catalyst - Google Patents
A kind of degradating organic dye CuMOFs method for preparing catalyst Download PDFInfo
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- CN105032489B CN105032489B CN201510354928.4A CN201510354928A CN105032489B CN 105032489 B CN105032489 B CN 105032489B CN 201510354928 A CN201510354928 A CN 201510354928A CN 105032489 B CN105032489 B CN 105032489B
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Abstract
The invention discloses a kind of preparation method of degradating organic dye CuMOFs (Cu (bpmbd) (CHDC)) catalyst, comprise the following steps：Under room temperature condition, 0.6mmol CHDC (Isosorbide-5-Nitrae Cyclohexane dicarboxylic acid) are dissolved into 20ml water, 1.2mmol NaOH is added, fully adds 0.6mmol Cu (NO after dissolving3)2·3H2O, filtered after dissolving, filtrate, which is slowly dropped to, has dissolved 0.6mmol bpmbd (N, the ylmethylene benzene 1 of N bis pyridin 4,4 diamine) part 20ml methanol solutions in, stirring reaction 3h at room temperature, it is required sample that vacuum filtration, which is dried to obtain black powder,；Prepare sample and can be used for catalytic degradation organic dyestuff.Advantages of the present invention is：Preparation process is very simple, Non-energy-consumption etc.；Prepared sample has higher catalytic oxidation activity, energy efficient degradation of organic dye waste water, new technique direction is provided for purification of waste water, there is potential application value in terms of dye wastewater treatment.
Description
Technical field
The present invention relates to a kind of preparation method of CuMOFs catalyst, specially a kind of Cu (bpmbd) (CHDC) catalyst
Preparation method.
Background technology
MOFs has good adsorption separation performance and photo-catalysis capability, and in recent years, research worker utilizes MOFs pairs
Many kinds of substance is separated and studied in aqueous phase, and MOFs shows the incomparable good treatment effect of other materials, is
Wastewater purification technology provides new technique direction.Ligand species containing N are various, and configuration is various, for example, imidazoles, pyridine, triazole,
Tetrazole and their derivative etc., N atoms have very strong coordination ability, and the part of heterocyclic containing N has multiple coordinations
Point, can be with the multidimensional complex of metallic ion coordination composite structure stabilization；The carboxyl of carboxylic acids part has unique electronics knot
Structure can form the topological structure of uniqueness and interesting property.Therefore, when constructing metal-organic framework materials, can make full use of
The coordination mode and design feature of both parts, obtain the MOFs materials of unique energy.
The content of the invention
, being capable of catalysis oxidation drop to provide one kind it is an object of the invention to provide a kind of preparation method of CuMOFs catalyst
Solve a kind of raw catelyst of organic dyestuff.
The purpose of the present invention can be achieved through the following technical solutions.
A kind of preparation method of CuMOFs catalyst, its step are as follows：
（1）Weigh 0.6mmol CHDC to be dissolved into 20ml deionized waters, add 1.2mmol NaOH, treat fully to react
Afterwards, 0.6mmol mantoquitas are added, are fully filtered after reaction.
（2）Bpmbd 0.1718g are weighed to be dissolved into 20ml organic solvents.
（3）Filtrate in step 1 is slowly dropped in the solution of step 2, stirring reaction, vacuum filtration is dried to obtain required
Sample.
Step（1）Middle mantoquita is Cu (NO3)2·3H2O。
Step（2）Middle organic solvent is methanol, ethanol, ether.
Step（3）The middle stirring reaction time is 1h, 2h, 3h.
Brief description of the drawings
Fig. 1 is the SEM figures that sample is made in embodiment 1；
Fig. 2 is the infrared spectrum that sample is made in embodiment 1；
Fig. 3 is the XRD that sample is made in embodiment 1；
Fig. 4 is the BET figures that sample is made in embodiment 1；
Fig. 5 is that the degradation curve figure that sample is catalyzed dyestuff, (1) methyl orange is made in embodiment 1;(2) it is orange;(3) it is sub-
Methyl blue;(4) rose-red;(5) malachite green.
Embodiment
Further detailed, complete explanation is done to the present invention with reference to embodiment：
Embodiment 1
Under room temperature condition, 0.6mmol CHDC are weighed, are dissolved into 20ml water, add 1.2mmol NaOH to above-mentioned solution
In, after dissolving completely, add 0.6mmol Cu (NO3)2·3H2O, filtered after dissolving, filtrate is slowly dropped to dissolving
In the 20ml methanol solutions of 0.6mmol bpmbd parts, stirring reaction 3h, vacuum filtration are dried to obtain black powder at room temperature
Sample.
Embodiment 2
The operating procedure of embodiment 1 is repeated, difference is that organic solvent is ethanol, as a result similar with embodiment 1, but
It is that sample growing amount is less.
Embodiment 3
The operating procedure of embodiment 1 is repeated, difference is that organic solvent is ether, as a result similar with embodiment 1, but
The sample bolus of generation is got together.
Embodiment 4
The operating procedure of embodiment 1 is repeated, difference is that the reaction time is 1h, as a result similar with embodiment 1.
Embodiment 5
The operating procedure of embodiment 1 is repeated, difference is that the reaction time is 2h, as a result similar with embodiment 1.
Fig. 1 is the SEM figures that sample is made in embodiment 1, and sample is bulk, and its particle diameter is about 2-5 μm.Fig. 2 is that embodiment 1 is made
Obtain the infrared spectrum of sample；Sample functional group does not change before and after catalysis, 2924.81cm-1Locate to stretch for C-H in CHDC phenyl ring skeletons
Contracting vibration peak, 2852.73cm-1It is carboxylic for C-H stretching vibrations on organic ligand bpmbd phenyl ring and pyridine ring, 1633.03,1605
Base vibration peak, 1477-1213cm-1For the skeletal vibration of phenyl ring and pyridine ring.Fig. 3 is the XRD that sample is made in embodiment 1；Urge
XRD after change before the XRD of sample and catalysis is almost just the same, and is all polycrystalline, and the crystal quality after catalysis is constant, recyclable
Utilize.Fig. 4 is the BET figures that sample is made in embodiment 1；The N of sample2Isothermal adsorption desorption curve is IV type, for typical mesoporous material
Expect, in whole adsorption process, adsorbance gently increases.CuMOFs specific surface areas are 57.03364m2/ g, langmuir compare surface
Product is 96.318m2/ g, BJH absorption average pore size are 8.418 nm, and BJH absorption accumulation total pore volumes are 0.214cm3/g.Fig. 5
The degradation curve figure that sample is catalyzed dyestuff is made for embodiment 1, and sample is to methyl orange and orange has obvious degradation selectivity to imitate
Fruit, at room temperature, 20mg samples 2h is respectively 58.71% to 125ml 12ppm methyl oranges, orange catalyzing oxidizing degrading rate,
33.26%。
The preferred embodiments of the present invention are the foregoing is only, are not intended to limit the invention, for those skilled in the art
For member, the present invention can have various modifications and variations.Any modification within the spirit and principles of the invention, being made,
Equivalent substitution, improvement etc., it all should be included within protection scope of the present invention.
Claims (4)
- A kind of 1. preparation method of degradating organic dye CuMOFs catalyst, it is characterised in that：Its step is as follows：（1）Weigh 0.6mmol CHDC to be dissolved into 20ml deionized waters, add 1.2mmol NaOH, after abundant reaction, add Enter 0.6mmol mantoquitas, fully filtered after reaction；（2）Bpmbd 0.1718g are weighed to be dissolved into 20ml organic solvents；（3）By step（1）Middle filtrate is slowly dropped to step（2）Solution in, stirring reaction, vacuum filtration be dried to obtain needed for Sample.
- A kind of 2. preparation method of degradating organic dye CuMOFs catalyst according to claim 1, it is characterised in that：Step Suddenly（1）Middle mantoquita is Cu (NO3)2·3H2O。
- A kind of 3. preparation method of degradating organic dye CuMOFs catalyst according to claim 1, it is characterised in that：Step Suddenly（2）Middle organic solvent is one kind in methanol, ethanol or ether.
- A kind of 4. preparation method of degradating organic dye CuMOFs catalyst according to claim 1, it is characterised in that：Step Suddenly（3）The middle stirring reaction time is 1h, 2h, 3h.
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| CN102784562A (en) * | 2012-08-09 | 2012-11-21 | 大连理工大学 | Method for preparing metal organic framework film |
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