CN101585529A - Method for in-situ preparation of ordered mesoporous carbon/metal composite material by organic template method - Google Patents
Method for in-situ preparation of ordered mesoporous carbon/metal composite material by organic template method Download PDFInfo
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Abstract
The invention relates to a method for in-situ preparation of an ordered mesoporous carbon/metal composite material by an organic template method. Triblock copolymer as a structure guide reagent, polymer resin as a carbon precursor, solid alkali as a catalyst, metal salt with magnetic particles as a metal source are firstly assembled into an organic/inorganic composite film in nonaqueous solvent by sol-gel technology, and then the organic/inorganic composite film is carbonized into the ordered mesoporous carbon/metal composite material. The method used for preparing organic/inorganic composites has the advantages of quick, simple and convenient operation, time conservation and high yield, and realizes the breakthrough of technology for in-situ synthesis of the ordered mesoporous carbon/metal magnetic material with regular pore arrangement under alkaline condition by the organic template method.
Description
Technical field:
The present invention relates to a kind of method of organic formwork method in-situ preparation of ordered mesoporous carbon charcoal/metal composite, belong to technical field of inorganic nanometer material.
Background technology:
Ordered mesoporous carbon material (Ordered Mesoporous Carbon is hereinafter to be referred as OMC) is that a class has that regular pore canal is arranged, the aperture at 2nm between the 50nm, the raw material of wood-charcoal material of aperture size homogeneous.Ordered mesoporous carbon material not only has the high and narrow characteristics of pore size distribution of specific surface area, and has hydrophobicity, unreactiveness, good hydrothermal stability, high mechanical strength and high conductivity.For widening the application of ordered mesopore carbon, introduce metallic particles, make it all have using value widely at aspects such as support of the catalyst, energy storage material, transmitter and conducting materials.
At present, there are two kinds of methods to introduce metallic particles usually.A kind of is by with the ordered mesoporous carbon method of impregnating metal salt repeatedly; Another kind is that carbon source and source metal are introduced in the orderly silicon template simultaneously, obtains the matrix material of ordered mesoporous carbon/metal by carbonization and silica removal process.Dipping-charing that method one need be carried out is repeatedly handled, method two need be removed tensio-active agent and silicon template, operating process is very complicated, have length consuming time, repetition stability is poor, be difficult to deficiency such as a large amount of preparations, thereby limited the extensive application of ordered mesoporous carbon material.
It is corresponding to plant the hard template route therewith, and original position is synthetic to be directly to utilize organic macromolecule to be template, by the effect of non covalent bond organic and inorganic self-assembly, and the method for synthesizing ordered mesoporous charcoal/metal composite.People such as Zhao are at document " the synthesizing ordered mesoporous charcoal/titanic oxide nano compound material of organic and inorganic amphiphilic surfactant self-assembly " (Chem.Mater., 2008,20,1140) report employing resol is carbon matrix precursor in, triblock copolymer is a structure directing agent, ordered mesoporous carbon/titanium dioxide compound has been synthesized in assembling under the neutrallty condition in ethanol system, has investigated the influence of content of titanium dioxide to the mesoscopic structure of gained material simultaneously.As everyone knows, first, synthetic resol is generally line style or low-molecular-weight network size structure in acidity or neutral medium, this structural polymer becomes very easily to cave in the carbon process and destroy in further pyrolysis, be difficult to keep original organic-ordered structure of organic assembly, strengthened the preparation difficulty of ordered mesoporous carbon, and the charcoal aperture that obtains is also less.Synthetic resol then is the higher three-dimensional crosslinked network structure of thermostability in the alkaline medium, easier maintenance ordered structure in carbonization process, and the aperture is shunk less.Second, because mesoporous carbon material has bigger specific surface area and pore volume, make them have wide practical use at aspects such as support of the catalyst, absorption, separation, but the raw material of wood-charcoal material is difficult to separate from solution, be unfavorable for recycling, so utilize the isolating mesoporous carbon material that is magnetic to solve this difficult problem.
On the basis of our former work, with the triblock copolymer is structure directing agent, resin is a carbon matrix precursor, solid alkali is a catalyzer, metal-salt with magnetic particle is a source metal, and wherein the water-wet side PEO in metal-salt and the triblock copolymer molecule forms coordination compound by hydrogen bond action, and assembles the mixture that obtains the three jointly with RF colloidal sol, handle through charing and directly obtain ordered mesoporous carbon/metallicl magnetic material, this material can be used for fields such as magnetic resolution.
Summary of the invention:
The object of the present invention is to provide a kind of method of organic formwork method in-situ preparation of ordered mesoporous carbon charcoal/metal composite, with solve complicated operating process in the prior art, length consuming time, repetition stability poor, be difficult to deficiency such as a large amount of preparations.The material that obtains is convenient to recycling owing to have magnetic after the use.
Method of the present invention is structure directing agent with the segmented copolymer, fluoropolymer resin is a carbon matrix precursor, solid alkali is a catalyzer, metal-salt is a source metal, adopt sol-gel technique to be assembled into the organic/inorganic composite film earlier in volatile polar nonaqueous solvent, charing obtains ordered mesoporous carbon/metal composite then;
Concrete grammar and step are:
The preparation of A organic/inorganic composite film: will gather oxyethylene-poly-propylene oxide-poly-oxyethylene class triblock copolymer and metal-salt, phenol or Resorcinol are dissolved in respectively in the volatile polar nonaqueous solvent, stir and form uniform solution, again two kinds of solution are mixed, add solid alkali as catalyzer, the alkali number that control adds makes the pH value of solution between 7.5～8, stir, then solution is sprawled, treat solvent evaporation, form the organic/inorganic composite film, phenol or Resorcinol, triblock copolymer, solvent, the mass ratio of metal-salt is 3.2: 2: 28: 0.25-1;
The B charing: under nitrogen protection, in 400～1000 ℃ of charings, temperature rise rate is 1 ℃/min, obtains ordered mesoporous carbon/metal composite with steps A synthetic organic/inorganic composite film.
The triblock copolymer that is adopted in organic/inorganic composite synthetic in the steps A of the present invention is poly-oxyethylene-poly-propylene oxide-poly-oxyethylene class triblock copolymer, and (molecular formula is EO as P123
20PO
70EO
20Abbreviation), (molecular formula is EO to P103
17PO
56EO
17Abbreviation), (molecular formula is EO to F127
106PO
70EO
106Abbreviation) or F108 (molecular formula is EO
127PO
48EO
127Abbreviation) etc. (wherein P series expression triblock copolymer is a mashed prod, and F series expression triblock copolymer is a flap, and EO is an oxyethane, and PO is a propylene oxide).
Said metal-salt is Nickelous nitrate hexahydrate, iron nitrate or Xiao Suangu.
Said solid alkali is preferably sodium hydroxide, potassium hydroxide, salt of wormwood or yellow soda ash.
Said volatile polar nonaqueous solvent is the lower volatile polar solvent of boiling point, as ethanol, ethylene glycol or tetrahydrofuran (THF) etc.
The vaporization temperature of solvent is controlled between 10-30 ℃ in the steps A.
The carbonization process of the crosslinking curing of resin and step B is known technology in the steps A.
The vaporization temperature of solvent of the present invention should be controlled between 10-30 ℃, and temperature is low excessively, and evaporation rate is slow, and the time that needs is long, and the product combined coefficient is low; Temperature is too high, and evaporation rate of solvent is fast, will cause organic macromolecule not have the enough time to be assembled into ordered structure in solution and solidifies, and is difficult to form organic assembly of high-sequential.
The present invention adopts segmented copolymer, and resin and metal-salt are assembled the organic/inorganic composite that obtains in alkaline non-aqueous solvent, has swift to operate easyly, saves time the advantage that productive rate is high.Realized adopting the synthetic technological breakthrough of original position under organic formwork method, the alkaline condition with ordered mesoporous carbon/metallicl magnetic material of regular pore canal arrangement.Because the gained material has magnetic, is convenient to recycling during use.
Description of drawings:
Small angle X-ray diffraction (XRD) spectrogram of the ordered mesoporous carbon/nickel composite material of Fig. 1: embodiment 1 preparation.
Suction/desorption the curve of the ordered mesoporous carbon/nickel composite material of Fig. 2: embodiment 1 preparation.
The pore size distribution curve of the ordered mesoporous carbon/nickel composite material of Fig. 3: embodiment 1 preparation.
The magnetic property curve of the ordered mesoporous carbon/nickel composite material of Fig. 4: embodiment 1 preparation.
Embodiment:
The following examples will the present invention is further illustrated, but not thereby limiting the invention.Embodiment 1
For to adopt resorcinol-formaldehyde resin be carbon matrix precursor, triblock copolymer F127 as structure directing agent, sodium hydroxide is that catalyzer, ethanol are that solvent, Nickelous nitrate hexahydrate are that the step of the synthesizing ordered mesoporous raw material of wood-charcoal material/nickel composite material of system of source metal is as follows:
The 2g Resorcinol is dissolved in the 20ml ethanol, magnetic agitation at room temperature, treat its dissolving fully after, dropwise add massfraction and be 37% formaldehyde solution 2.2ml, add 0.03g solid NaOH subsequently, continue stir about 1h.2g F127 and 0.6g Ni (NO
3)
26H
2O is dissolved in the 15ml ethanol, and magnetic agitation treats that it dissolves fully in 30 ℃ of water-baths, adds the above-mentioned ethanolic soln that comprises Resorcinol and formaldehyde then, mixes back stirring in water bath 2h and forms jade-green uniform solution.The pH value that records solution is 7.5～8.0.This solution is transferred in a dishful of shape culture dish, and (25 ℃) make ethanol evaporation under the room temperature, form a jade-green film behind about 12h.With this film 100 ℃ of oven dry 24h in baking oven, make its thermopolymerization diaphragm become dark-brown subsequently.
Above-mentioned film heat-up rate with 1 ℃/min under nitrogen protection is warming up to 700 ℃ of charings, is incubated and naturally cools to room temperature after 2 hours and obtain mesoporous charcoal/nickel composite material.The XRD spectra of this mesoporous charcoal/nickel composite material as shown in Figure 1.On (100), (200) and (211) three crystal faces, the obvious diffraction peak is arranged as can be seen from Figure, illustrate that this material has a cube hole void structure (spacer is Im3m).The N of this material
2Suction/desorption curve as shown in Figure 2, curve is the feature adsorption isotherm thread shape that typically has the mesoporous material of obvious hysteresis loop as can be seen from Figure.The specific surface area of calculating it according to BET (Brunauer-Emmett-Teller) method is 309.3m
2/ g, the pore volume that is calculated by adsorptive capacity is 0.19cm
3/ g.The pore size distribution of this material as shown in Figure 3, its aperture concentrates on 3.52nm as we know from the figure.Learn that from Fig. 4 sample shows significantly magnetic hysteresis loop, has less saturation magnetization and residual magnetization, shows that they not only have certain ferromegnetism but also show paramagnetic feature preferably.
Working method is with embodiment 1, and difference is Ni (NO
3)
26H
2The O consumption is 0.25g, obtains ordered mesoporous carbon/nickel composite material at last.XRD analysis test shows gained material is that the duct has cube ordered mesoporous carbon/nickel composite material of hole void structure.
Working method is with embodiment 1, and difference is Ni (NO
3)
26H
2The O consumption is 1g, obtains ordered mesoporous carbon/nickel composite material at last.XRD analysis test shows gained material is that the duct has cube ordered mesoporous carbon/nickel composite material of hole void structure.
Working method is with embodiment 1, and difference is that the charing organic-inorganic composition obtains ordered mesoporous carbon/nickel composite material under 400 ℃ carbonization temperature.XRD analysis test shows gained material is that the duct has cube ordered mesoporous carbon/nickel composite material of hole void structure.
Working method is with embodiment 1, and difference is that the charing organic-inorganic composition obtains ordered mesoporous carbon/nickel composite material under 1000 ℃ carbonization temperature.XRD analysis test shows gained material is that the duct has cube ordered mesoporous carbon/nickel composite material of hole void structure.
Working method is with embodiment 1, and difference is that ethanol evaporable temperature is controlled at 30 ℃, forms a jade-green polymeric film after about 8 hours, handles the acquisition duct through 400 ℃ charings and has cube ordered mesoporous carbon/nickel composite material of hole void structure.
Embodiment 7
The 2g Resorcinol is dissolved in the 20ml ethanol, magnetic agitation at room temperature, treat its dissolving fully after, dropwise add massfraction and be 37% formaldehyde solution 2.2ml, add 0.025g solid NaOH subsequently, continue stir about 2h.2P123 and 0.6g Ni (NO
3)
26H
2O is dissolved in the 20ml ethanol, and magnetic agitation treats that it dissolves fully in 21 ℃ of water-baths, adds the above-mentioned ethanolic soln that comprises Resorcinol and formaldehyde then, mixes back stirring in water bath 2h and forms jade-green uniform solution.The pH value that records solution is 7.5～8.0.This solution is transferred in a dishful of shape culture dish, and (20 ℃) make ethanol evaporation under the room temperature, form a jade-green film behind about 24h.With this film 100 ℃ of oven dry 24h in baking oven, make its thermopolymerization diaphragm become dark-brown subsequently.
Above-mentioned film heat-up rate with 1 ℃/min under nitrogen protection is warming up to 700 ℃ of charings, is incubated and naturally cools to room temperature after 2 hours and obtain mesoporous charcoal/nickel composite material.XRD analysis test shows gained material is the mesoporous charcoal/nickel composite material of laminate structure.
For to adopt resorcinol-formaldehyde resin be carbon matrix precursor, triblock copolymer F108 as structure directing agent, sodium hydroxide is that catalyzer, ethanol are that solvent, Nickelous nitrate hexahydrate are that the step of the synthesizing ordered mesoporous raw material of wood-charcoal material/nickel composite material of system of source metal is as follows: working method is with embodiment 1, difference be with F108 substitute F127 synthetic organic/organic double compound.XRD analysis test shows gained material is mesoporous charcoal/nickel composite material that the duct has cubic mesoporous structure.
Embodiment 9
For to adopt phenol-formaldehyde resin be carbon matrix precursor, triblock copolymer F127 as structure directing agent, sodium hydroxide is that catalyzer, ethanol are that solvent, Nickelous nitrate hexahydrate are that the step of the synthesizing ordered mesoporous raw material of wood-charcoal material/nickel composite material of system of source metal is as follows: working method is with embodiment 1, and difference is to substitute Resorcinol and the synthetic organic/inorganic composite of formaldehyde with P-F.XRD analysis test shows gained material is mesoporous charcoal/nickel composite material that the duct has cube hole void structure.
For to adopt resorcinol-formaldehyde resin be carbon matrix precursor, triblock copolymer F127 as structure directing agent, nitric hydrate cobalt is that source metal, ethanol are that the step of the synthesizing ordered mesoporous charcoal/cobalt composite material of system of solvent is as follows: working method is with embodiment 1, and difference is to substitute the hydration nickelous nitrate with the hydration Xiao Suangu.XRD analysis test shows gained material is mesoporous charcoal/cobalt composite material that the duct has cube hole void structure.
Embodiment 11
For to adopt resorcinol-formaldehyde resin be carbon matrix precursor, triblock copolymer F127 as structure directing agent, Ferric Chloride Hydrated is that source metal, ethanol are that the step of the synthesizing ordered mesoporous charcoal/iron composite material of system of solvent is as follows: working method is with embodiment 1, and difference is to substitute the hydration nickelous nitrate with Ferric Chloride Hydrated.XRD analysis test shows gained material is mesoporous charcoal/iron composite material that the duct has cube hole void structure.
Embodiment 12
For to adopt resorcinol-formaldehyde resin be carbon matrix precursor, triblock copolymer F127 as structure directing agent, yellow soda ash is that catalyzer, ethanol are that solvent, Nickelous nitrate hexahydrate are that the step of the synthesizing ordered mesoporous raw material of wood-charcoal material/nickel composite material of system of source metal is as follows: working method is with embodiment 1, and difference is with the synthetic organic/inorganic composite of yellow soda ash replace sodium hydroxide.XRD analysis test shows gained material is mesoporous charcoal/nickel composite material that the duct has cube hole void structure.
Embodiment 13
For to adopt resorcinol-formaldehyde resin be carbon matrix precursor, triblock copolymer F127 as structure directing agent, sodium hydroxide is that catalyzer, ethylene glycol are that solvent, Nickelous nitrate hexahydrate are that the step of the synthesizing ordered mesoporous raw material of wood-charcoal material/nickel composite material of system of source metal is as follows: working method is with embodiment 1, and difference is that the spent glycol instead of ethanol synthesizes organic/inorganic composite.XRD analysis test shows gained material is mesoporous charcoal/nickel composite material that the duct has cube hole void structure.
Claims (6)
1. the method for an organic formwork method in-situ preparation of ordered mesoporous carbon charcoal/metal composite, with poly-oxyethylene-poly-propylene oxide-poly-oxyethylene class triblock copolymer is structure directing agent, phenol-formaldehyde resin, resorcinol-formaldehyde resin are carbon matrix precursor, alkali is catalyzer, metal-salt is a source metal, adopt sol-gel technique to be assembled into the organic/inorganic composite film earlier in volatile polar nonaqueous solvent, charing obtains ordered mesoporous carbon/metal then; Concrete grammar and step are:
The preparation of A organic/inorganic composite film: will gather oxyethylene-poly-propylene oxide-poly-oxyethylene class triblock copolymer and metal-salt, phenol or Resorcinol are dissolved in respectively in the volatile polar nonaqueous solvent, stir and form uniform solution, again two kinds of solution are mixed, add solid alkali as catalyzer, the alkali number that control adds makes the pH value of solution between 7.5～8, stir, then solution is sprawled, treat solvent evaporation, form the organic/inorganic composite film, phenol or Resorcinol, triblock copolymer, solvent, the mass ratio of metal-salt is 3.2: 2: 28: 0.25-1;
B charing: steps A synthetic organic/inorganic composite film under nitrogen protection, is obtained ordered mesoporous carbon/metal composite in 400～1000 ℃ of charings.
2. according to the method for claim 1, it is characterized in that: used triblock copolymer is EO
20PO
70EO
20, EO
17PO
56EO
17, EO
106PO
70EO
106Or EO
127PO
48EO
127, wherein EO is an oxyethane, PO is a propylene oxide.
3. according to the method for claim 1, it is characterized in that: said metal-salt is Nickelous nitrate hexahydrate, iron nitrate or Xiao Suangu.
4. according to the method for claim 1, it is characterized in that: said volatile polar nonaqueous solvent is ethanol, ethylene glycol or tetrahydrofuran (THF).
5. according to the method for claim 1, it is characterized in that: said solid alkali is sodium hydroxide, potassium hydroxide, salt of wormwood or yellow soda ash.
6. according to the method for claim 1, it is characterized in that: the vaporization temperature of solvent is controlled between 10-30 ℃ in the steps A.
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