CN109569605A - A kind of preparation method of new iron-based composite material - Google Patents
A kind of preparation method of new iron-based composite material Download PDFInfo
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- CN109569605A CN109569605A CN201811392304.1A CN201811392304A CN109569605A CN 109569605 A CN109569605 A CN 109569605A CN 201811392304 A CN201811392304 A CN 201811392304A CN 109569605 A CN109569605 A CN 109569605A
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/74—Iron group metals
- B01J23/745—Iron
Abstract
The present invention provides a kind of preparation method of new iron-based composite material, method includes the following steps: mixed solution A is made after (1) measures DMF, methanol and deionization mixing respectively；(2) molysite and 2,5-Dihydroxyterephthalic acid are taken respectively, is placed in mixed solution A, are ultrasonically treated, are obtained mixed solution B；(3) dry carbon cloth and solution B is taken to be transferred together in the stainless steel water heating kettle of teflon lined, then incubation water heating reaction is carried out, it is cooled to room temperature to reaction kettle, take out carbon cloth, air drying is stand-by, removes the upper solution in reaction kettle, centrifugation, again with methanol or ethyl alcohol repeatedly wash, and gained sample is dried in vacuo to obtain sample F e-MOF-74；(4) carbon cloth for taking air drying stand-by, is placed in porcelain boat, and 350~1000 DEG C are calcined 1~5 hour, is cooled to room temperature, new iron-based composite material is made.
Description
Technical field
The present invention relates to a kind of preparation methods of composite material, and in particular to a kind of preparation side of new iron-based composite material
Method.
Background technique
The energy is the important supporting substances of national development, is related to the various aspects such as politics, economic, society and military affairs.Many institutes
Known, world energy sources stock number is limited, and however as the continuous development of current world economy, energy consumption is growing day by day,
It rises one after another all over the world because disputing caused by energy problem, energy crisis is increasingly prominent, corresponding environmental pollution
It is also one of current major issue, countries in the world just actively take measures to be coped with.Therefore, reasonable, clean and efficient land productivity
With the current energy, it is of great significance to global economy and health, stabilization and the sustainable development of society.
Metal-organic framework material (Metal-Organic Frameworks, abbreviation MOFs) be it is a kind of by metal ion with
The novel porous mesh material that organic ligand is connected to form by coordination.It is to utilize organic ligand and metal ion or gold
Belong to cluster by having one-dimensional, two-dimentional or three-dimensional infinite network knot made of coordinate bond or intermolecular interaction self assembly
The crystalline material of structure.Metal ion in MOFs structure is coupled by organic ligand and high degree of dispersion is isolated, while these organic are matched
Body in thermal decomposition process height carbonization can barrier metal reunion, thus be hopeful be made high dispersive, partial size it is small and
Uniform metal or metal oxide nanoparticles, these nanoparticles can be used as active catalytic center.In addition, MOFs heat point
Solution prepares metal or metal oxide also has the advantage that, i.e. the porous carbon of the organic matter pyrolysis generation of ligand or filling,
Meeting portion envelops live metallic particles, to improve the stability of catalyst.
Porous carbon materials have chemical stability height, adsorption capacity strong, acidproof, and alkaline-resisting, heat resistance is strong and more regular
The advantages that gap structure, makes it be used widely in fields such as catalyst carrier, adsorbent and electrochemical energy storages.
The combination of MOFs material derived metallic catalyst and carbon cloth, metallic catalyst can be dispersed in carbon cloth
Surface is conducive to the more catalytic sites of metallic catalyst exposure, is more advantageous to the raising of the mass transfer effect of fluid, make its be forced with
Metallic catalyst derived from MOFs comes into full contact with and reacts.Therefore the new iron-based composite material Fe that the present invention synthesizes3O4@
CFC is expected to the new catalyst as function admirable.
Summary of the invention
The present invention provides a kind of preparation method of new iron-based composite material, method includes the following steps:
(1) after measuring DMF, methanol and deionization mixing respectively, mixed solution A is made, wherein DMF, methanol and deionization
The volume ratio of water is (0.5~50): 1:1；
(2) molysite and 2,5-Dihydroxyterephthalic acid are taken respectively, are placed in mixed solution A obtained by step (1), in ultrasound
Frequency is the condition of 50~100kHz, is ultrasonically treated 30~60 minutes, obtains mixed solution B；
(3) dry carbon cloth and step (2) acquired solution B is taken to be transferred together the stainless steel of teflon lined
In water heating kettle, incubation water heating reaction is then carried out, hydro-thermal reaction 3~72 hours under conditions of temperature is 100~200 DEG C, to
Reaction kettle is cooled to room temperature, and takes out carbon cloth, and air drying is stand-by, removes the upper solution in reaction kettle, centrifugation, then use first
Alcohol or ethyl alcohol repeatedly wash, and gained sample is dried in vacuo to obtain sample F e-MOF-74；
(4) carbon cloth that air drying is stand-by in step (3) is taken, is placed in porcelain boat, 350~1000 DEG C of calcinings 1~5 are small
When, it is cooled to room temperature, new iron-based composite material is made.
Solution temperature in preferred step (2) the of the present invention ultrasonication is no more than 40 DEG C.
Preferably the molar ratio of step (2) the of the present invention molysite and 2,5-Dihydroxyterephthalic acid is 0.5~20:1,
Molysite is Iron(III) chloride hexahydrate or Fe(NO3)39H2O.
Preferred molysite of the present invention is Iron(III) chloride hexahydrate, and Iron(III) chloride hexahydrate and 2,5- dihydroxy is to benzene
The molar ratio of dioctyl phthalate is (1~10): 1.
Preferred molysite of the present invention is Fe(NO3)39H2O, Fe(NO3)39H2O and 2,5- dihydroxy terephthaldehyde
Sour molar ratio is (1~15): 1.
Under conditions of supersonic frequency described in preferred step (2) of the present invention is 60kHz, it is ultrasonically treated 30 minutes.
Preferred step (4) of the present invention is in logical N2Under the conditions of carry out, until its temperature is cooled to room temperature.
The present invention include it is following the utility model has the advantages that
The present invention is auxiliary with hydrothermal synthesis method, so that the Fe-MOF-74 of synthesis is supported on the surface of carbon cloth, then is passed through
Carbonization is crossed, is made and loads a kind of new iron-based multiple of the derivative metallic catalyst of Fe-MOF-74 by catalyst carrier of carbon cloth
Condensation material Fe3O4@CFC, and optimize technological reaction condition, significantly simplified synthesis technology and reduce experimental cost.
Detailed description of the invention
Fig. 1: for the XRD spectrum of Fe-MOF-74 made from embodiment 1；
Fig. 2: for the SEM shape appearance figure of Fe-MOF-74 made from embodiment 1；
Fig. 3: for Fe made from embodiment 13O4The XRD spectrum of@CFC；
Fig. 4: for Fe made from embodiment 13O4The SEM shape appearance figure of@CFC.
Specific embodiment
Embodiment 1: the preparation method of new iron-based composite material includes the following steps
(1) mixed solution A is made after measurement DMF (45mL), methanol (3mL) and deionized water (3mL) mixing respectively,
The volume ratio of middle DMF, methanol and deionized water are 15:1:1；
(2) 0.2728g Iron(III) chloride hexahydrate and 0.1g 2,5-Dihydroxyterephthalic acid are weighed respectively, and one is placed in
In mixed solution A obtained by step 1, in the condition that supersonic frequency is 60kHz, it is ultrasonically treated 30 minutes, obtains mixed solution B；Its
In the molar ratio of six nitric hydrate iron and 2,5- dihydric para-phthalic acid be 3.34:1；
(3) carbon cloth (carbon fiber cloth (CFC)) and step 2 acquired solution B mono- for taking a fritter dry
With being transferred in the stainless steel water heating kettle of teflon lined, incubation water heating reaction is then carried out, the item for being 100 DEG C in temperature
Hydro-thermal reaction 24 hours, are cooled to room temperature to reaction kettle under part, take out carbon cloth, and air drying is stand-by；It is anti-with methanol replacement
The solvent in kettle is answered, it is primary every displacement in 10 hours, it replaces 4 times；Gained sample vacuum under conditions of temperature is 100 DEG C is dry
Dry 8 hours, sample F e-MOF-74 is made；
(4) carbon cloth obtained by step (3) is taken out, is placed in porcelain boat, in logical N2Under conditions of, 600 DEG C are calcined 3 hours,
New iron-based composite material Fe is made3O4@CFC。
Embodiment 2: the preparation method of new iron-based composite material includes the following steps
(1) mixed solution A is made after measurement DMF (17mL), methanol (17mL) and deionized water (17mL) mixing respectively,
Wherein the volume ratio of DMF, methanol and deionized water is 1:1:1；
(2) 0.1633g Iron(III) chloride hexahydrate and 0.1g 2,5-Dihydroxyterephthalic acid are weighed respectively, and one is placed in
In mixed solution A obtained by step 1, in the condition that supersonic frequency is 60kHz, it is ultrasonically treated 30 minutes, obtains mixed solution B；Its
In the molar ratio of six nitric hydrate iron and 2,5- dihydric para-phthalic acid be 2:1；
(3) carbon cloth (carbon fiber cloth (CFC)) and step 2 acquired solution B mono- for taking a fritter dry
With being transferred in the stainless steel water heating kettle of teflon lined, incubation water heating reaction is then carried out, the item for being 110 DEG C in temperature
Hydro-thermal reaction 24 hours, are cooled to room temperature to reaction kettle under part, take out carbon cloth, and air drying is stand-by；It is anti-with ethyl alcohol replacement
The solvent in kettle is answered, it is primary every displacement in 12 hours, it replaces 4 times；Gained sample is dried in vacuo under conditions of temperature is 80 DEG C
10 hours, sample F e-MOF-74 is made；
(4) carbon cloth obtained by step (3) is taken out, is placed in porcelain boat, in logical N2Under conditions of, 550 DEG C are calcined 4 hours,
New iron-based composite material Fe is made3O4@CFC。
Embodiment 3: the preparation method of new iron-based composite material includes the following steps
(1) mixed solution A is made after measurement DMF (45mL), methanol (5mL) and deionized water (5mL) mixing respectively,
The volume ratio of middle DMF, methanol and deionized water are 9:1:1；
(2) 0.3267g Iron(III) chloride hexahydrate and 0.1g 2,5-Dihydroxyterephthalic acid are weighed respectively, and one is placed in
In mixed solution A obtained by step 1, in the condition that supersonic frequency is 100kHz, it is ultrasonically treated 20 minutes, obtains mixed solution B；
Wherein the molar ratio of six nitric hydrate iron and 2,5- dihydric para-phthalic acid are 4:1；
(3) carbon cloth (carbon fiber cloth (CFC)) and step 2 acquired solution B mono- for taking a fritter dry
With being transferred in the stainless steel water heating kettle of teflon lined, incubation water heating reaction is then carried out, the item for being 130 DEG C in temperature
Hydro-thermal reaction 12 hours, are cooled to room temperature to reaction kettle under part, take out carbon cloth, and air drying is stand-by；It is anti-with methanol replacement
The solvent in kettle is answered, it is primary every displacement in 12 hours, it replaces 5 times；Gained sample is dried in vacuo under conditions of temperature is 60 DEG C
12 hours, sample F e-MOF-74 is made；
(4) carbon cloth obtained by step (3) is taken out, is placed in porcelain boat, in logical N2Under conditions of, 700 DEG C are calcined 3 hours,
New iron-based composite material Fe is made3O4@CFC。
Embodiment 4: the preparation method of new iron-based composite material includes the following steps
(1) mixed solution A is made after measurement DMF (45mL), methanol (9mL) and deionized water (9mL) mixing respectively,
The volume ratio of middle DMF, methanol and deionized water are 5:1:1；
(2) 0.408g Iron(III) chloride hexahydrate and 0.1g 2,5-Dihydroxyterephthalic acid are weighed respectively, and one is placed in step
In rapid gained mixed solution A, in the condition that supersonic frequency is 100kHz, it is ultrasonically treated 20 minutes, obtains mixed solution B；Its
In the molar ratio of six nitric hydrate iron and 2,5- dihydric para-phthalic acid be 5:1；
(3) carbon cloth (carbon fiber cloth (CFC)) and step 2 acquired solution B mono- for taking a fritter dry
With being transferred in the stainless steel water heating kettle of teflon lined, incubation water heating reaction is then carried out, the item for being 150 DEG C in temperature
Hydro-thermal reaction 12 hours, are cooled to room temperature to reaction kettle under part, take out carbon cloth, and air drying is stand-by；It is anti-with methanol replacement
The solvent in kettle is answered, it is primary every displacement in 12 hours, it replaces 5 times；Gained sample is dried in vacuo under conditions of temperature is 110 DEG C
6 hours, sample F e-MOF-74 is made；
(4) carbon cloth obtained by step (3) is taken out, is placed in porcelain boat, in logical N2Under conditions of, 800 DEG C are calcined 2 hours,
New iron-based composite material Fe is made3O4@CFC。
Embodiment 5: the preparation method of new iron-based composite material includes the following steps
(1) mixed solution is made after measurement DMF (50mL), methanol (2.5mL) and deionized water (2.5 mL) mixing respectively
A, wherein the volume ratio of DMF, methanol and deionized water is 20:1:1；
(2) 0.49g Iron(III) chloride hexahydrate and 0.1g 2,5-Dihydroxyterephthalic acid are weighed respectively, and one is placed in step
In rapid gained mixed solution A, in the condition that supersonic frequency is 80kHz, it is ultrasonically treated 30 minutes, obtains mixed solution B；Wherein
The molar ratio of six nitric hydrate iron and 2,5- dihydric para-phthalic acid are 6:1；
(3) carbon cloth (carbon fiber cloth (CFC)) and step 2 acquired solution B mono- for taking a fritter dry
With being transferred in the stainless steel water heating kettle of teflon lined, incubation water heating reaction is then carried out, the item for being 160 DEG C in temperature
Hydro-thermal reaction 18 hours, are cooled to room temperature to reaction kettle under part, take out carbon cloth, and air drying is stand-by；It is anti-with methanol replacement
The solvent in kettle is answered, it is primary every displacement in 12 hours, it replaces 4 times；Gained sample is dried in vacuo under conditions of temperature is 100 DEG C
10 hours, sample F e-MOF-74 is made；
(4) carbon cloth obtained by step (3) is taken out, is placed in porcelain boat, in logical N2Under conditions of, 400 DEG C are calcined 5 hours,
New iron-based composite material Fe is made3O4@CFC。
The content of present invention is not limited only to the content of the respective embodiments described above, the group of one of them or several specific embodiments
The purpose of invention also may be implemented in contract sample.
The XRD spectrum for obtaining Fe-MOF-74 material by embodiment 1 is as shown in Figure 1, it was demonstrated that resulting sample is pure phase
Fe-MOF-74 crystal.
Obtain Fe-MOF-74 material SEM appearance figure by embodiment one as shown in Fig. 2, as can be seen from the figure according to
The Fe-MOF-74 of experimental method preparation is spherulite.
New iron-based composite material Fe is obtained by embodiment 13O4The XRD spectrum of@CFC obviously finds Fe-MOF- by Fig. 3
74 after carbonization, and the oxide of iron highlights, more conducively the raising of catalytic activity.
New iron-based composite material Fe is obtained by embodiment 13O4The SEM appearance figure of@CFC is as shown in figure 4, can from figure
To find out the Fe prepared according to embodiment one3O4@CFC material, metallic catalyst derived from Fe-MOF-74 are supported on carbon fiber
The surface of cloth, dispersibility preferably, show new iron-based composite material Fe3O4The success of@CFC preparation.
Claims (7)
1. a kind of preparation method of new iron-based composite material, which is characterized in that method includes the following steps:
(1) after measuring DMF, methanol and deionization mixing respectively, mixed solution A is made, wherein DMF, methanol and deionized water
Volume ratio is (0.5~50): 1:1；
(2) molysite and 2,5-Dihydroxyterephthalic acid are taken respectively, are placed in mixed solution A obtained by step (1), in supersonic frequency
For the condition of 50~100kHz, it is ultrasonically treated 30~60 minutes, obtains mixed solution B；
(3) dry carbon cloth and step (2) acquired solution B is taken to be transferred together the stainless steel hydro-thermal of teflon lined
In kettle, incubation water heating reaction is then carried out, hydro-thermal reaction 3~72 hours under conditions of temperature is 100~200 DEG C, wait react
Kettle is cooled to room temperature, take out carbon cloth, air drying is stand-by, remove reaction kettle in upper solution, centrifugation, again with methanol or
Ethyl alcohol repeatedly washs, and gained sample is dried in vacuo to obtain sample F e-MOF-74；
(4) carbon cloth that air drying is stand-by in step (3) is taken, is placed in porcelain boat, 350~1000 DEG C are calcined 1~5 hour,
It is cooled to room temperature, new iron-based composite material is made.
2. preparation method according to claim 1, which is characterized in that the solution in step (2) described ultrasonication
Temperature is no more than 40 DEG C.
3. preparation method according to claim 1, which is characterized in that step (2) molysite and 2,5- dihydroxy is to benzene
The molar ratio of dioctyl phthalate is (0.5~20): 1, molysite is Iron(III) chloride hexahydrate or Fe(NO3)39H2O.
4. preparation method according to claim 3, which is characterized in that the molysite is Iron(III) chloride hexahydrate, six hydrations
The molar ratio of ferric trichloride and 2,5- dihydric para-phthalic acid are (1~10): 1.
5. preparation method according to claim 3, which is characterized in that the molysite is Fe(NO3)39H2O, nine hydration nitre
Sour iron and 2,5- dihydric para-phthalic acid's molar ratio are (1~15): 1.
6. preparation method according to claim 1, which is characterized in that supersonic frequency described in step (2) is the item of 60kHz
Under part, it is ultrasonically treated 30 minutes.
7. preparation method according to claim 1, which is characterized in that step (4) is in logical N2Under the conditions of carry out, Zhi Daoqi
Temperature is cooled to room temperature.
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Cited By (1)
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