CN108940208A - MIL-100(Fe) material and its preparation method and application - Google Patents
MIL-100(Fe) material and its preparation method and application Download PDFInfo
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/223—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material containing metals, e.g. organo-metallic compounds, coordination complexes
- B01J20/226—Coordination polymers, e.g. metal-organic frameworks [MOF], zeolitic imidazolate frameworks [ZIF]
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/02—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
- B01J20/28057—Surface area, e.g. B.E.T specific surface area
- B01J20/28066—Surface area, e.g. B.E.T specific surface area being more than 1000 m2/g
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
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- B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
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- B01D2257/00—Components to be removed
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- B01D2257/702—Hydrocarbons
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Abstract
The present invention relates to a kind of MIL-100 (Fe) materials and its preparation method and application, mainly solve the problems, such as that adsorbance is low in the prior art.The present invention is 1500-2500m by using a kind of MIL-100 (Fe) material, the specific surface area of MIL-100 (Fe) material2/ g, mesoporous pore size are that the technical solution of 2.6-20nm and its preparation method and application preferably solves the above problem, be can be used in benzene homologues absorption.
Description
Technical field
The present invention relates to a kind of MIL-100 (Fe) materials and its preparation method and application.
Background technique
In recent years, the environmental pollution got worse has caused extensive concern both domestic and external, and how effective Environment control is dirty
Dye also becomes the research hotspot of today's society.Volatile organic matter (VOCs) is a key factor for leading to environmental pollution,
VOCs includes benzene homologues (benzene,toluene,xylene, ethylbenzene etc.), alkanes, aldoketones and chlorinated hydrocabon etc., its production, storage and transportation,
It can be diffused into due to volatilization in environment in use process, so as to cause environmental pollution.Wherein, benzene homologues are due to having strong cause
Cancer and refractory organics cause very big threat to human health and ecological environment.In addition, country " petroleum refining industry pollutant row
Put standard " (GB31570-2015) and " petro chemical industry pollutant emission standard " (GB31571-2015) to the rows of benzene homologues
Putting limitation, more stringent (emission limit of benzene,toluene,xylene is respectively 4,15,20mg/m3).Therefore, effective Environment control
In benzene homologues, reduce to the harm of human body and the destruction of ecological environment, be very necessary.
Adsorption technology be in processing environment in, one of the effective technology of medium/low concentration benzene series matter VOCs, and adsorbent material is whole
The core of a adsorption technology.Porous material is the adsorbent of most-often used removing benzene homologues, the active charcoal of common adsorbent,
Activated carbon fibre, silica gel, molecular sieve etc..Lesser specific surface area (the 200-1000m such as silica gel, molecular sieve2/ g) it limits to benzene
It is the adsorption capacity of object；And active carbon limits diffusion and biography of the macromoleculars such as benzene homologues in its duct mostly based on micropore
Matter rate, desorption process are also more difficult.Therefore, developing novel, safe, efficient benzene homologues adsorbent material is a future
Project that is bright but having much challenge.
Metal-organic framework materials (MOFs) are a kind of novel stephanoporate framework materials, it is to be matched by metal ion with organic
The three-dimensional network skeleton crystalline material for the compound with regular structure that body is self-assembly of.With traditional adsorbent material phase such as active carbon, molecular sieve
Than the huge specific surface area (1000-10000m of MOFs material2/ g), high porosity, adjustable pore size, multiplicity skeleton knot
The advantages that structure, makes it have very high gas absorption capacity and adsorptive selectivity.However, most of MOFs belong to micropore (< 2nm)
Material limits the diffusion to macromoleculars such as benzene homologues and mass transfer rate, affects adsorption capacity to a certain extent.And contain Jie
The MOFs material of hole (2-50nm) structure has in terms of benzene homologues absorption to have great advantage.On the one hand, the microcellular structure in material
The high-specific surface area and high porosity that ensure that material can accommodate more benzene homologues molecules；On the other hand, meso-hole structure mentions
High diffusions and mass transfer rate of the benzene homologues in material duct, are expected to realize efficient, the quick suction of benzene homologues VOCs in environment
Attached removal.MIL-100 (Fe) material skeleton structure is stablized, but in reported MIL-100 (Fe) material, cannot have simultaneously compared with
High-specific surface area and biggish mesoporous pore size, so that limiting the adsorbance to benzene homologues.
Therefore, MIL-100 (Fe) material a kind of containing meso-hole structure and with high specific surface area is developed, ring is used for
In in border, the removal of the efficient, quick adsorption of medium/low concentration benzene series matter be that very significant and currently available technology needs to solve
The problem of.
Summary of the invention
The first technical problem to be solved by the present invention is the problem that adsorbance is low in the prior art, is provided a kind of new
MIL-100 (Fe) material.The material has the advantages that adsorbance is high.The second technical problem to be solved by the present invention is proposition one
The preparation method of kind and corresponding MIL-100 (Fe) material one of the technical issues of solution.Technology to be solved by this invention
Problem third is that proposing a kind of with the purposes of corresponding MIL-100 (Fe) material one of the technical issues of solution.
One of in order to solve the above problem, The technical solution adopted by the invention is as follows: a kind of MIL-100 (Fe) material, described
The specific surface area of MIL-100 (Fe) material is 1500-2500m2/ g, mesoporous pore size 2.6-20nm.
In above-mentioned technical proposal, it is preferable that the mesoporous pore size of MIL-100 (Fe) material is 2.6-10nm.
In above-mentioned technical proposal, it is highly preferred that the mesoporous pore size of the MIL-100 (Fe) material is 2.7-9nm.
In order to solve the above problem two, The technical solution adopted by the invention is as follows: a kind of preparation of MIL-100 (Fe) material
Method includes the following steps:
(1) raw material mixes: weighing metal salt, organic ligand, template, expanding agent by required molar ratio, is added separately to
It fills in the reaction vessel of reaction dissolvent, stirs evenly；
(2) heating reaction: uniformly mixed reaction solution is moved in pressure-resistant reaction vessel, heating stirring is anti-in oil bath pan
It answers；
(3) it removes removing template: stopping heating, be cooled to room temperature, filter；Obtained solid is washed with solvent, and it is molten that low boiling point is added
Agent is heated to reflux；
(4) activate: it is cooling to filter, by solid in drying box heat-activated to get MIL-100 (Fe) material；
Wherein, in step (1), the metal salt is Fe (NO3)3·9H2O、FeCl3·6H2One of O；It is described organic
Ligand is Trimesic acid or 1,3,5- benzenetricarboxylic acid trimethyl；The template is cetyl trimethylammonium bromide or 12
Alkyl phosphate；The expanding agent is 1,3,5- trimethylbenzene or citric acid；Metal salt and organic ligand molar ratio are 1~3:1；
Organic ligand, template and expanding agent molar ratio are 1:0.1~0.3:0.05~0.1；Reaction dissolvent is N, N- dimethyl methyl
Amide or N, N- diethylformamide.
In above-mentioned technical proposal, it is preferable that in step (1), the metal salt is Fe (NO3)3·9H2O, it is described organic to match
Body is Trimesic acid, and the template is cetyl trimethylammonium bromide, and the expanding agent is 1,3,5- trimethylbenzenes.
In above-mentioned technical proposal, it is preferable that in step (2), the oil bath pan stirring rate is 200-800rpm, heating temperature
Degree is 60-150 DEG C, heating time 6-48h.
In above-mentioned technical proposal, it is highly preferred that the oil bath pan stirring rate is 300-500rpm, heating in step (2)
Temperature is 100-150 DEG C, heating time 12-24h.
In above-mentioned technical proposal, it is preferable that in step (3), the cleaning solvent includes ethyl alcohol, N, N- diethylformamide
Or N,N-dimethylformamide；Low boiling point solvent is at least one of ethyl alcohol, methylene chloride, chloroform.
In above-mentioned technical proposal, it is preferable that in step (4), heating temperature is 80-150 DEG C, activation time 2-48h.
In above-mentioned technical proposal, it is highly preferred that heating temperature is 120-150 DEG C, activation time 12- in step (4)
24h。
In above-mentioned technical proposal, it is preferable that metal salt is 1~2:1 with organic ligand molar ratio.
In order to solve the above problem three, The technical solution adopted by the invention is as follows: MIL-100 (Fe) material is used for benzene homologues
Adsorption.
Compared with prior art, the present invention MIL-100 (Fe) the adsorbent material specific surface area containing meso-hole structure provided
Greatly, porosity is high, stability is good, benzene homologues adsorption capacity and the rate of adsorption with higher.In addition, such MOFs adsorbent material
Preparation method be simple and convenient to operate, low in raw material price.Mesoporous MIL-100 (Fe) adsorbent material provided by the invention is in ring
It has broad application prospects in terms of the improvement of benzene homologues VOCs in border, achieves preferable technical effect.
The present invention will be further described below by way of examples, but is not limited only to the present embodiment.
Specific embodiment
Embodiment 1
By metal salt Fe (NO3)3·9H2O (5.0mmol, 2.05g), organic ligand Trimesic acid (5.0mmol,
1.05g), it is added in the reaction flask for filling 5mL n,N-Dimethylformamide, stirs evenly at room temperature.It is anti-by what is be uniformly mixed
It answers liquid to move in heavy wall pressure resistance reaction flask, 12h is heated at 100 DEG C with the mixing speed of 300rpm.It is cooled to room temperature, filters,
Obtained solid uses DMF, ethanol washing respectively, and is heated to reflux for 24 hours twice with chloroform solvent.By solid in drying box in 120 DEG C
At a temperature of, heat-activated 12h is up to final products.Measuring its Langmuir specific surface area using physical adsorption appearance is 1846m2/
G, mesoporous pore size 2.7nm.
MIL-100 (Fe) the material benzene homologues absorption property obtained to the present embodiment is evaluated, and intelligent weight point is utilized
Analyzer (IGA-003) uses gravimetric method to measure the material to the saturated extent of adsorption of toluene as 600mg/g.
Embodiment 2
By metal salt Fe (NO3)3·9H2O (7.5mmol, 3.05g), organic ligand Trimesic acid (5.0mmol,
1.05g), it is added in the reaction flask for filling 5mL n,N-Dimethylformamide, stirs evenly at room temperature.It is anti-by what is be uniformly mixed
It answers liquid to move in heavy wall pressure resistance reaction flask, 16h is heated at 110 DEG C with the mixing speed of 350rpm.It is cooled to room temperature, filters,
Obtained solid uses DMF, ethanol washing respectively, and is heated to reflux for 24 hours twice with chloroform solvent.By solid in drying box in 130 DEG C
At a temperature of, heat-activated 14h is up to final products.Measuring its Langmuir specific surface area using physical adsorption appearance is 2109m2/
G, mesoporous pore size 2.6nm.
MIL-100 (Fe) the material benzene homologues absorption property obtained to the present embodiment is evaluated, and intelligent weight point is utilized
Analyzer (IGA-003) uses gravimetric method to measure the material to the saturated extent of adsorption of toluene as 612mg/g.
Embodiment 3
By metal salt Fe (NO3)3·9H2O (5.0mmol, 2.05g), organic ligand Trimesic acid (5.0mmol,
1.05g), template cetyl trimethylammonium bromide (0.5mmol, 180mg) is added to and fills 5mL N, N- dimethylacetamide
In the reaction flask of amine, stir evenly at room temperature.Uniformly mixed reaction solution is moved in heavy wall pressure resistance reaction flask, with 400rpm's
Mixing speed heats 20h at 120 DEG C.It is cooled to room temperature, filters, obtained solid uses DMF, ethanol washing respectively, and uses chloroform
Solvent is heated to reflux for 24 hours twice.By solid at a temperature of drying box is in 140 DEG C, heat-activated 16h is up to final products.It utilizes
It is 2297m that physical adsorption appearance, which measures its Langmuir specific surface area,2/ g, mesoporous pore size 2.8nm.
MIL-100 (Fe) the material benzene homologues absorption property obtained to the present embodiment is evaluated, and intelligent weight point is utilized
Analyzer (IGA-003) uses gravimetric method to measure the material to the saturated extent of adsorption of toluene as 680mg/g.
Embodiment 4
By metal salt Fe (NO3)3·9H2O (5.0mmol, 2.05g), organic ligand Trimesic acid (5.0mmol,
1.05g), template cetyl trimethylammonium bromide (0.5mmol, 180mg), 1,3,5- trimethylbenzenes (0.25mmol, 45mg),
It is added in the reaction flask for filling 5mL n,N-Dimethylformamide, stirs evenly at room temperature.Uniformly mixed reaction solution is moved
Into heavy wall pressure resistance reaction flask, heated for 24 hours at 130 DEG C with the mixing speed of 350rpm.It is cooled to room temperature, filters, gained is solid
Body uses DMF, ethanol washing respectively, and is heated to reflux for 24 hours twice with chloroform solvent.By solid at a temperature of drying box is in 150 DEG C,
Heat-activated 18h is up to final products.Measuring its Langmuir specific surface area using physical adsorption appearance is 1604m2/ g, mesoporous hole
Diameter 3.1nm.
MIL-100 (Fe) the material benzene homologues absorption property obtained to the present embodiment is evaluated, and intelligent weight point is utilized
Analyzer (IGA-003) uses gravimetric method to measure the material to the saturated extent of adsorption of toluene as 632mg/g.
Embodiment 5
By metal salt Fe (NO3)3·9H2O (7.5mmol, 3.03g), organic ligand Trimesic acid (5.0mmol,
1.05g), cetyl trimethylammonium bromide (1.0mmol, 3.64mg), 1,3,5- trimethylbenzenes (0.38mmol, 45mg) are added
Into the reaction flask for filling 8mL n,N-Dimethylformamide, stir evenly at room temperature.Uniformly mixed reaction solution is moved into thickness
In wall pressure resistance reaction flask, 20h is heated at 140 DEG C with the mixing speed of 450rpm.It is cooled to room temperature, filters, obtained solid point
Not Yong DMF, ethanol washing, and be heated to reflux for 24 hours twice with chloroform solvent.By solid at a temperature of drying box is in 140 DEG C, heating
20h is activated up to final products.Measuring its Langmuir specific surface area using physical adsorption appearance is 1683m2/ g, mesoporous pore size
5.8nm。
MIL-100 (Fe) the material benzene homologues absorption property obtained to the present embodiment is evaluated, and intelligent weight point is utilized
Analyzer (IGA-003) uses gravimetric method to measure the material to the saturated extent of adsorption of toluene as 706mg/g.
Embodiment 6
By metal salt Fe (NO3)3·9H2O (10.0mmol, 4.10g), organic ligand Trimesic acid (5.0mmol,
1.05g), cetyl trimethylammonium bromide (1.5mmol, 546mg), citric acid (0.5mmol, 100mg), are added to and fill
In the reaction flask of 10mL n,N-dimethylacetamide, stir evenly at room temperature.Uniformly mixed reaction solution is moved into heavy wall pressure resistance
In reaction flask, heated for 24 hours at 150 DEG C with the mixing speed of 500rpm.It is cooled to room temperature, filters, obtained solid is used respectively
DEF, ethanol washing, and be heated to reflux for 24 hours twice with dichloromethane solvent.By solid at a temperature of drying box is in 150 DEG C, heating
Activation is for 24 hours up to final products.Measuring its Langmuir specific surface area using physical adsorption appearance is 1445m2/ g, mesoporous pore size
8.6nm。
MIL-100 (Fe) the material benzene homologues absorption property obtained to the present embodiment is evaluated, and intelligent weight point is utilized
Analyzer (IGA-003) uses gravimetric method to measure the material to the saturated extent of adsorption of toluene as 592mg/g.
Specific surface area, aperture and the benzene homologues absorption property of each embodiment of table 1 synthesis MOFs material
Obviously, MIL-100 (Fe) adsorbent material large specific surface area, the porosity provided by the invention containing meso-hole structure
Height, stability are good, benzene homologues adsorption capacity and the rate of adsorption with higher.In addition, such MIL-100 (Fe) adsorbent material
Preparation method is simple and convenient to operate, low in raw material price.Mesoporous MIL-100 (Fe) adsorbent material provided by the invention is in environment
It has broad application prospects in terms of the improvement of middle benzene homologues VOCs, achieves preferable technical effect.
Claims (10)
1. a kind of MIL-100 (Fe) material, the specific surface area of MIL-100 (Fe) material is 1500-2500m2/ g, mesoporous hole
Diameter is 2.6-20nm.
2. MIL-100 (Fe) material according to claim 1, it is characterised in that the mesoporous hole of MIL-100 (Fe) material
Diameter is 2.6-10nm.
3. MIL-100 (Fe) material according to claim 1, it is characterised in that the mesoporous hole of MIL-100 (Fe) material
Diameter is 2.7-9nm.
4. the preparation method of MIL-100 described in claim 1 (Fe) material, includes the following steps:
(1) raw material mixes: weighing metal salt, organic ligand, template, expanding agent by required molar ratio, is added separately to fill
In the reaction vessel of reaction dissolvent, stir evenly；
(2) heating reaction: uniformly mixed reaction solution is moved in pressure-resistant reaction vessel, and heating stirring is reacted in oil bath pan；
(3) it removes removing template: stopping heating, be cooled to room temperature, filter；Obtained solid is washed with solvent, and low boiling point solvent is added and adds
Heat reflux；
(4) it activates: it is cooling to filter, by solid heat-activated to get MIL-100 (Fe) material；
Wherein, in step (1), the metal salt is Fe (NO3)3·9H2O、FeCl3·6H2One of O；The organic ligand
For Trimesic acid or 1,3,5- benzenetricarboxylic acid trimethyl；The template is cetyl trimethylammonium bromide or dodecyl
Phosphate；The expanding agent is 1,3,5- trimethylbenzene or citric acid；Metal salt and organic ligand molar ratio are 1~3:1；It is organic
Ligand, template and expanding agent molar ratio are 1:0.1~0.3:0.05~0.1；Reaction dissolvent is N,N-dimethylformamide
Or N, N- diethylformamide.
5. the preparation method of MIL-100 (Fe) material according to claim 4, it is characterised in that in step (1), the metal
Salt is Fe (NO3)3·9H2O, the organic ligand are Trimesic acid, and the template is cetyl trimethylammonium bromide,
The expanding agent is 1,3,5- trimethylbenzene；It is characterized in that the oil bath pan stirring rate is 200-800rpm in step (2),
Heating temperature is 60-150 DEG C, heating time 6-48h.
6. the preparation method of MIL-100 (Fe) material according to claim 5, it is characterised in that in step (2), the oil bath
Pot stirring rate is 300-500rpm, and heating temperature is 100-150 DEG C, heating time 12-24h.
7. the preparation method of MIL-100 (Fe) material according to claim 4, it is characterised in that in step (3), the washing
Solvent includes ethyl alcohol, N, N- diethylformamide or N,N-dimethylformamide；Low boiling point solvent is ethyl alcohol, methylene chloride, chlorine
At least one of imitate；In step (4), heating temperature is 80-150 DEG C, activation time 2-48h.
8. the preparation method of MIL-100 (Fe) material according to claim 7, it is characterised in that in step (4), heating temperature
It is 120-150 DEG C, activation time 12-24h.
9. the preparation method of MIL-100 (Fe) material according to claim 4, it is characterised in that metal salt rubs with organic ligand
Your ratio is 1~2:1.
MIL-100 described in claim 1 10. (Fe) material, the Adsorption for benzene homologues.
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| CN113150689A (en) * | 2021-05-31 | 2021-07-23 | 上海交通大学 | Anti-condensation coating and preparation method and application thereof |
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| 马宸等: ""金属有机骨架材料MIL-100(Fe)的合成及其对甲苯的吸附/脱附性能"", 《热烈庆祝中国化学会成立80周年—中国化学会第16届反应性高分子学术研讨会论文集》 * |
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| CN113150689A (en) * | 2021-05-31 | 2021-07-23 | 上海交通大学 | Anti-condensation coating and preparation method and application thereof |
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