CN108751189A - The preparation and application of the aluminium base MOF porous carbon materials of high-specific surface area - Google Patents
The preparation and application of the aluminium base MOF porous carbon materials of high-specific surface area Download PDFInfo
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- CN108751189A CN108751189A CN201810776968.1A CN201810776968A CN108751189A CN 108751189 A CN108751189 A CN 108751189A CN 201810776968 A CN201810776968 A CN 201810776968A CN 108751189 A CN108751189 A CN 108751189A
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- C01B32/00—Carbon; Compounds thereof
- C01B32/30—Active carbon
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- C01B32/318—Preparation characterised by the starting materials
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- B—PERFORMING OPERATIONS; TRANSPORTING
- 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
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
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- C—CHEMISTRY; METALLURGY
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- C01B32/00—Carbon; Compounds thereof
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- C01B32/342—Preparation characterised by non-gaseous activating agents
- C01B32/348—Metallic compounds
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B01D2257/708—Volatile organic compounds V.O.C.'s
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- Y02A50/20—Air quality improvement or preservation, e.g. vehicle emission control or emission reduction by using catalytic converters
Abstract
The present invention provides a kind of preparation and application of the aluminium base MOF porous carbon materials of high-specific surface area, and the method comprises the following steps：MIL-100 (Al) materials and Additional carbon sources are scattered in ethyl alcohol, then temperature programming makes carbon source polymerize in aluminium base MOF materials, then high temperature cabonization；Carbonized product is mixed with activator, after heating activation, pickling, washing, vacuum drying can obtain the aluminium base MOF porous carbon materials of high-specific surface area, in terms of which can be used for gas absorption separation.This method preparation process is simple, and product has higher specific surface area and abundant duct, and has higher adsorption capacity to toluene.
Description
Technical field
The invention belongs to the preparation fields of porous carbon materials, and in particular to a kind of aluminium base MOF porous carbons of high-specific surface area
The preparation and application of material.
Background technology
Important presoma of the volatile organic matter (VOCs) as ozone and PM2.5, is that China's current zone is compound
One of significant contributor of air pollution, State Ministry of Environmental Protection have been classified as maximum air pollution member except fine particle
It is fierce.In recent years, with the quickening of China's rapid development of economy and process of industrialization, the discharge capacity of VOCs increases with surprising rapidity
It is long.There is these VOCs majorities toxicity and irritation, Long Term Contact can damage human nerve maincenter and immune system, and part is even
Also there is genotoxicity and carcinogenicity, can be seriously threatened to life zone.Meanwhile VOCs is under the excitation of ultraviolet light, can with it is big
Photochemical reaction occurs for the nitrogen oxides in gas, forms the photochemical fog of toxicity bigger.Calculate according to associated mechanisms, to 2020
Year, it is contemplated that accumulative up to 4,300,000 tons of the emission reduction demand of industrial source key industry VOCs, therefore it is very urgent to reinforce VOCs improvement.
Currently, VOCs Recovery Purifyings technology mainly has absorption process, condensation method, membrane separation process and absorption method etc. both at home and abroad.Wherein, absorption method
Due to the advantages that technological process is relatively easy and the VOCs rate of recovery is high, it is considered to be a kind of extremely potential VOCs is purified back
Receipts technology, the technology are widely used in terms of the Recovery Purifying of VOCs.
Adsorbent is the core of adsorption recovery technology.In many porous materials, porous carbon materials are because it is with high surface
Product and high porosity, while also having the characteristics that physical and chemical stability and mechanical stability, it is widely used in each research field,
Especially gas absorption and separation field.Currently, the preparation method of porous carbon materials mainly has soft template method and hard template method.Firmly
Template is by carbon source presoma by being either physically or chemically filled into the hole of hard template, by carbonization, is finally removed
Hard template can get the porous carbon materials with specified pore structure, but this method preparation process is complicated, time-consuming.Soft template method is
Using template and forerunner's precursor reactant, porous carbon materials are formed by a series of polymerization, carbonization, self assembly etc..Soft template method
It can be in order to avoid remove template, but available template is seldom at present, so its application is restricted.
In recent years, with metal-organic framework porous material (Metal-organic frameworks, MOFs) for precursor
The research that porous carbon materials are prepared with template is widely paid close attention to.Due to MOFs have huge specific surface area, high porosity,
The features such as structure diversity, becomes precursor and the ideal chose of template.(Jiang H.L., the et al.From such as Jiang
metal–organic framework to nanoporous carbon:toward a very high surface area
and hydrogen uptake.Journal of the American Chemical Society,2011,133,11854)
For the first time using ZIF-8 as predecessor and template, furancarbinol is introduced into ZIF-8 carbonizations, the ratio of prepared porous carbon materials
Surface area is up to 3405m2/ g, the material is under conditions of 77K and 1bar to H2Adsorbance is up to 2.77wt%.Wang seminars
(Wang Q.,et al.Functional zeolitic-imidazolate-framework-templated porous
carbon materials for CO2capture and enhanced capacitors.Chemistry,an Asian
Journal,2013,8:1879) 3 kinds of ZIFs materials (ZIF-8, ZIF-68, ZIF-69) of direct carbonization, activate through KOH, obtain 3
Kind porous carbon materials, wherein NPC8 shows highest hydrogen adsorption ability (2.59%, 77K and 1bar), and NPC69 is shown
Highest CO2Adsorption capacity (4.76mmol/g, 273K and 1bar).These are studies have shown that MOF bases porous carbon materials are inhaled in gas
Fufen has good application prospect from aspect.(Wang J., the et al.A versatile synthesis of such as Wang
metal–organic framework derived porous carbons for CO2capture and gas
Separation.Journal of Materials Chemistry A, 2016,4,19095-1910) direct carbonization MIL-100
(Al), MIL-100 (Al)/F127 compounds, MIL-100 (Al)/KOH mixtures etc. are prepared for a series of porous carbon materials,
And prepared porous carbon materials BET specific surface area highest only has 1097m2/g.Therefore, MIL- of the research with high-specific surface area
100 (Al) base porous carbon materials there is important science to grind the VOCs pollutions of improvement getting worse and Brownish haze phenomenon
Study carefully value and urgent social demand.
Invention content
The separation of VOCs gas absorptions is can be applied to the purpose of the present invention is to provide one kind and obtained material is with abundant
Micropore and the hierarchical porous structures such as mesoporous, and the aluminium base MOF of the high-specific surface area with good gas absorption performance is porous
The preparation and application of carbon material.
In order to realize that above-mentioned technical purpose, the technical solution adopted by the present invention be：
A kind of preparation method of the aluminium base MOF porous carbon materials of high-specific surface area comprising following steps：
(1) aluminium base MOF materials and Additional carbon sources are scattered in ethyl alcohol, then by mixed system heating treatment, are made additional
Carbon source polymerize in aluminium base MOF materials, and then again after carbonization treatment, carbonized product is made；
(2) carbonized product made from step (1) is mixed with activator, after then carrying out heating activation process again, is made
Activation products；
(3) by activation products made from step (2) sequentially after overpickling, washing and vacuum drying treatment, you can be made
The aluminium base MOF porous carbon materials of high specific area.
Further, the aluminium base MOF materials described in step (1) are MIL-100 (Al).
Preferably, the Additional carbon sources described in step (1) are glucose or sucrose.
Preferably, in step (1) aluminium base MOF materials and Additional carbon sources mass mixing ratio 1：0.5~2.5.
Further, mixed system is warming up to 50~60 DEG C of 1~3h of maintenance in step (1), is then warming up to 80~100 again
DEG C maintain 3~5h, be then warming up to again 150~170 DEG C maintenance 5~7h；Carbon is finally carried out with 600~800 DEG C of temperature condition
Change 2~5h of processing.
Preferably, nitrogen is continually fed into as protective gas during carbonization treatment.
Preferably, after maintaining 5~7h at 150~170 DEG C, in the case where being continually fed into nitrogen with 5~10 DEG C/min's
Heating rate is warming up to 600~800 DEG C.
Further, the activator in step (2) is potassium hydroxide or zinc chloride, the ratio of carbonized product and activator mixing
It is 1：1~7, and the activation that heats up is to be warming up to 600~900 DEG C of 1~3h of maintenance under nitrogen protection with 5 DEG C/min.
Further, the pickling in step (3) is with the salt acid elution of concentration 1mol/L；The temperature of vacuum drying treatment is
120~150 DEG C, drying time is 8~12h.
According to the application of the aluminium base MOF porous carbon materials of high-specific surface area made from above-mentioned preparation method, by height obtained
The adsorbing separation that the aluminium base MOF porous carbon materials of specific surface area are applied to VOCs gases purifies.
Using above-mentioned technical solution, the device have the advantages that being：
(1) present invention is using green cheap carbon source such as glucose or sucrose, you can the aluminium base MOF of synthesizing high specific surface area
Porous carbon materials；
(2) the aluminium base MOF porous carbon materials prepared by the present invention, while there is abundant micropore and central hole structure, micropore pair
Adsorbate has strong adsorption, is conducive to the absorption of adsorbate, and mesoporous is conducive to the diffusion of adsorbate；
(3) use aluminium base MOF porous carbon materials prepared by the method for the invention that there is height to volatile organic matter toluene
Adsorption capacity, adsorption capacity can reach 11.7mmolg-1, it is far above original MIL-100 (Al) material.
Description of the drawings
The present invention is further elaborated with reference to the accompanying drawings and detailed description：
The aluminium base MOF for the high-specific surface area that Fig. 1 is MIL-100 (Al) prepared by the embodiment of the present invention 1 and prepared by embodiment 2
The N of porous carbon materials2Adsorption/desorption isotherms.
The aluminium base MOF for the high-specific surface area that Fig. 2 is MIL-100 (Al) prepared by the embodiment of the present invention 1 and prepared by embodiment 2
Adsorption isotherm of the porous carbon materials to toluene.
Specific implementation mode
Embodiment 1
The preparation method of the aluminium base MOF porous carbon materials of high-specific surface area of the present invention is equal to all aluminium base MOF materials
There is effect.For ease of the effect of the synthetic method of the aluminium base MOF porous carbon materials of comparative illustration high-specific surface area of the present invention,
The present embodiment 1 provides a kind of method of MIL-100 (Al) material prepared according to conventional method, and specific preparation method is as follows：
By 3.75g Al (NO3)3.9H2O and 1.68g trimesic acids (H3BTC it) is dissolved in 50mL deionized waters, room temperature is stirred
It mixes and is slowly added dropwise 0.5mLDMF, then with nitre acid for adjusting pH be 1.7, continue stirring 15 minutes, be then placed in air dry oven,
200 DEG C of reaction 6h, by reaction product sequentially through centrifugation, ethyl alcohol washes, and the dry 8h of 150 DEG C of vacuum is to get to MIL-100 (Al) material
Material.
Embodiment 2
A kind of preparation method of the aluminium base MOF porous carbon materials of high-specific surface area, includes the following steps：
0.5g MIL-100 (Al) materials and 0.5g sucrose carbon sources are scattered in 2mL ethyl alcohol, continues to stir evenly, then put
Enter with 60 DEG C of maintenance 2h in air dry oven, then again with 100 DEG C of maintenance 4h, then again with 160 DEG C of maintenance 6h；It finally will mixing
Object is put into tube furnace, is warming up to 700 DEG C under nitrogen protection with 5 DEG C/min, maintains to cool after 3h；
KOH (carbonized samples/KOH=1 are added in sample after being carbonized:3) it, is put into tube furnace after mixing, is protected in nitrogen
800 DEG C of maintenance 1h are warming up to 5 DEG C/min under shield, are then cooled；Salt pickling, the washing of 1mol/L are used later, finally again
The dry 8h of 150 DEG C of vacuum is to get to the aluminium base MOF porous carbon materials of high-specific surface area.
Embodiment 3
A kind of preparation method of the aluminium base MOF porous carbon materials of high-specific surface area, includes the following steps：
0.5g MIL-100 (Al) materials and 0.5g glucose carbon sources are scattered in 2mL ethyl alcohol, continue to stir evenly, then
It is put into air dry oven with 50 DEG C of maintenance 3h, then again with 90 DEG C of maintenance 7h, then again with 150 DEG C of maintenance 6h；It will finally mix
It closes object and is put into tube furnace, be warming up to 800 DEG C under nitrogen protection with 5 DEG C/min, maintain to cool after 5h；
ZnCl is added in sample after being carbonized2(carbonized samples/ZnCl2=1:4) it, is put into tube furnace after mixing, in nitrogen
800 DEG C of maintenance 1h are warming up to 5 DEG C/min under protection, are cooled；Salt pickling, the washing of 1mol/L are used later, it is finally true again
150 DEG C of dry 8h of sky are to get to the aluminium base MOF porous carbon materials of high-specific surface area.
Embodiment 4
A kind of preparation method of the aluminium base MOF porous carbon materials of high-specific surface area, includes the following steps：
0.5g MIL-100 (Al) materials and 1.0g sucrose carbon sources are scattered in 2mL ethyl alcohol, continues to stir evenly, then put
Enter with 50 DEG C of maintenance 3h in air dry oven, then again with 100 DEG C of maintenance 6h, then again with 160 DEG C of maintenance 6h；It finally will mixing
Object is put into tube furnace, is warming up to 700 DEG C under nitrogen protection with 5 DEG C/min, maintains to cool after 6h；
KOH (carbonized samples/KOH=1 are added in sample after being carbonized:5) it, is put into tube furnace after mixing, is protected in nitrogen
700 DEG C of maintenance 3h are warming up to 5 DEG C/min under shield, are cooled；Salt pickling, the washing of 1mol/L are used later, finally vacuum again
120 DEG C of dry 10h are to get to the aluminium base MOF porous carbon materials of high-specific surface area.
Embodiment 5
A kind of preparation method of the aluminium base MOF porous carbon materials of high-specific surface area, includes the following steps：
0.5g MIL-100 (Al) materials and 1.25g glucose carbon sources are scattered in 2mL ethyl alcohol, continue to stir evenly, so
After be put into air dry oven with 60 DEG C maintenance 3h, then again with 80 DEG C maintenance 5h, then again with 150 DEG C maintenance 5h；It will finally mix
It closes object and is put into tube furnace, be warming up to 700 DEG C under nitrogen protection with 5 DEG C/min, maintain to cool after 6h；
ZnCl is added in sample after being carbonized2(carbonized samples/ZnCl2=1:5) it, is put into tube furnace after mixing, in nitrogen
700 DEG C of maintenance 3h are warming up to 5 DEG C/min under protection, are cooled；Salt pickling, the washing of 1mol/L are used later, it is finally true again
150 DEG C of dry 10h of sky are to get to the aluminium base MOF porous carbon materials of high-specific surface area.
Performance detection is analyzed
As a control group with MIL-100 (Al) material obtained by embodiment 1, then it is more with the aluminium base MOF of the preparation of embodiment 2
The characterization result of hole carbon material is the effect that representative illustrates the present invention, aluminium base MOF porous carbon materials prepared by other embodiments
Characterization result is not just provided and is repeated one by one substantially with embodiment 2.
(1) specific surface area and pore structure property representation of MIL-100 (Al) and its porous carbon materials：
Adsorption instrument 3Flex is mostly used to embodiment 1 using three station full functions of Micromertics companies of U.S. production
The specific surface area and pore structure of MIL-100 (Al) materials and the aluminium base MOF porous carbon materials of embodiment 2 are characterized, knot
Fruit is as shown in table 1.
The specific surface area and parameter of pore structure of 1 MIL-100 of table (Al) materials and its porous carbon materials
By table 1 it can be seen that the BET specific surface area of original MIL-100 (Al) is 1201.2m2·g-1.And use this hair
Aluminium base MOF porous carbon materials specific surface areas prepared by bright the method are 2567.5m2·g-1, total pore volume is up to 1.35cm3·g-1, Micropore volume is up to 0.81cm3·g-1, mesopore volume is up to 0.54cm3·g-1, illustrate that the aluminium base MOF that embodiment 2 obtains is more
Hole carbon material has large specific surface area and higher porosity, and has middle micro-diplopore skeleton structure.
Fig. 1 is the N of MIL-100 (Al) materials prepared by Examples 1 and 2 and its porous carbon materials2Adsorption/desorption isotherms.
As shown in Figure 1, MIL-100 (Al) material adsorption isotherm belongs to typical I type thermoisopleth, shows the micropore knot for having abundant
Structure.And the adsorption isotherm of aluminium base MOF porous carbon materials is different from MIL-100 (Al) materials, to N under relatively low relative pressure2
Adsorbance drastically increased with the increase of pressure, show the micropore for having abundant, its subsequent adsorbance is with the increase of pressure
Continue to be slowly increased, shows that the material has central hole structure.
(2) absorption property of MIL-100 (Al) and its porous carbon materials to toluene：
Adsorption instrument 3Flex is mostly used using three station full functions of Micromertics companies of U.S. production to measure under 298K in fact
MIL-100 (Al) materials of example 1 and the aluminium base MOF porous carbon materials of embodiment 2 are applied to the adsorption isotherm of toluene.Sample is surveyed
Pretreatment condition before examination is：By sample vacuum drying 12h at 150 DEG C, vacuum degree is 5~10Pa.As a result such as Fig. 2 institutes
Show.
By Fig. 2, it can be seen that, the toluene adsorption curves of the aluminium base MOF porous carbon materials of embodiment 2 is apparently higher than original
MIL-100 (Al) material.It is 11.7mmolg to the adsorbance of toluene in the aluminium base MOF porous carbons of 308K embodiments 2-1, it is former
2.3 times of beginning MIL-100 (Al) material.This shows MIL-100 (Al) base that high-specific surface area is prepared for using the method for the present invention
Porous carbon materials, and excellent absorption property is shown to toluene.
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, it is other it is any without departing from the spirit and principles of the present invention made by changes, modifications, substitutions, combinations, simplifications,
Equivalent substitute mode is should be, is included within the scope of the present invention.
Claims (10)
1. a kind of preparation method of the aluminium base MOF porous carbon materials of high-specific surface area, it is characterised in that：It includes the following steps：
（1）Aluminium base MOF materials and Additional carbon sources are scattered in ethyl alcohol, then by mixed system heating treatment, make Additional carbon sources
It polymerize in aluminium base MOF materials, then again after carbonization treatment, carbonized product is made；
（2）By step（1）Carbonized product obtained is mixed with activator, and after then carrying out heating activation process again, activation is made
Product；
（3）By step（2）Activation products obtained are sequentially after overpickling, washing and vacuum drying treatment, you can high ratio is made
The aluminium base MOF porous carbon materials of area.
2. a kind of preparation method of the aluminium base MOF porous carbon materials of high-specific surface area according to claim 1, feature exist
In：Step（1）Described in aluminium base MOF materials be MIL-100 (Al).
3. a kind of preparation method of the aluminium base MOF porous carbon materials of high-specific surface area according to claim 2, feature exist
In：Step（1）Described in Additional carbon sources be glucose or sucrose.
4. a kind of preparation method of the aluminium base MOF porous carbon materials of high-specific surface area according to claim 3, feature exist
In：Step（1）The mass mixing ratio 1 of middle aluminium base MOF materials and Additional carbon sources：0.5~2.5.
5. a kind of preparation method of the aluminium base MOF porous carbon materials of high-specific surface area according to claim 1, feature
It is：Step（1）It is middle that mixed system is warming up to 50~60 DEG C of 1~3 h of maintenance, it is then warming up to 80~100 DEG C again and maintains 3
~5 h are then warming up to 150~170 DEG C of 5~7 h of maintenance again；Finally carried out at carbonization with 600~800 DEG C of temperature condition
Manage 2~5 h.
6. a kind of preparation method of the aluminium base MOF porous carbon materials of high-specific surface area according to claim 5, feature exist
In：Nitrogen is continually fed into as protective gas during carbonization treatment.
7. a kind of preparation method of the aluminium base MOF porous carbon materials of high-specific surface area according to claim 5, feature
It is：After maintaining 5~7 h at 150~170 DEG C, in the case where being continually fed into nitrogen with the heating rate of 5~10 DEG C/min
It is warming up to 600~800 DEG C.
8. a kind of preparation method of the aluminium base MOF porous carbon materials of high-specific surface area according to claim 1, feature
It is：Step（2）In activator be potassium hydroxide or zinc chloride, the ratio of carbonized product and activator mixing is 1：1~7,
And heating activation is to be warming up to 600~900 DEG C of 1~3 h of maintenance under nitrogen protection with 5 DEG C/min.
9. a kind of preparation method of the aluminium base MOF porous carbon materials of high-specific surface area according to claim 1, feature
It is：Step（3）In pickling be with the salt acid elution of 1 mol/L of concentration；The temperature of vacuum drying treatment is 120~150
DEG C, drying time is 8~12 h.
10. according to the aluminium base MOF porous carbon materials of high-specific surface area made from one of claim 1 to 9 preparation method
Using, it is characterised in that：The aluminium base MOF porous carbon materials of high-specific surface area obtained are applied to the absorption of VOCs gases.
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