CN110404509A - A kind of preparation method of the ILs@ZIF composite material of class with multi-layer structure " nanometer rectifying column " - Google Patents

A kind of preparation method of the ILs@ZIF composite material of class with multi-layer structure " nanometer rectifying column " Download PDF

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CN110404509A
CN110404509A CN201910518731.8A CN201910518731A CN110404509A CN 110404509 A CN110404509 A CN 110404509A CN 201910518731 A CN201910518731 A CN 201910518731A CN 110404509 A CN110404509 A CN 110404509A
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rectifying column
composite material
zif
class
nanometer
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CN110404509B (en
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刘大欢
韩国鹏
仲崇立
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Beijing University of Chemical Technology
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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
    • 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
    • B01D53/14—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 absorption
    • B01D53/1456—Removing acid components
    • B01D53/1475—Removing carbon dioxide
    • 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
    • B01D53/14—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 absorption
    • B01D53/1493—Selection of liquid materials for use as absorbents
    • 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]
    • 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
    • B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28014—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 form
    • B01J20/28033—Membrane, sheet, cloth, pad, lamellar or mat
    • B01J20/28035—Membrane, sheet, cloth, pad, lamellar or mat with more than one layer, e.g. laminates, separated sheets
    • 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
    • B01J20/30—Processes for preparing, regenerating, or reactivating
    • B01J20/3085—Chemical treatments not covered by groups B01J20/3007 - B01J20/3078
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2252/00—Absorbents, i.e. solvents and liquid materials for gas absorption
    • B01D2252/30—Ionic liquids and zwitter-ions
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2253/00—Adsorbents used in seperation treatment of gases and vapours
    • B01D2253/20—Organic adsorbents
    • B01D2253/204—Metal organic frameworks (MOF's)
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    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
    • Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
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    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02C—CAPTURE, STORAGE, SEQUESTRATION OR DISPOSAL OF GREENHOUSE GASES [GHG]
    • Y02C20/00—Capture or disposal of greenhouse gases
    • Y02C20/40—Capture or disposal of greenhouse gases of CO2

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Abstract

A kind of preparation method of class " nanometer rectifying column " composite material IL (a)-ZIF-IL (b) based on ILs@ZIF multilayered structure, belongs to new material technology field.The material passes through specific synthetic method by two different ionic liquids and ZIF-8, form a type " nanometer rectifying column " layer composite material, gas molecule experienced the multiple adsorbing separation similar to principles of rectification during mass transfer, realize CO2And N2Multistage gradually separate, the results showed that CO2/N2There is highest selectivity at normal temperatures and pressures.Guaranteeing considerable CO2Under the premise of adsorbance (40 cc/g), separation selectivity has been more than other conventional porous materials in CO2Separate the performance of aspect.The specific synthetic method of the material has stronger novelty, after successfully synthesizing, has best separating property by experiment test.Because such " nanometer rectifying column " composite material has important industrial application value in gas use aspects, while class " nanometer rectifying column " composite material also has important reference significance in terms of new material design and synthesis.

Description

A kind of ILs@ZIF composite material of class with multi-layer structure " nanometer rectifying column " Preparation method
Technical field
The invention belongs to new material technology field, provide that a kind of based on ILs@ZIF to construct class " nanometer rectifying column " compound The preparation method of material (IL (a)-ZIF-IL (b)).
Background technique
In recent years, the carbon dioxide (CO in air2) in constantly incremental trend, earth average surface temperature also therewith by Year is incremented by, and greenhouse effects increasingly sharpen, and a series of environmental problems thus caused causes the extensive concern of people.In order to Realize CO2Energy-saving and emission-reduction, research and develop it is a kind of clean effective adsorbent material have to the sustainable development of future society it is far-reaching Meaning.
Currently, common CO in factory2The advantages of capture method is mainly to rely on lye to absorb, this method is processing Ability is strong, high-efficient.But this method is to the serious corrosion of equipment, and regenerability is poor, gas recycles difficulty etc. A series of problems is limited to CO in air2A large amount of trappings.Therefore we are badly in need of developing a kind of effective adsorbent of cleaning For CO in industry2Trapping.Adsorbent based on novel porous solid material has adsorbance in terms of gas separation The advantages that height, selectivity is high, does not have corrosivity to equipment, and regenerability is good, simple to operate, causes scientific worker's Research interest.As zeolite, carbon nanotube, active carbon, lignin, metal-organic framework (MOFs) material, covalently-organic frame (COFs) material etc. has a potentiality of gas absorption separation, especially MOFs material, by inorganic metal ion or metal cluster with Organic ligand is by being self-assembly of, and with high specific surface area and porosity, duct height adjustability, stable structure is convenient Synthesis, therefore stored in gas, adsorbing separation, chemical sensitisation, catalysis, the absorption of heavy metal ions in wastewater or organic dyestuff, The fields such as the sustained release of drug have potential application prospect.
However most of MOFs materials are to CO2Adsorbance or selectivity be not all it is very high, after amino modified MOFs material often can significantly promote adsorbance and selectivity, conventional method of modifying is amido grafting or amine dipping, This method can also face CO2The problem of induction inactivation or thermodynamic stability.Ionic liquid (ILs), by organic cation and Anion composition in room temperature or the salt being in a liquid state lower than 373 K, non-volatile, nonhazardous, referred to as green solvent, in CO2 Trapping aspect has wide application potential, and the ionic liquid of functional amido is to CO2It can achieve equimolar absorption.However Often viscosity is larger by the ILs of functionalization, seriously affects the mass transfer velocity of gas.If ILs loaded in MOFs material, formed ILs in nanometer confinement improves the adsorbance and selectivity of MOFs material, and solves the mass transfer problem of ILs.We are based on two kinds It is compound to have synthesized a type " nanometer rectifying column " multilayered structure by specific synthetic method for different ionic liquids and ZIF-8 Material, gas molecule experienced the multiple adsorbing separation similar to principles of rectification during mass transfer, realize CO2And N2's Multistage gradually separates, the results showed that CO2 /N2There is highest separation selectivity at normal temperatures and pressures.It is specific due to the material Synthetic method has stronger novelty, and finds it with best separating property by experiment test.Because of such " nanometer Rectifying column " composite material has important industrial application value, while class " nanometer rectifying column " composite wood in gas use aspects Material also has important reference significance in terms of new material design and synthesis.
Summary of the invention
The object of the present invention is to provide a kind of preparation methods for preparing class " nanometer rectifying column " composite material.We are with zeolite Imidazole skeleton material (ZIF-8) is used as skeleton, loads two different ILs, structure respectively inside and outside this caged skeleton Build multilayered structure.Every layer of structure is to CO2Have the function of that adsorbing separation, the process of the layer-by-layer mass transfer of gas ecto-entad are similar to The process of each column plate separated step by step in rectifying column, therefore the compound constituted can regard class " nanometer rectifying column " as, lead to It crosses and constructs class " nanometer rectifying column " Lai Shixian CO2The multi-stage separation of gas, has reached S at normal temperatures and pressuresCO2/N2=73148 choosing Selecting property (IAST).
1, class " nanometer rectifying column " of the present invention, specific synthetic method is as follows:
(1) a certain amount of ionic liquid [TETA] L is weighed in beaker, the anhydrous methanol of 5-30 ml is added, until being completely dissolved Afterwards, then activated a certain amount of ZIF-8 powder is added in the beaker, is stirred at room temperature dry to solvent volatilization Only.The product of acquisition is put into vacuum drying oven, drying in several hours is carried out under hot conditions.
(2) obtained solid powder is washed for several times with anhydrous n,N-Dimethylformamide (DMF), until filtrate after centrifugation Noresidue substance after being evaporated completely under elevated temperature in vacuo.By the solid matter obtained after centrifugation be put into high-temperature vacuum baking oven into Row drying in several hours.
(3) a certain amount of ionic liquid [TEPA] [FV] is weighed in certain specification centrifuge tube, and it is anhydrous that 1-10 ml is added The product obtained in (2) is added thereto by DMF until ILs is completely dissolved, and is sufficiently mixed uniformly, after several hours, will be obtained Product be put into high-temperature vacuum baking oven and carry out drying in several hours, obtain target product.
2, the load form with when ectonexine for changing two kinds of ILs and ZIF-8 prepares various forms of classes " nanometer essence Evaporate tower ".
3, in first step loading process use water, methanol, ethyl alcohol, acetone etc. difference solvent flashing ILs is loaded.
4, solvent is removed using forms such as different heating, vacuums in loading process.
5, it is combined using the other materials of different amido ILs and ZIF series, the composite material being variously formulated.
Class " nanometer rectifying column " of the present invention is used for CO2Capture, including Batch Adsorption method and ADSORPTION IN A FIXED BED method two Kind.
Class " nanometer rectifying column " material interval absorption method separates CO2Method it is as follows:
(1) start physical adsorption appearance, white group " nanometer rectifying column " composite powder after grinding is added to after being precisely weighed In sample cell, it is de-gassed.
(2) sample after deaerating weighs obtain the dry weight of gross weight and sample again, and is placed on adsorption instrument test position.
(3) the relevant test parameter of setting adsorption instrument, opens test.
(4) material is obtained at 298 K to CO2, N2Adsorption isotherm.
(5) by analysis, we can achieve the separating property data of material, and be evaluated.
Compared with prior art, present invention has the advantage that
One, the experimental data of Batch Adsorption method shows that material is at 298 K with class " nanometer rectifying column ", to CO2/N2Point From selectivity up to 73148, considerably beyond traditional sorbent material, achieve the effect that molecule sieves.
Two, the experiment of Batch Adsorption method shows that the composite material with class " nanometer rectifying column " structure can efficiently divide in 298 K Separate out CO2/N2。
Three, composite material and preparation method thereof of the present invention simply can be synthesized in high volume, and synthesis material is cheap, can To be widely used in CO in industry2Absorption and separation.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of class " nanometer rectifying column " composite material.
Fig. 2 is the pictorial diagram of class " nanometer rectifying column " composite material.
Fig. 3 is polycrystal X ray diffraction (PXRD) phenogram of class " nanometer rectifying column " composite material.
Fig. 4 is class " nanometer rectifying column " composite material to CO2/N2Isolated adsorbance with pressure variation relation figure.
Fig. 5 is class " nanometer rectifying column " composite material to CO2/N2Isolated selectivity with pressure variation relation figure.
Specific embodiment
Below by specific example, the present invention will be further described, but the present invention is not limited thereto.
Experimental method is tried described in following embodiments, is conventional method unless otherwise specified；The reagent and material, Unless otherwise specified, it commercially obtains.
Embodiment 1
(1) 0.4 g ionic liquid [TETA] L is weighed in beaker, and the anhydrous methanol of 20 ml is added, until after being completely dissolved, so Activated 0.6 g ZIF-8 powder is added in the beaker afterwards, is stirred at room temperature clean to solvent volatilization.It will obtain Product be put into vacuum drying oven, drying in 12 hours is carried out under the conditions of 350 K.
(2) obtained solid powder is washed for several times with anhydrous n,N-Dimethylformamide (DMF), until filtrate after centrifugation Noresidue substance after being evaporated completely under elevated temperature in vacuo.The vacuum that the solid matter obtained after centrifugation is put into 350 K is dried Case carries out drying in 12 hours.
(3) 0.25 g ionic liquid [TEPA] [FV] is weighed in 10 ml centrifuge tubes, and 3 ml anhydrous DMFs are added, until ILs is completely dissolved, and the product obtained in (2) is added thereto, and is sufficiently mixed uniformly, after 4 hours, the product of acquisition is put into The vacuum drying oven of 350 K carries out drying in 12 hours, obtains target product.
Embodiment 2
(1) 0.4 g ionic liquid [TEPA] [FV] is weighed in beaker, the anhydrous methanol of 20 ml is added, until being completely dissolved.3 g Zn(NO3)2·6H2The methanol solution of O is added, and stirs evenly.The methanol solution of the 2-methylimidazole of 6.6 g is added, room temperature Under be sufficiently stirred 2 hours, be centrifuged, vacuum drying, obtain the ZIF-8 of white powder.
(2) obtained solid powder is washed for several times with anhydrous n,N-Dimethylformamide (DMF), until filtrate after centrifugation Noresidue substance after being evaporated completely under elevated temperature in vacuo.The vacuum that the solid matter obtained after centrifugation is put into 350 K is dried Case carries out drying in 12 hours.
(3) 0.25 g ionic liquid [TETA] L is weighed in 10 ml centrifuge tubes, 3 ml anhydrous DMFs are added, until ILs It is completely dissolved, the product obtained in (2) is added thereto, be sufficiently mixed uniformly, after 4 hours, the product of acquisition is put into 350 The vacuum drying oven of K carries out drying in 12 hours, obtains target product.
Embodiment 3
(1) 0.4 g ionic liquid [TETA] L is weighed in beaker, and the deionized water of 20 ml is added, until after being completely dissolved, so Activated 0.6 g ZIF-8 powder is added in the beaker afterwards, is stirred at room temperature clean to solvent volatilization.It will obtain Product be put into vacuum drying oven, drying in 12 hours is carried out under the conditions of 350 K.
(2) obtained solid powder is washed for several times with anhydrous n,N-dimethylacetamide (DMA), until filtrate after centrifugation Noresidue substance after being evaporated completely under elevated temperature in vacuo.The vacuum that the solid matter obtained after centrifugation is put into 350 K is dried Case carries out drying in 12 hours.
(3) 0.25 g ionic liquid [TEPA] [FV] is weighed in 10 ml centrifuge tubes, and 3 ml anhydrous DMFs are added, until ILs is completely dissolved, and the product obtained in (2) is added thereto, and is sufficiently mixed uniformly, after 4 hours, the product of acquisition is put into The vacuum drying oven of 350 K carries out drying in 12 hours, obtains target product.

Claims (4)

1. a kind of preparation of the class for the multilayered structure being made of two different ILs and ZIF-8 " nanometer rectifying column " composite material Method and its in CO2Related application in capture, the functionalization material are class " nanometer rectifying column " composite material IL (a)- ZIF-IL (b) is used for CO2/CH4/N2/H2 Efficiently separate.
2. content described in accordance with the claim 1, which is characterized in that prepared material is class " nanometer rectifying column " composite material IL (a)-ZIF-IL (b), the multilayered structure being made of two different ILs and the ZIF-8 with cage pore structure.
3. purposes described in accordance with the claim 1, which is characterized in that its separation method includes that Batch Adsorption separation and fixed bed connect Continuous adsorbing separation.
4. purposes described in accordance with the claim 1, which is characterized in that separated object includes CO2, CH4, N2, H2Deng mixing Gas.
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