CN106311152A - Mesoporous zeolite imidazate framework material as well as preparation method and application thereof - Google Patents
Mesoporous zeolite imidazate framework material as well as preparation method and application thereof Download PDFInfo
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- CN106311152A CN106311152A CN201610772191.2A CN201610772191A CN106311152A CN 106311152 A CN106311152 A CN 106311152A CN 201610772191 A CN201610772191 A CN 201610772191A CN 106311152 A CN106311152 A CN 106311152A
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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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- 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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2257/00—Components to be removed
- B01D2257/50—Carbon oxides
- B01D2257/504—Carbon dioxide
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2258/00—Sources of waste gases
- B01D2258/06—Polluted air
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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
The invention discloses a mesoporous zeolite imidazate framework material as well as a preparation method and an application thereof and belongs to the field of energy-saving and emission-reducing clean production. In the preparation process, in order to effectively improve the CO2 adsorption capacity and the adsorption selectivity of the mesoporous zeolite imidazate framework material, six brand-new organic ligands are adopted and comprise 2-amino benzimidazole with amino functional groups, 4,5-dicyano-2-aminoimidazole, 5-nitrobenzimidazole with strongly polar functional groups, benzimidazole-2-acetonitrile, 2-methylbenzimidazole with power supply base groups and 2-mercaptobenzimidazole. The prepared mesoporous zeolite imidazate framework material has the characteristics of higher crystallinity, larger specific surface area, higher heat stability and the like. With introduction of characteristic functional groups such as amino and the like, the mesoporous zeolite imidazate framework material has good characteristics of mild conditions, low operation cost, good removal effect and the like in actual CO2 adsorption operation, and the framework material is convenient to regenerate and good in circular adsorption effect.
Description
Technical field
The invention belongs to energy-saving and emission-reduction cleaning production field, be specifically related to a kind of mesoporous class zeolitic imidazolate framework material and
Its preparation method and application.
Background technology
Although the development technique of the new forms of energy such as nuclear energy, solar energy, wind energy, tide energy, geothermal energy is increasingly mature, whole people
In the energy resource structure of class society, ratio is also improving day by day.But in following decades, the mankind also will make with fossil energy
For main energy source, and the consequence thus brought is exactly a large amount of artificial CO produced2The discharge of gas.Before the industrial revolution greatly
CO in gas2Concentration is about 278ppm, and o. 11th " the greenhouse gas issued on November 19th, 2015 according to World Meteorological Organization
Body publication " display, CO average in global atmosphere in 20142Molar fraction has reached before the industrial revolution the 143% of level, for
397.7ppm.And along with the fast development of global economy, since entering 21 century, CO in air2The balanced growth of concentration
Speed is more than 2ppm/, even if the rate of rise of 2013 to 2014 has slowed down, also reaches 1.9ppm/, far above 20
The balanced growth speed (about 1.5ppm/) of the nineties in century.According to current CO2Discharge growth rate, by 2035, artificially
Produce and be discharged into CO in air243,000,000,000 tons can be reached, will be that the whole world in 2009 artificially produces CO2The 150% of amount.
The CO of air middle and high concentration2Existence, can absorb and discharge the infra-red radiation from air to ground, this mistake again
Journey, i.e. greenhouse effect, can cause average surface temperature more much higher than the situation not having this effect.Due to CO2In an atmosphere
Concentration is far above steam or some other non-solidifying property greenhouse gases (such as methane, nitrous oxide and CFCs etc.), so
CO2Being most important artificial greenhouse gases in air, the contribution to overall greenhouse effect about can account for 65%.Past 10 years
The greenhouse effect value added of 83% and the greenhouse effect value added of 5 years 82% in the past are all by CO2Concentration growth causes.And
Greenhouse effect can bring a series of serious consequences such as global climate deteriorates, and sea level rise, therefore uses various technology and absorption
Absorbent carries out CO2Trapping and storage, become CO in reduction air2The task of top priority of concentration.
Current industrial many employing alkali liquor drip washing, organic base (monoethanolamine, diethanolamine etc.) absorb enrichment CO2.These
Alkali liquid corrosion is relatively strong, can bring potential safety hazard for commercial production, and after absorption, or it is discarded to produce more absorption
Thing, or circular regeneration power consumption is higher.Therefore in the urgent need to exploitation, corrosivity is relatively low, Cheap highly effective, the solid CO that is readily transported2
Adsorbent.
Zeolitic imidazolate framework material (Zeolitic Imdazolate Framework, ZIFs), is new the having of a class
The metal of zeolite topological and machine framework material (Metal-Organic Frameworks, MOFs).It not only has similar
In the highest heat stability of zeolite and chemical stability, and have porosity the highest for MOFs, big specific surface area with
And the characteristic such as the adjustability in duct.ZIFs is to CO simultaneously2Having preferable affinity, this makes ZIFs at CO2Absorption and trapping aspect
There is huge application prospect.ZIFs material can come control hole structure and size by selecting different organic ligands, passes through
On organic ligand, the introducing of functional group improves the absorption to gas and separates.Such as, on part amido functional group or some
The introducing of highly polar functional group, ZIFs material and CO2Between Interaction enhanced so that ZIFs material has higher CO2Absorption
Performance.At present, the ZIFs material using target ligand synthesis is the most less, and CO2Absorption property needs to improve further, this
Also be the present invention attempt solve problem.
Summary of the invention
In order to overcome the shortcoming of prior art with not enough, the primary and foremost purpose of the present invention is to provide a kind of mesoporous class zeolite miaow
The preparation method of azoles ester framework material.Specifically, the present invention have no in have chosen 6 kinds of documents report with specificity official's energy
The imdazole derivatives part of group, uses solvent thermal process synthesising mesoporous class zeolitic imidazolate framework material.
Another object of the present invention is to provide the mesoporous class zeolite imidazole ester bone prepared by above-mentioned preparation method
Frame material.Framework material degree of crystallinity is higher, specific surface area is bigger for this, thermally-stabilised preferable with chemical stability.
It is still another object of the present invention to provide the application of above-mentioned mesoporous class zeolitic imidazolate framework material, mainly used
In CO2Absorption with separate.
The purpose of the present invention is achieved through the following technical solutions:
The preparation method of a kind of mesoporous class zeolitic imidazolate framework material, this material uses solvent thermal process synthesis, and wraps
Include following steps:
(1) by slaine and imdazole derivatives part, add to DMF (DMF), stir after mixing
Uniformly, mixed liquor is obtained;
(2) mixed solution that step (1) is obtained is transferred in polytetrafluoroethyllining lining stainless steel cauldron, reaction;
(3) reactor is naturally cooled to room temperature, the reactant liquor of centrifugal gained, precipitate separated after add N, N-dimethyl
Methanamide carries out supersound washing, is dried, i.e. obtains mesoporous class zeolitic imidazolate framework material.
Described slaine is zinc nitrate hexahydrate (Zn (NO3)2·6H2O), Zinc vitriol (ZnSO4·7H2O), two
Hydration zinc acetate (Zn (OAc)2·2H2And zinc chloride (ZnCl O)2One in).
Described imdazole derivatives part is 2-aminobenzimidazole, 4,5-dicyano-2-aminooimidazole, 5-nitro benzo
One in imidazoles, benzimidazolyl-2 radicals-acetonitrile, 2-tolimidazole and 2-mercaptobenzimidazole, structural formula is as follows:
The mol ratio of described slaine and imdazole derivatives part is 1:2~1:4, the consumption of DMF be 40~
100mL;
The condition of described reaction is 120~160 DEG C of reactions 20~30h;
The described condition being dried is 110~130 DEG C and is dried 16~32h.
A kind of mesoporous class zeolitic imidazolate framework material, is prepared by above-mentioned preparation method.
Described mesoporous class zeolitic imidazolate framework material is at CO2Adsorb with separate in application.
Compared with the technology such as existing alkali liquor drip washing, organic base absorption, present invention have the advantage that and effect:
(1) in preparation process, present invention employs 6 kinds of brand-new organic ligands, including the 2-ammonia of band amido functional group
Base benzimidazole, 4,5-dicyano-2-aminooimidazole, the 5-nitrobenzimidazole with highly polar functional group, benzimidazolyl-2 radicals-second
Nitrile, band is powered from the 2-tolimidazole of base, 2-mercaptobenzimidazole.
(2) mesoporous class zeolitic imidazolate framework material prepared by the present invention, have that degree of crystallinity is higher, specific surface area is relatively big,
Heat stability relatively high;Due to the introducing of the characteristic groups such as amino, CO can be effectively improved2Adsorption capacity and suction
Attached selectivity.
(3) at actual CO2Adsorption operations in, the present invention not only can be effectively prevented from the corrosion to container, also shows
Going out the good characteristics such as mild condition, running cost is low, removal effect is good, and the regeneration of this framework material is convenient, circulation absorption is imitated
The best.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is described in further detail, but embodiments of the present invention are not limited to this.
Embodiment 1
The synthesis of the class ZIFs material with 2-aminobenzimidazole as part and for CO2Absorption
Weigh 0.414g (3mmol) ZnCl2It is dissolved in 40mL DMF, adds 0.798g (6mmol) 2-amino benzo miaow
Azoles;Proceed to polytetrafluoroethyllining lining stainless steel cauldron after stirring, constant temperature blast drying oven reacts at 120 DEG C 30h;
With DMF supersound washing 5min, after circulation washs 3 times, centrifugation, gained is deposited at 120 DEG C drying 16h, i.e. can get mesh
Mark material.Take this material 0.1g, after the pre-treatments such as dry, degassing, multi-functional adsorption instrument carries out 15vol%CO2's
Breakthrough curve is tested, and records this material CO when 45 DEG C2Adsorption capacity is 58.1mg/g.
Embodiment 2
The synthesis of the class ZIFs material with 4,5-dicyano-2-aminooimidazole as part and for CO2Absorption
Weigh 0.891g (3mmol) Zn (NO3)2·6H2O is dissolved in 60mL DMF, adds 0.798g (6mmol) 4,5-
Dicyano-2-aminooimidazole;Polytetrafluoroethyllining lining stainless steel cauldron is proceeded to, in constant temperature blast drying oven after stirring
24h is reacted at 140 DEG C;With DMF supersound washing 5min, after circulation washs 3 times, centrifugation, gained is deposited at 110 DEG C drying
32h, i.e. can get target material.Take this material 0.1g, after the pre-treatments such as dry, degassing, enterprising at multi-functional adsorption instrument
Row 15vol%CO2Breakthrough curve experiment, record this material CO when 35 DEG C2Adsorption capacity is 59.4mg/g.
Embodiment 3
The synthesis of the class ZIFs material with 5-nitrobenzimidazole as part and for CO2Absorption
Weigh 0.861g (3mmol) ZnSO4·7H2O is dissolved in 80mL DMF, adds 0.978g (6mmol) 5-Nitrobenzol
And imidazoles;Proceed to polytetrafluoroethyllining lining stainless steel cauldron after stirring, react at 160 DEG C in constant temperature blast drying oven
20h;With DMF supersound washing 5min, after circulation washs 3 times, centrifugation, gained is deposited at 130 DEG C drying 16h,
To target material.Take this material 0.1g, after the pre-treatments such as dry, degassing, multi-functional adsorption instrument carries out 15vol%
CO2Breakthrough curve experiment, record this material CO when 45 DEG C2Adsorption capacity is 55.0mg/g.
Embodiment 4
The synthesis of the class ZIFs material with benzimidazolyl-2 radicals-acetonitrile as part and for CO2Absorption
Weigh 0.657g (3mmol) Zn (OAc)2·2H2O is dissolved in 100mL DMF, adds 1.880g (12mmol) benzene
And imidazoles-2-acetonitrile;Polytetrafluoroethyllining lining stainless steel cauldron is proceeded to, in constant temperature blast drying oven 160 after stirring
20h is reacted at DEG C;With DMF supersound washing 5min, after circulation washs 3 times, centrifugation, gained is deposited at 120 DEG C drying
24h, i.e. can get target material.Take this material 0.1g, after the pre-treatments such as dry, degassing, enterprising at multi-functional adsorption instrument
Row 15vol%CO2Breakthrough curve experiment, record this material CO when 35 DEG C2Adsorption capacity is 63.4mg/g.
Embodiment 5
The synthesis of the class ZIFs material with 2-tolimidazole as part and for CO2Absorption
Weigh 0.891g (3mmol) Zn (NO3)2·6H2O is dissolved in 90mL DMF, adds 1.188g (9mmol) 2-first
Base benzimidazole;Polytetrafluoroethyllining lining stainless steel cauldron is proceeded to, in constant temperature blast drying oven at 150 DEG C after stirring
Reaction 23h;With DMF supersound washing 5min, after circulation washs 3 times, centrifugation, gained is deposited at 120 DEG C drying 20h, i.e.
Available target material.Take this material 0.1g, after the pre-treatments such as dry, degassing, multi-functional adsorption instrument is carried out
15vol%CO2Breakthrough curve experiment, record this material CO when 35 DEG C2Adsorption capacity is 56.7mg/g.
Embodiment 6
The synthesis of the class ZIFs material with 2-mercaptobenzimidazole as part and for CO2Absorption
Weigh 0.891g (3mmol) Zn (NO3)2·6H2O is dissolved in 60mL DMF, adds 1.170g (7.8mmol) 2-
Mercaptobenzimidazole;Polytetrafluoroethyllining lining stainless steel cauldron is proceeded to after stirring, in constant temperature blast drying oven 140 DEG C
Lower reaction 26h;With DMF supersound washing 5min, after circulation washs 3 times, centrifugation, gained is deposited at 120 DEG C drying 20h,
I.e. can get target material.Take this material 0.1g, after the pre-treatments such as dry, degassing, multi-functional adsorption instrument is carried out
15vol%CO2Breakthrough curve experiment, record this material CO when 35 DEG C2Adsorption capacity is 61.8mg/g.
Above-described embodiment is the present invention preferably embodiment, but embodiments of the present invention are not by above-described embodiment
Limit, the change made under other any spirit without departing from the present invention and principle, modify, substitute, combine, simplify,
All should be the substitute mode of equivalence, within being included in protection scope of the present invention.
Claims (8)
1. the preparation method of a mesoporous class zeolitic imidazolate framework material, it is characterised in that use solvent thermal process synthesis, and
Comprise the following steps:
(1) by slaine and imdazole derivatives part, add to DMF, stir after mixing, obtain mixed liquor;
(2) mixed solution that step (1) is obtained is transferred in polytetrafluoroethyllining lining stainless steel cauldron, reaction;
(3) reactor is naturally cooled to room temperature, the reactant liquor of centrifugal gained, precipitate separated after add N, N-dimethyl formyl
Amine carries out supersound washing, is dried, i.e. obtains mesoporous class zeolitic imidazolate framework material.
The preparation method of mesoporous class zeolitic imidazolate framework material the most according to claim 1, it is characterised in that: described
Slaine is the one in zinc nitrate hexahydrate, Zinc vitriol, Zinc diacetate dihydrate and zinc chloride.
The preparation method of mesoporous class zeolitic imidazolate framework material the most according to claim 1, it is characterised in that: described
Imdazole derivatives part be 2-aminobenzimidazole, 4,5-dicyano-2-aminooimidazole, 5-nitrobenzimidazole, benzimidazole-
One in 2-acetonitrile, 2-tolimidazole and 2-mercaptobenzimidazole.
The preparation method of mesoporous class zeolitic imidazolate framework material the most according to claim 1, it is characterised in that: described
Slaine is 1:2~1:4 with the mol ratio of imdazole derivatives part, and the consumption of DMF is 40~100mL.
The preparation method of mesoporous class zeolitic imidazolate framework material the most according to claim 1, it is characterised in that: described
The condition of reaction is 120~160 DEG C of reactions 20~30h.
The preparation method of mesoporous class zeolitic imidazolate framework material the most according to claim 1, it is characterised in that: described
The condition being dried is 110~130 DEG C and is dried 16~32h.
7. a mesoporous class zeolitic imidazolate framework material, it is characterised in that by the preparation described in any one of claim 1~6
Method prepares.
8. the mesoporous class zeolitic imidazolate framework material described in claim 7 is at CO2Adsorb with separate in application.
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN106964316A (en) * | 2017-03-17 | 2017-07-21 | 华南理工大学 | A kind of zeolite imidazole ester skeleton functionalized ion liquid composite and its preparation and application |
CN108686623A (en) * | 2017-04-05 | 2018-10-23 | 中国科学院上海高等研究院 | Metal-organic framework materials-molecular sieves compound material and preparation method thereof |
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CN102895954A (en) * | 2012-10-16 | 2013-01-30 | 中国石油大学(北京) | Preparation method for novel gasoline sweetening adsorbent and application of novel gasoline sweetening adsorbent |
CN102921377A (en) * | 2012-06-01 | 2013-02-13 | 中国科学院宁波材料技术与工程研究所 | Preparation method for nitrogen-rich ZMOF type metal-organic framework porous material |
CN103951684A (en) * | 2014-04-10 | 2014-07-30 | 吉林大学 | Mixed ligand zeolitic imidazole framework, preparation method and application to carbon dioxide selective adsorption |
US20150191491A1 (en) * | 2014-01-03 | 2015-07-09 | National Central University | Preparation method of zeolitic imidazolate framework-90 in water-based system |
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US20120247328A1 (en) * | 2011-04-04 | 2012-10-04 | Georgia Tech Research Corporation | Mof nanocrystals |
CN102921377A (en) * | 2012-06-01 | 2013-02-13 | 中国科学院宁波材料技术与工程研究所 | Preparation method for nitrogen-rich ZMOF type metal-organic framework porous material |
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
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CN106964316A (en) * | 2017-03-17 | 2017-07-21 | 华南理工大学 | A kind of zeolite imidazole ester skeleton functionalized ion liquid composite and its preparation and application |
CN108686623A (en) * | 2017-04-05 | 2018-10-23 | 中国科学院上海高等研究院 | Metal-organic framework materials-molecular sieves compound material and preparation method thereof |
CN108686623B (en) * | 2017-04-05 | 2020-12-04 | 中国科学院上海高等研究院 | Metal organic framework material-molecular sieve composite material and preparation method thereof |
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