CN112724418A - Preparation method and application of calcium-based metal organic framework material - Google Patents
Preparation method and application of calcium-based metal organic framework material Download PDFInfo
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- CN112724418A CN112724418A CN202110063046.8A CN202110063046A CN112724418A CN 112724418 A CN112724418 A CN 112724418A CN 202110063046 A CN202110063046 A CN 202110063046A CN 112724418 A CN112724418 A CN 112724418A
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- 239000000463 material Substances 0.000 title claims abstract description 59
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 title claims abstract description 35
- 229910052791 calcium Inorganic materials 0.000 title claims abstract description 35
- 239000011575 calcium Substances 0.000 title claims abstract description 35
- 239000012621 metal-organic framework Substances 0.000 title claims abstract description 31
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 28
- 238000006243 chemical reaction Methods 0.000 claims abstract description 18
- 238000000926 separation method Methods 0.000 claims abstract description 15
- 239000007787 solid Substances 0.000 claims abstract description 12
- 229910052751 metal Inorganic materials 0.000 claims abstract description 9
- 239000002184 metal Substances 0.000 claims abstract description 9
- 239000002994 raw material Substances 0.000 claims abstract description 9
- 238000001291 vacuum drying Methods 0.000 claims abstract description 8
- 238000000034 method Methods 0.000 claims abstract description 5
- 238000005406 washing Methods 0.000 claims abstract description 5
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims description 11
- 229910001628 calcium chloride Inorganic materials 0.000 claims description 11
- 239000001110 calcium chloride Substances 0.000 claims description 11
- 238000001179 sorption measurement Methods 0.000 claims description 11
- SQJQLYOMPSJVQS-UHFFFAOYSA-N 4-(4-carboxyphenyl)sulfonylbenzoic acid Chemical compound C1=CC(C(=O)O)=CC=C1S(=O)(=O)C1=CC=C(C(O)=O)C=C1 SQJQLYOMPSJVQS-UHFFFAOYSA-N 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 4
- 238000002156 mixing Methods 0.000 abstract description 8
- 238000002474 experimental method Methods 0.000 abstract description 5
- 230000035515 penetration Effects 0.000 abstract description 5
- -1 polytetrafluoroethylene Polymers 0.000 abstract description 4
- 238000007789 sealing Methods 0.000 abstract description 4
- 229920001343 polytetrafluoroethylene Polymers 0.000 abstract description 3
- 239000004810 polytetrafluoroethylene Substances 0.000 abstract description 3
- 229910018503 SF6 Inorganic materials 0.000 description 29
- SFZCNBIFKDRMGX-UHFFFAOYSA-N sulfur hexafluoride Chemical compound FS(F)(F)(F)(F)F SFZCNBIFKDRMGX-UHFFFAOYSA-N 0.000 description 28
- 229960000909 sulfur hexafluoride Drugs 0.000 description 19
- 239000007789 gas Substances 0.000 description 18
- 235000019441 ethanol Nutrition 0.000 description 10
- 235000011148 calcium chloride Nutrition 0.000 description 9
- 238000012360 testing method Methods 0.000 description 5
- 239000005431 greenhouse gas Substances 0.000 description 4
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 3
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 229910002092 carbon dioxide Inorganic materials 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 238000009210 therapy by ultrasound Methods 0.000 description 2
- 238000010792 warming Methods 0.000 description 2
- 230000000274 adsorptive effect Effects 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 229910003460 diamond Inorganic materials 0.000 description 1
- 239000010432 diamond Substances 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000004817 gas chromatography Methods 0.000 description 1
- 238000002329 infrared spectrum Methods 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 238000000696 nitrogen adsorption--desorption isotherm Methods 0.000 description 1
- 239000013384 organic framework Substances 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000001144 powder X-ray diffraction data Methods 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 239000012925 reference material Substances 0.000 description 1
- 239000003507 refrigerant Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000002411 thermogravimetry Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G83/00—Macromolecular compounds not provided for in groups C08G2/00 - C08G81/00
- C08G83/008—Supramolecular polymers
-
- 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]
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B17/00—Sulfur; Compounds thereof
- C01B17/45—Compounds containing sulfur and halogen, with or without oxygen
- C01B17/4507—Compounds containing sulfur and halogen, with or without oxygen containing sulfur and halogen only
- C01B17/4515—Compounds containing sulfur and halogen, with or without oxygen containing sulfur and halogen only containing sulfur and fluorine only
- C01B17/453—Sulfur hexafluoride
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B21/00—Nitrogen; Compounds thereof
- C01B21/04—Purification or separation of nitrogen
- C01B21/0405—Purification or separation processes
- C01B21/0433—Physical processing only
- C01B21/045—Physical processing only by adsorption in solids
- C01B21/0455—Physical processing only by adsorption in solids characterised by the adsorbent
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2210/00—Purification or separation of specific gases
- C01B2210/0001—Separation or purification processing
- C01B2210/0009—Physical processing
- C01B2210/0014—Physical processing by adsorption in solids
- C01B2210/0015—Physical processing by adsorption in solids characterised by the adsorbent
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- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Analytical Chemistry (AREA)
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- Polymers & Plastics (AREA)
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Abstract
The invention discloses a preparation method and application of a calcium-based metal organic framework material, wherein the preparation method comprises the following steps: adding a proper amount of calcium-based metal, 4' -sulfonyl dibenzoic acid and ethanol into a reaction kettle with a polytetrafluoroethylene lining; uniformly mixing the raw materials in a reaction kettle; sealing the uniformly mixed raw materials in a reaction kettle, and reacting in an oven for a set time; after the reaction is finished, the temperature is returned to the room temperature, and then the reacted materials are subjected to centrifugal separation to obtain white solids; washing the white solid with an ethanol solution; putting the washed materials in a vacuum drying boxDrying to obtain the calcium-based metal organic framework material. The calcium-based metal organic framework material Ca-MOF prepared by the method has excellent separation selectivity at low concentration, and the mixed kinetics penetration experiment proves that the Ca-MOF can completely separate SF6/N2(SF6：N210:90) the material has high thermal stability and reproducibility and good air stability.
Description
Technical Field
The invention relates to the technical field of metal framework materials, in particular to a preparation method and application of a calcium-based metal organic framework material.
Background
Atmospheric pollution is closely related to people's life, and the common greenhouse gas is carbon dioxide (CO)2) Methane (CH)4). In addition, Hydrofluorocarbons (HCFs), Perfluorocarbons (PFCs), sulfur hexafluoride (SF)6) Is also a greenhouse gas and has a very strong ability to cause greenhouse effect. Global warming has become an important obstacle for the sustainable development of human economy and society, and the control of pollutant and greenhouse gas emissions is an important means for controlling global warming. Among the six greenhouse gases, CO2The content of sulfur hexafluoride in the atmosphere is the highest, but the service life of sulfur hexafluoride in the atmosphere is as long as 3200 years, so that the control is more needed. Current SF6The gas is mainly used in the power industry, and sulfur hexafluoride gas is used for various types of electrical equipment as an insulation and arc extinguishing gas, and is also a refrigerant gas widely used in gas-insulated substations and circuit breakers. Pure sulfur hexafluoride is liquefied at room temperature of 20 deg.C and pressure of 2MPa, if sulfur hexafluoride is mixed with nitrogen (SF)6:N210:90), it is liquefied at a pressure of 20 Mpa. Therefore, SF is required to be developed6/N2The high-efficiency separation means controls the emission of sulfur hexafluoride gas, reduces the influence of greenhouse effect and improves the utilization rate of the sulfur hexafluoride. Therefore, the invention starts from the metal framework material and develops the SF which can be efficiently separated under low concentration6/N2A metal skeleton material of mixed gas.
Disclosure of Invention
To this end, the technical problem to be solved by the invention is to overcome the prior art for separating SF6/N2The defects of the mixed gas further provide a preparation method and application of the calcium-based metal organic framework material.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of a calcium-based metal organic framework material comprises the following steps:
s1: adding a proper amount of calcium-based metal, 4' -sulfonyl dibenzoic acid and ethanol into a reaction kettle with a polytetrafluoroethylene lining;
s2: uniformly mixing the raw materials in a reaction kettle;
s3: sealing the uniformly mixed raw materials in the step S2 in a reaction kettle, and reacting in an oven for a set time;
s4: after the reaction is finished, the temperature is returned to the room temperature, and then the reacted materials are subjected to centrifugal separation to obtain white solids;
s5: washing the white solid obtained in the step S4 with an ethanol solution;
s6: and (5) drying the material washed in the step S5 in a vacuum drying oven to obtain the calcium-based metal organic framework material.
Preferably, the calcium-based metal in step S1 is calcium chloride, and the weight ratio of the calcium chloride to the 4,4' -sulfonyl dibenzoic acid is (0.2-0.45): 1.
Preferably, the step S2 is performed by using ultrasonic waves for 3 hours to mix the materials uniformly.
Preferably, the temperature of the oven in the step S3 is 440-460K; the reaction time is set to 96-100 hours.
Preferably, the white solid obtained in step S4 is washed twice or more with fresh ethanol.
Preferably, the set temperature of the vacuum drying oven in the step S6 is 373-393K.
A calcium-based metal organic framework material obtainable by any of the methods described above.
The calcium-based metal organic framework material is applied to adsorption separation of SF6/N2And (4) mixing the gases.
The invention has the beneficial effects that:
the calcium-based metal organic framework material Ca-MOF prepared by the method has excellent separation selectivity at low concentration, and the mixed kinetics penetration experiment proves that the Ca-MOF can completely separate SF6/N2(SF6：N210:90) mixing ofThe material has high thermal stability and renewability, and good air stability.
Drawings
In order that the present invention may be more readily and clearly understood, reference is now made to the following detailed description taken in conjunction with the accompanying drawings, in which:
FIG. 1 is a calcium-based metal organic framework material (Ca-MOF) of the present invention2) Schematic structural diagram of (a);
FIG. 2a is a PXRD pattern of the Ca-MOF material of the present invention;
FIG. 2b is a plot of the N2 adsorption-desorption isotherm at 77K for the Ca-MOF material of the invention;
FIG. 3 is SF of a Ca-MOF material of the invention6And N2Gas adsorption isotherms at 298K;
FIG. 4a is a graph of adsorptive separation selectivity at different concentrations;
FIG. 4b is a comparison of the separation performance of the Ca-MOF material of the invention with various reference materials;
FIG. 5 is a mixed kinetic penetration experiment of Ca-MOF materials of the invention;
FIG. 6 is a thermogravimetric analysis of a Ca-MOF material of the invention;
FIG. 7 is a chart of the infrared spectrum of a Ca-MOF material of the present invention;
FIG. 8a is a 10 μm scanning electron micrograph of a Ca-MOF material of the present invention;
FIG. 8b is a 1 μm scanning electron micrograph of a Ca-MOF material of the present invention.
Detailed Description
A preparation method of a calcium-based metal organic framework material comprises the following steps:
s1: adding a proper amount of calcium chloride, 4' -sulfonyl dibenzoic acid and ethanol into a reaction kettle with a polytetrafluoroethylene lining;
s2: uniformly mixing the raw materials in a reaction kettle;
s3: sealing the uniformly mixed raw materials in the step S2 in a reaction kettle, and reacting in an oven for a set time;
s4: after the reaction is finished, the temperature is returned to the room temperature, and then the reacted materials are subjected to centrifugal separation to obtain white solids;
s5: washing the white solid obtained in the step S4 with an ethanol solution;
s6: and (5) drying the material washed in the step S5 in a vacuum drying oven to obtain the calcium-based metal organic framework material.
The weight ratio of the calcium chloride to the 4,4' -sulfonyl dibenzoic acid in the step S1 is (0.2-0.45): 1. And in the step S2, ultrasonic treatment is adopted for 3 hours to uniformly mix the materials. The temperature of the oven in the step S3 is 440-460K; the reaction time is set to 96-100 hours. The white solid obtained in step S4 was washed twice more with fresh ethanol. The set temperature of the vacuum drying oven in the step S6 is 373-393K.
The calcium-based metal organic framework material is applied to adsorption separation of SF6/N2And (4) mixing the gases.
In a specific embodiment, the selected raw materials are calcium chloride (CaCl2, 98% or more), 4,4 '-sulfonyl dibenzoic acid (4,4' -SDB, 98%), and ethanol (C2H5OH, 95%). Adding CaCl2 (0.074g,0.6mmol), 4,4' -SDB (0.198g,0.6mmol) and a C2H5OH solution (10g,12.7mL) into a 25mL polytetrafluoroethylene-lined reaction kettle, performing ultrasonic treatment for 3 hours to mix uniformly, sealing, reacting in a 453K oven for 4 days, recovering the room temperature after the reaction is finished, performing centrifugal separation to obtain a white solid, washing with a fresh ethanol solution for multiple times, and further drying in a 383K vacuum drying oven to obtain the calcium-based metal organic framework material Ca-MOF, wherein the chemical formula of the Ca-MOF is as follows: c14H8CaO6And S. The weight ratio (0.2-0.45) of the calcium chloride to the 4,4 '-sulfonyl dibenzoic acid is 1, the calcium chloride and the 4,4' -sulfonyl dibenzoic acid can meet the requirement, the specific embodiment is only the best embodiment, and the invention is not limited to the proportion.
Referring to FIGS. 1-8b, the complex reaction of a calcium-based metal with 4,4' -sulfonyldibenzoic acid by the above method solvothermally synthesizes a material Ca-MOF in which one-dimensional (1D) diamond open channels, mainly formed of four aromatic rings of low polarity and having an average size of four, are present along the crystalline b-axis in the formed three-dimensional (3D) framework
The calcium-based metal organic framework material is used for separating SF6/N2And (4) mixing the gases.
Referring to fig. 1-8b, the invention synthesizes a calcium-based metal organic framework material (i.e. Ca-MOF) with stable properties, the IAST selectivity of Ca-MOF is as high as 326 under 298K and 1bar conditions, which is superior to that of the existing porous adsorption material, and the selectivity is 694,727 under low concentration (y is 0.002, 0.0003). In addition, the experimental breakthrough curve shows that the organic framework material of the invention can be prepared from SF6/N2Efficient recovery of SF from mixed gas6The efficiency is over 99 percent, and is SF in practical industrial application6/N2The ideal choice for separation. The calcium-based metal organic framework material has better thermal stability and regenerability, good air stability and excellent separation selectivity at low concentration, and a mixed kinetic penetration experiment (see figure 5) proves that the Ca-MOF can completely separate SF6/N2(SF6：N210:90) and (3) mixing. As a result of the penetration test, sulfur hexafluoride (SF) was injected over a period of time6) Is absorbed away from the mixed gas so as to achieve the purpose of separating the mixed gas from the mixed gas.
Ca-MOF material adsorption test of the invention: the activated sample (0.5g) was subjected to adsorption test using a Quantachrome Autosorb IQ analyzer. Prior to the adsorption measurement, the sample was degassed under vacuum at 290 ℃ for 12h and then allowed to cool to room temperature. During the test, a water bath was used to maintain the temperature of the system. And collecting adsorption data, wherein the equilibrium time of each data point on the adsorption isotherm is 30 min. (see FIG. 3 in particular)
Breakthrough adsorption testing of the Ca-MOF material of the invention: to evaluate the dynamic separation performance of SBMOF-1, SF was used directly6/N2Mixture (SF)6 Volume concentration 10%) were subjected to breakthrough experiments. The activated powder sample (0.24g) was loaded into a cylindrical stainless steel column having a length of 150mm and an inner diameter of 4.5mm, and the loaded length of the sample was about 60 mm. Gas flow and pressure at the inletControl is effected by use of mass flow controllers and pressure control valves. The column was placed in a temperature controlled environment. After cooling to room temperature, the mixed gas was fed to the bed at 298K and 1bar with a total flow rate of 15 mL/min. The component concentrations in the effluent gas were continuously monitored by gas chromatography (GC2030, DAOJIN), see fig. 5.
The above embodiments are merely to explain the technical solutions of the present invention in detail, and the present invention is not limited to the above embodiments, and it should be understood by those skilled in the art that all modifications and substitutions based on the above principles and spirit of the present invention should be within the protection scope of the present invention.
Claims (8)
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117563557A (en) * | 2023-11-03 | 2024-02-20 | 江苏海普功能材料有限公司 | Defluorination adsorbent, preparation method thereof and defluorination method of lithium battery recovery liquid |
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| US20130066093A1 (en) * | 2011-09-09 | 2013-03-14 | Chung Yuan Christian University | Metal (ii) coordination polymers and synthesizing method thereof |
| CN110465272A (en) * | 2019-09-09 | 2019-11-19 | 北京化工大学 | A kind of two-dimensional metallic-organic framework material is in SF6/N2Application in separation |
| KR20200007237A (en) * | 2018-07-12 | 2020-01-22 | 연세대학교 산학협력단 | Adsorbents with sulphur hexafluoride selectivity and method for gas separation using the same |
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- 2021-01-18 CN CN202110063046.8A patent/CN112724418A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20130066093A1 (en) * | 2011-09-09 | 2013-03-14 | Chung Yuan Christian University | Metal (ii) coordination polymers and synthesizing method thereof |
| TW201311732A (en) * | 2011-09-09 | 2013-03-16 | 私立中原大學 | Metal (II) coordination polymers and synthesizing method thereof |
| KR20200007237A (en) * | 2018-07-12 | 2020-01-22 | 연세대학교 산학협력단 | Adsorbents with sulphur hexafluoride selectivity and method for gas separation using the same |
| CN110465272A (en) * | 2019-09-09 | 2019-11-19 | 北京化工大学 | A kind of two-dimensional metallic-organic framework material is in SF6/N2Application in separation |
Non-Patent Citations (1)
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| RUI SUN 等: "Hierarchical Porous Carbon Synthesized from Novel Porous Amorphous Calcium or Magnesium Citrate with Enhanced SF6 Uptake and SF6/N2 Selectivity", 《APPLIED NANO MATERIALS》 * |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN117563557A (en) * | 2023-11-03 | 2024-02-20 | 江苏海普功能材料有限公司 | Defluorination adsorbent, preparation method thereof and defluorination method of lithium battery recovery liquid |
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