CN109575305A - Preparation method of Co-MOF air-sensitive nano material and products thereof and application - Google Patents
Preparation method of Co-MOF air-sensitive nano material and products thereof and application Download PDFInfo
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- CN109575305A CN109575305A CN201811560516.6A CN201811560516A CN109575305A CN 109575305 A CN109575305 A CN 109575305A CN 201811560516 A CN201811560516 A CN 201811560516A CN 109575305 A CN109575305 A CN 109575305A
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- air
- mof
- nano material
- sensitive nano
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- 239000012921 cobalt-based metal-organic framework Substances 0.000 title claims abstract description 28
- 239000002086 nanomaterial Substances 0.000 title claims abstract description 28
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 238000006243 chemical reaction Methods 0.000 claims abstract description 15
- 239000012621 metal-organic framework Substances 0.000 claims abstract description 12
- 238000000034 method Methods 0.000 claims abstract description 11
- 229910052751 metal Inorganic materials 0.000 claims abstract description 8
- 230000035484 reaction time Effects 0.000 claims abstract description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 15
- OYFRNYNHAZOYNF-UHFFFAOYSA-N 2,5-dihydroxyterephthalic acid Chemical compound OC(=O)C1=CC(O)=C(C(O)=O)C=C1O OYFRNYNHAZOYNF-UHFFFAOYSA-N 0.000 claims description 10
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 10
- 235000019441 ethanol Nutrition 0.000 claims description 10
- 230000001376 precipitating effect Effects 0.000 claims description 10
- 238000005303 weighing Methods 0.000 claims description 10
- 229940011182 cobalt acetate Drugs 0.000 claims description 5
- QAHREYKOYSIQPH-UHFFFAOYSA-L cobalt(II) acetate Chemical compound [Co+2].CC([O-])=O.CC([O-])=O QAHREYKOYSIQPH-UHFFFAOYSA-L 0.000 claims description 5
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 5
- 239000007787 solid Substances 0.000 claims description 5
- 239000002904 solvent Substances 0.000 claims description 5
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 239000002184 metal Substances 0.000 claims description 3
- 238000001291 vacuum drying Methods 0.000 claims description 3
- 238000001514 detection method Methods 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 12
- 238000011084 recovery Methods 0.000 abstract description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000003446 ligand Substances 0.000 description 2
- 229910021645 metal ion Inorganic materials 0.000 description 2
- 239000012922 MOF pore Substances 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 210000003850 cellular structure Anatomy 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 230000000717 retained effect Effects 0.000 description 1
- 238000001338 self-assembly Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
Classifications
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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
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
- G01N33/0004—Gaseous mixtures, e.g. polluted air
- G01N33/0009—General constructional details of gas analysers, e.g. portable test equipment
- G01N33/0027—General constructional details of gas analysers, e.g. portable test equipment concerning the detector
- G01N33/0036—General constructional details of gas analysers, e.g. portable test equipment concerning the detector specially adapted to detect a particular component
- G01N33/004—CO or CO2
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Engineering & Computer Science (AREA)
- Medicinal Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Physics & Mathematics (AREA)
- Biochemistry (AREA)
- Combustion & Propulsion (AREA)
- Polymers & Plastics (AREA)
- Food Science & Technology (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Analytical Chemistry (AREA)
- Organic Chemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating Or Analyzing Materials By The Use Of Fluid Adsorption Or Reactions (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
Abstract
The invention discloses preparation methods of a kind of Co-MOF air-sensitive nano material and products thereof and application, this method constructs a kind of using Co as the metal-organic framework of metal center, the conditions such as concentration, ratio, reaction time, reaction temperature by adjusting presoma, prepare Co-MOF air-sensitive nano material.The content of metal center is higher compared with other metal-organic framework materials, has more gas-sensitive reaction active sites；The Co-MOF air-sensitive nano material purity is high of invention preparation, size uniformity, large specific surface area, air-sensitive response limit is low, and response recovery time is short.
Description
Technical field
The invention belongs to metal organic frame field of nanometer material technology, and in particular to a kind of system of Co-MOF air-sensitive nano material
Preparation Method and products thereof and application.
Background technique
Metal organic framework (Metal-organic frameworks, MOFs) material be by metal ion with it is organic
Hollow mesh material made of ligand (being fragrant polyacid and polybase mostly) self assembly, compared with conventional porous materials,
There is MOF large specific surface area, cellular structure to enrich, porosity height, stable structure, easily select different metal ion and organic bridge
The unique advantages such as ligand are connect, cause sizable concern in the past 10 years.Currently, MOFs investigation of materials is concentrated mainly on gas suction
Echo gas separation.And since gas-sensitive reaction usually occurs to it requires that material has bigger specific surface on gas sensitive surface
Long-pending and higher porosity, and gas-sensitive reaction is also related to gas absorption desorption process, so MOFs material is applied in air-sensitive field
It has a extensive future.This porous MOFs is converted into derivative oxide material often through self-sacrifice method, to improve its gas
Quick response performance.
Summary of the invention
In view of the deficiencies of the prior art, it is an object of that present invention to provide a kind of preparation sides of Co-MOF air-sensitive nano material
Method.
Another object of the present invention is: providing a kind of Co-MOF air-sensitive nano material product of above method preparation.
Another object of the present invention is to: a kind of application of the said goods is provided.
The object of the invention is realized by following proposal: a kind of preparation method of Co-MOF air-sensitive nano material constructs one
Kind passes through the concentration for adjusting presoma, ratio, reaction time, reaction temperature using Co as the metal-organic framework of metal center
Degree condition prepares Co-MOF air-sensitive nano material, includes the following steps:
(1) cobalt acetate for weighing 1.0-1.5g is dissolved in 35mL deionized water, and is stirred evenly, and solution 1 is obtained；
(2) 2,5-Dihydroxyterephthalic acid for weighing 0.4-0.6g is dissolved in 35mL tetrahydrofuran, and is stirred evenly, and is obtained molten
Liquid 2；
(3) solution 2 is poured into rapidly in solution 1, is stirred evenly, obtain solution 3；
(4) solution 3 is transferred in reaction kettle, is heated to 100-140 DEG C and reaction is sufficiently stirred, precipitating is filtered, and washes
Wash drying；
(5) it then disperses precipitating in 120mL ethyl alcohol one day；
(6) alcohol solvent is poured out, by solid in vacuum drying 12h, obtains Co-MOF air-sensitive nano material.
Wherein, it is described be stirred to react the time be 1-4 days.
The vacuum drying temperature is 120-180 DEG C.
The present invention also provides a kind of Co-MOF air-sensitive nano materials, are prepared according to any of the above-described the method.
Also, the application present invention provides a kind of Co-MOF air-sensitive nano material in CO gas detection.
The present invention has synthesized cobalt-based MOF material using very easy method and has been improved by the improvement to synthesis technology
The stability of material makes it not need to be converted to corresponding oxide and applied.Its special pattern and huge compare table
Area is retained, and shows lower Monitoring lower-cut to CO gas.
The content of metal center is higher compared with other metal-organic framework materials, has more gas-sensitive reaction active sites
Point；Using the Co-MOF air-sensitive nano material purity is high of the method for the present invention preparation, size uniformity, large specific surface area, air-sensitive response
The limit is low, and response recovery time is short.
Detailed description of the invention
Fig. 1 is the real-time response curve of Co-MOF air-sensitive nano material of the invention to 200ppb CO gas.
Specific embodiment
Embodiment 1:
A kind of preparation method of Co-MOF air-sensitive nano material constructs a kind of using Co as the metal organic frame knot of metal center
Structure prepares Co-MOF air-sensitive nano material, presses by adjusting concentration, ratio, reaction time, the reaction temperature condition of presoma
Following steps:
(1) cobalt acetate for weighing 1.0g is dissolved in 35mL deionized water, and is stirred evenly, and solution 1 is obtained；
(2) 2,5-Dihydroxyterephthalic acid for weighing 0.4g is dissolved in 35mL tetrahydrofuran, and is stirred evenly, and solution 2 is obtained；
(3) solution 2 is poured into rapidly in solution 1, is stirred evenly, obtain solution 3；
(4) solution 3 is transferred in reaction kettle, is heated to 120 DEG C and reacts 2day；Precipitating is filtered, and washs drying；
(5) it then disperses precipitating in 120mL ethyl alcohol one day；
(6) alcohol solvent is poured out, by solid 150 DEG C of dry 12h in a vacuum, obtains Co-MOF air-sensitive nano material.
Fig. 1 is the real-time response curve of Co-MOF air-sensitive nano material of the invention to 200ppb CO gas, operating temperature
200 DEG C, wherein susceptibility about 1.836, show that material has good response for the CO gas of ppb rank.
Embodiment 2:
A kind of preparation method of Co-MOF air-sensitive nano material, it is approximate with embodiment 1, as follows:
(1) cobalt acetate for weighing 1.5g is dissolved in 35mL deionized water, and is stirred evenly, and solution 1 is obtained；
(2) 2,5-Dihydroxyterephthalic acid for weighing 0.5g is dissolved in 35mL tetrahydrofuran, and is stirred evenly, and solution 2 is obtained；
(3) solution 2 is poured into rapidly in solution 1, is stirred evenly, obtain solution 3；
(4) solution 3 is transferred in reaction kettle, is heated to 130 DEG C and reacts 3day；Precipitating is filtered, and washs drying；
(5) it then disperses precipitating in 120mL ethyl alcohol one day；
(6) alcohol solvent is poured out, by solid 180 DEG C of dry 12h in a vacuum, obtains Co-MOF air-sensitive nano material.
Embodiment 3:
A kind of preparation method of Co-MOF air-sensitive nano material, it is approximate with embodiment 1, as follows:
(1) cobalt acetate for weighing 1.3g is dissolved in 35mL deionized water, and is stirred evenly, and solution 1 is obtained；
(2) 2,5-Dihydroxyterephthalic acid for weighing 0.6g is dissolved in 35mL tetrahydrofuran, and is stirred evenly, and solution 2 is obtained；
(3) solution 2 is poured into rapidly in solution 1, is stirred evenly, obtain solution 3；
(4) solution 3 is transferred in reaction kettle, is heated to 100 DEG C and reacts 4day；Precipitating is filtered, and washs drying；
(5) it then disperses precipitating in 120mL ethyl alcohol one day；
(6) alcohol solvent is poured out, by solid 130 DEG C of dry 12h in a vacuum, obtains Co-MOF air-sensitive nano material.
Claims (5)
1. a kind of preparation method of Co-MOF air-sensitive nano material, it is characterised in that this method constructs one kind using Co as in metal
The metal-organic framework of the heart prepares Co- by adjusting concentration, ratio, reaction time, the reaction temperature condition of presoma
MOF air-sensitive nano material, includes the following steps:
(1) cobalt acetate for weighing 1.0-1.5g is dissolved in 35mL deionized water, and is stirred evenly, and solution 1 is obtained；
(2) 2,5-Dihydroxyterephthalic acid for weighing 0.4-0.6g is dissolved in 35mL tetrahydrofuran, and is stirred evenly, and is obtained molten
Liquid 2；
(3) solution 2 is poured into rapidly in solution 1, is stirred evenly, obtain solution 3；
(4) solution 3 is transferred in reaction kettle, is heated to 100-140 DEG C and reaction is sufficiently stirred；The precipitating of generation is filtered, and
Wash drying；
(5) it then disperses precipitating in 120mL ethyl alcohol one day；
(6) alcohol solvent is poured out, solid is dried in vacuo 12h, obtains Co-MOF air-sensitive nano material.
2. preparation method according to claim 1, which is characterized in that it is described be stirred to react the time be 1-4 days.
3. preparation method according to claim 1, which is characterized in that vacuum drying temperature is 120-180 DEG C.
4. a kind of Co-MOF air-sensitive nano material, it is characterised in that -3 any the methods are prepared according to claim 1.
5. a kind of application of the Co-MOF air-sensitive nano material in CO gas detection according to claim 4.
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| CN201811560516.6A CN109575305B (en) | 2018-12-20 | 2018-12-20 | Preparation method of Co-MOF gas-sensitive nano material, product and application thereof |
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Cited By (2)
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| CN110026242A (en) * | 2019-05-10 | 2019-07-19 | 上海纳米技术及应用国家工程研究中心有限公司 | A kind of preparation method of Co/Ce bimetallic MOF base ozone catalyst and products thereof and application |
| CN115651258A (en) * | 2022-10-27 | 2023-01-31 | 陕西科技大学 | Co-BPDC/MXene composite material, preparation method and application |
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