CN116120573A - Coordination polymer material and preparation method and application thereof - Google Patents
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- 239000000463 material Substances 0.000 title claims abstract description 36
- 239000013256 coordination polymer Substances 0.000 title claims abstract description 33
- 229920001795 coordination polymer Polymers 0.000 title claims abstract description 33
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 41
- 239000007788 liquid Substances 0.000 claims abstract description 8
- 238000000034 method Methods 0.000 claims abstract description 7
- PVCWVPYGNHEGIZ-UHFFFAOYSA-N 3-(2,3,4-tripyridin-3-ylcyclobutyl)pyridine Chemical group N1=CC(=CC=C1)C1C(C(C1C=1C=NC=CC=1)C=1C=NC=CC=1)C=1C=NC=CC=1 PVCWVPYGNHEGIZ-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000010438 heat treatment Methods 0.000 claims abstract description 5
- 239000013078 crystal Substances 0.000 claims description 18
- 238000006243 chemical reaction Methods 0.000 claims description 13
- 238000001179 sorption measurement Methods 0.000 claims description 7
- 239000011148 porous material Substances 0.000 claims description 4
- LJUIBUKIAISMFU-AATRIKPKSA-N 3-[(e)-2-pyridin-3-ylethenyl]pyridine Chemical group C=1C=CN=CC=1/C=C/C1=CC=CN=C1 LJUIBUKIAISMFU-AATRIKPKSA-N 0.000 claims description 3
- QOYRNHQSZSCVOW-UHFFFAOYSA-N cadmium nitrate tetrahydrate Chemical compound O.O.O.O.[Cd+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O QOYRNHQSZSCVOW-UHFFFAOYSA-N 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 3
- 238000006352 cycloaddition reaction Methods 0.000 claims description 3
- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
- 238000001914 filtration Methods 0.000 claims description 3
- 230000001699 photocatalysis Effects 0.000 claims description 3
- -1 polytetrafluoroethylene Polymers 0.000 claims description 3
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 3
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 3
- 238000007789 sealing Methods 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- 238000007146 photocatalysis Methods 0.000 claims 1
- 238000001308 synthesis method Methods 0.000 abstract 1
- 239000003463 adsorbent Substances 0.000 description 4
- 239000013505 freshwater Substances 0.000 description 4
- 238000010586 diagram Methods 0.000 description 3
- LJUIBUKIAISMFU-UHFFFAOYSA-N 3-(2-pyridin-3-ylethenyl)pyridine Chemical group C=1C=CN=CC=1C=CC1=CC=CN=C1 LJUIBUKIAISMFU-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 238000007259 addition reaction Methods 0.000 description 2
- 150000001336 alkenes Chemical class 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical group C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 1
- 239000005977 Ethylene Substances 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 229910021536 Zeolite Inorganic materials 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 239000002808 molecular sieve Substances 0.000 description 1
- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 239000013259 porous coordination polymer Substances 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 239000000741 silica gel Substances 0.000 description 1
- 229910002027 silica gel Inorganic materials 0.000 description 1
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
- 239000010457 zeolite Substances 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
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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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- E—FIXED CONSTRUCTIONS
- E03—WATER SUPPLY; SEWERAGE
- E03B—INSTALLATIONS OR METHODS FOR OBTAINING, COLLECTING, OR DISTRIBUTING WATER
- E03B3/00—Methods or installations for obtaining or collecting drinking water or tap water
- E03B3/28—Methods or installations for obtaining or collecting drinking water or tap water from humid air
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- Polymers & Plastics (AREA)
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Abstract
The invention discloses a coordination polymer material, a preparation method and application thereof, wherein the coordination polymer material is [ Cd (1, 3-bdc) (3, 3' -tpcb) 0.5 ] n Wherein 3,3' -tpcb is 1,2,3, 4-tetra (3-pyridyl) cyclobutane, 1,3-bdc is 1, 3-phthalate, and n is a repeating unit number, which is any positive integer. Coordination Polymer Material [ Cd (1, 3-bdc) (3, 3' -tpcb) 0.5 ] n Placed in a low humidity environment, can absorb moisture in the environment and generate [ Cd (1, 3-bdc) (3, 3' -tpcb) 0.5 (H 2 O)] n The method comprises the steps of carrying out a first treatment on the surface of the The water adsorbed by the coordination polymer is volatilized by heating through the solar heat collector and is condensed into liquid water, so that the air circulation water taking is realized. The method comprisesThe synthesis method of the coordination polymer material has simple operation, good repeatability and high product yield, and can circularly take water from the air.
Description
Technical Field
The invention belongs to the field of novel materials, and particularly relates to a coordination polymer material capable of being used for dispersing, small-scale and portable water taking from air in a low-humidity area and a preparation method thereof.
Background
Fresh water resources are the most important natural resources and are the basis of all biological life activities. The fresh water resources that humans can actually utilize are quite limited.
The water vapor content in the air is large, renewable and clean, and the water content in the air is estimated to be 12.9x10 12 m 3 . While the fresh water resources in the atmosphere are still not fully exploited and utilized. In theory, the adsorbent is utilized, the adsorption type air water taking technology is adopted to adsorb vapor in the atmosphere, the vapor volatilizes from the adsorbent under the drive of solar energy, the dew point temperature of the vapor is reduced, the vapor is condensed into liquid water, and the liquid water is converted into fresh water for people to use. The adsorption type air water taking method has the advantages of great potential, flexibility, convenience and low energy consumption.
In the adsorption type air water intake technology, the performance of the adsorbent is a key factor. The high-performance adsorbent can remarkably improve the water taking efficiency. The coordination polymer material is an effective pore material, and has the unique advantages of controllable and adjustable hydrophilicity, low desorption regeneration temperature and the like compared with the traditional adsorption materials of zeolite, silica gel and molecular sieve. Research and development of novel porous coordination polymer materials is becoming a hotspot in the field of water intake from air.
Disclosure of Invention
The invention provides a coordination polymer material, a preparation method and application thereof. The coordination polymer material can quickly adsorb moisture in air in a low-humidity environment with the air humidity of 20-30%. The adsorbed water is volatilized from the coordination polymer lattice and is condensed into liquid water by the high temperature generated by the solar heat collector, thereby realizing small-scale air water intake.
The coordination polymer material of the invention is [ Cd (1, 3-bdc) (3, 3' -tpcb) 0.5 ] n Wherein 3,3' -tpcb is 1,2,3, 4-tetra (3-pyridyl) cyclobutane, 1,3-bdc is 1, 3-phthalate, and n is a repeating unit number, which is any positive integer.
Wherein, the structural formulas of the 1,2,3, 4-tetra (3-pyridyl) cyclobutane and the 1, 3-phthalate are respectively as follows:
1,2,3, 4-tetra (3-pyridyl) cyclobutane
The coordination polymer material of the invention is a crystalline inorganic-organic hybrid material, belongs to triclinic system,
space group, unit cell parameter is->
α＝112.88(3)°，β＝90.29(3)°，γ＝103.76(3)°。
The preparation method of the coordination polymer material comprises the following steps:
step 1: placing 1, 2-di (3-pyridyl) ethylene, 1, 3-phthalic acid, tetrahydrate cadmium nitrate and deionized water into a polytetrafluoroethylene reaction kettle, sealing the reaction kettle, reacting at high temperature and high pressure, and slowly cooling to room temperature after the reaction is finished to obtain colorless blocky crystals [ Cd (1, 3-bdc) (3, 3' -bpe)] n Filtering, washing, airing and collecting the blocky crystals.
In step 1, the structural formula of 1, 2-bis (3-pyridyl) ethylene is shown as follows:
in step 1, bulk Crystal [ Cd (1, 3-bdc) (3, 3' -bpe)] n The unit cell parameters of (2) are:
α＝114.07(3)°，β＝91.09(3)°，γ＝102.82(3)°。
step 2: the bulk crystal obtained in the step 1 is irradiated under sunlight, and the photo-catalytic cycloaddition reaction is carried out to generate [ Cd (1, 3-bdc) (3, 3' -tpcb) 0.5 (H 2 O)] n 。[Cd(1,3-bdc)(3,3'-tpcb) 0.5 (H 2 O)] n The unit cell parameters are:
α＝64.85(3)°，β＝87.73(3)°，γ＝75.14(3)°。
step 3: heating the colorless bulk crystal obtained in the step 2 to 120 ℃ to remove water molecules in the pore canal, thereby obtaining a coordination polymer material [ Cd (1, 3-bdc) (3, 3' -tpcb) 0.5 ] n 。
In [ Cd (1, 3-bdc) (3, 3' -bpe)] n Wherein adjacent olefinic bonds are arranged in parallel, and the distance between the olefinic bonds is as follows
Conforming to the theory of the alkene light cycloaddition reaction proposed by Schmidt: the olefinic bonds in adjacent olefinic molecules are arranged in parallel, and the distance between adjacent olefinic bonds is within +.>
The olefin can exhibit photoreactivity. Ordered regular arrangement of atoms, close packing, small atom-to-atom gaps, coordination polymer [ Cd (1, 3-bdc) (3, 3' -bpe)] n Does not absorb water. Will [ Cd (1, 3-bdc) (3, 3' -bpe)] n And the two adjacent 1, 2-di (3-pyridyl) ethylene are placed under the irradiation of sunlight to perform addition reaction to generate 1,2,3, 4-tetra (3-pyridyl) cyclobutane (shown below). After the photocatalytic addition reaction, atoms are obviously displaced, two adjacent ethylene molecules are close to each other, and tiny gaps (pores occupy about 4% of coordination polymer unit cells) are formed in the molecules. The material absorbs water molecules in the air and forms hydrogen bonds with the water molecules. The bond lengths of the two hydrogen bonds are respectively: />
And
the coordination polymer material is applied to an air water taking device as an adsorption material to realize the adsorption and collection of liquid water from air.
In the present invention, a coordination polymer material [ Cd (1, 3-bdc) (3, 3' -tpcb) 0.5 ] n Placing in a low humidity environment with air humidity of 20% -30% for 10 min, and absorbing water in the environment to generate [ Cd (1, 3-bdc) (3, 3' -tpcb) 0.5 (H 2 O)] n . The water adsorbed by the coordination polymer is volatilized by heating through the solar heat collector and is condensed into liquid water, so that domestic small-scale air circulation water taking is realized.
The preparation method disclosed by the invention is simple to operate, good in repeatability and high in product yield.
Drawings
FIG. 1 is [ Cd (1, 3-bdc) (3, 3' -bpe)] n Is a crystal structure diagram of (a).
FIG. 2 is [ Cd (1, 3-bdc) (3, 3' -tpcb) 0.5 (H 2 O)] n Is a crystal structure diagram of (a).
FIG. 3 is [ Cd (1, 3-bdc) (3, 3' -tpcb) 0.5 ] n Is a crystal structure diagram of (a).
Detailed Description
Non-limiting examples are described as follows:
1、[Cd(1,3-bdc)(3,3'-bpe)] n is synthesized by (a)
1.82g (10 mmol) of 1, 2-bis (3-pyridyl) ethylene, 1.66g (10 mmol) of 1, 3-phthalic acid, 3.08g (10 mmol) of cadmium nitrate tetrahydrate and 50mL of deionized water are placed in a polytetrafluoroethylene reaction kettle with a volume of 100 mL; sealing the reaction kettle, and placing the reaction kettle in a constant-temperature drying oven at 170 ℃ for high-temperature and high-pressure reaction for 12 hours; after the reaction is finished, slowly cooling to room temperature to obtain colorless blocky crystals, filtering, washing, airing and collecting blocky crystals. Yield: 3.31g, yield: 72%.
[Cd(1,3-bdc)(3,3'-bpe)] n Part of the crystallographic parameters of (a): c (C) 20 H 14 CdN 2 O 4 ,M r ＝458.74,triclinic,
α＝114.07(3)°,β＝91.09(3)°,γ＝102.82(3)°,/>
Z＝2,D c ＝1.785g·cm -3 ,μ＝1.310mm -1 ,R 1 ＝0.0184,wR 2 ＝0.0481,S＝1.131。
[Cd(1,3-bdc)(3,3'-bpe)] n The single crystal structure of (2) is shown in FIG. 1.
2、[Cd(1,3-bdc)(3,3'-tpcb) 0.5 (H 2 O)] n Is synthesized by (a)
Will [ Cd (1, 3-bdc) (3, 3' -bpe)] n (2.29 g,5 mmol) was placed in a 15cm diameter petri dish and spread out. The dishes were exposed to sunlight. After 2 hours, samples were collected. Yield: 2.38g, yield: 100%.
[Cd(1,3-bdc)(3,3'-tpcb) 0.5 (H 2 O)] n Part of the crystallographic parameters of (a): c (C) 20 H 16 CdN 2 O 5 ,M r ＝476.75,Triclinic,
α＝64.85(3)°,β＝87.73(3)°,γ＝75.14(3)°,/>
Z＝2,D c ＝1.750g·cm -3 ,μ＝1.242mm -1 ,R 1 ＝0.0254,wR 2 ＝0.0713,S＝1.119。
[Cd 2 (1,3-bdc) 2 (3,3’-tpcb)(H 2 O) 2 ] n The single crystal structure of (2) is shown in FIG. 2.
3、[Cd(1,3-bdc)(3,3'-tpcb) 0.5 ] n Is synthesized by (a)
Will [ Cd (1, 3-bdc) (3, 3' -tpcb) 0.5 (H 2 O)] n (2.38 g,5 mmol) was placed in an open reaction flask, which was placed in a vacuum oven at 120 ℃. After 1 hour, the reaction flask was taken out of the drying oven and immediately sealed, and cooled to room temperature to obtain [ Cd (1, 3-bdc) (3, 3' -tpcb) 0.5 ] n . Yield: 2.29g, yield: 100%.
[Cd(1,3-bdc)(3,3'-tpcb) 0.5 ] n Part of the crystallographic parameters of (a): c (C) 20 H 14 CdN 2 O 4 ,M r ＝458.74,Triclinic,
α＝112.88(3)°,β＝90.29(3)°,γ＝103.76(3)°,/>
Z＝2,D c ＝1.741g·cm -3 ,μ＝1.277mm -1 ,R 1 ＝0.0211,wR 2 ＝0.0533,S＝1.183。/>
4、[Cd(1,3-bdc)(3,3'-tpcb) 0.5 ] n Is used for studying the air water taking property
10g of a coordination polymer material [ Cd (1, 3-bdc) (3, 3' -tpcb) 0.5 ] n The materials were weighed at 1 minute intervals in a constant temperature and humidity box with a humidity of 20% and a temperature of 25 ℃. After 10 minutes, the mass of the material did not increase. The weighing result showed that the mass of 10g of the coordination polymer was increased by 0.4g after water absorption, and the water absorption was about 4% of its own weight. The material absorbs moisture in low-humidity air through X-ray single crystal diffraction to generate [ Cd (1, 3-bdc) (3, 3' -tpcb) 0.5 (H 2 O)] n 。
Claims (7)
1. A coordination polymer material characterized by:
the coordination polymer material is [ Cd (1, 3-bdc) (3, 3' -tpcb) 0.5 ] n Wherein 3,3' -tpcb is 1,2,3, 4-tetra (3-pyridyl) cyclobutane, 1,3-bdc is 1, 3-phthalate, and n is a repeating unit number, which is any positive integer.
2. The coordination polymer material of claim 1, wherein:
the coordination polymer material is a crystalline inorganic-organic hybrid material, belongs to a triclinic system, is P ī space group, and has unit cell parameters of
α＝112.88(3)°，β＝90.29(3)v，γ＝103.76(3)°。
3. A method of preparing the coordination polymer material of claim 1 or 2, comprising the steps of:
step 1: placing 1, 2-di (3-pyridyl) ethylene, 1, 3-phthalic acid, tetrahydrate cadmium nitrate and deionized water into a polytetrafluoroethylene reaction kettle, sealing the reaction kettle, reacting at high temperature and high pressure, and slowly cooling to room temperature after the reaction is finished to obtain colorless blocky crystals [ Cd (1, 3-bdc) (3, 3' -bpe)] n Filtering, washing, airing and collecting blocky crystals;
step 2: the bulk crystal obtained in the step 1 is irradiated under sunlight to generate photocatalysis cycloaddition reaction, and the product is generated
[Cd(1,3-bdc)(3,3'-tpcb) 0.5 (H 2 O)] n ；
Step 3: heating the colorless bulk crystal obtained in the step 2 to 120 ℃ to remove water molecules in the pore canal, thereby obtaining a coordination polymer material [ Cd (1, 3-bdc) (3, 3' -tpcb) 0.5 ] n 。
4. A method of preparation according to claim 3, characterized in that:
in step 1, bulk Crystal [ Cd (1, 3-bdc) (3, 3' -bpe)] n The unit cell parameters of (2) are:
α＝114.07(3)°，β＝91.09(3)°，γ＝102.82(3)°。
5. a method of preparation according to claim 3, characterized in that:
in step 2, [ Cd (1, 3-bdc) (3, 3' -tpcb) 0.5 (H 2 O)] n The unit cell parameters of (2) are:
α＝64.85(3)°，β＝87.73(3)°，γ＝75.14(3)°。
6. use of the coordination polymer material according to claim 1 or 2, characterized in that:
the coordination polymer is used as an adsorption material to be applied to an air water taking device, so that water vapor is adsorbed from air and liquid water is collected.
7. The use according to claim 6, characterized in that:
coordination Polymer Material [ Cd (1, 3-bdc) (3, 3' -tpcb) 0.5 ] n Placing in a low humidity environment with air humidity of 20% -30% for 10 min, and absorbing water in the environment to generate [ Cd (1, 3-bdc) (3, 3' -tpcb) 0.5 (H 2 O)] n The method comprises the steps of carrying out a first treatment on the surface of the The water adsorbed by the coordination polymer is volatilized by heating through the solar heat collector and is condensed into liquid water, so that the air circulation water taking is realized.
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