Hydrogen bond covalent organic aerogel material HCMethod for synthesizing OA-3
1. Hydrogen bond covalent organic aerogel material HCA synthesis method of OA-3 comprises the following steps:
the method comprises the following steps: dissolving benzene-1, 3, 5-triacyl hydrazine in an organic solvent dimethyl sulfoxide, keeping the concentration of the solution at 0.04mol/L, and naming the solution as A;
step two: dissolving 1, 5-naphthalene disulfonic acid in the solution A, keeping the concentration of the solution at 0.12mol/L and naming the solution B as the solution B;
step three: 4, 4-biphenyl dicarboxaldehyde is dissolved in the solution B, the concentration of the solution B is kept to be 0.06mol/L, and the solution B is named as solution C;
the molar ratio of the solution C is as follows: benzene-1, 3, 5-trihydrazide: 1, 5-naphthalenedisulfonic acid: 4, 4-biphenyldicarbaldehyde ═ 2: 6: 3;
step four: placing the solution C in a constant-temperature oil bath pan, and heating and reacting at 100 ℃ for 30 minutes to obtain a bright yellow polymer;
step five: putting the bright yellow polymer obtained in the step four into a dialysis bag, taking distilled water as dialysate, removing the organic solvent, and taking out after obvious layering appears in the dialysis bag after 2-3 days to obtain an obtained product;
step six: pouring the obtained substance obtained in the fifth step into a beaker, freezing at low temperature, and then freeze-drying to obtain the hydrogen bond covalent organic aerogel material HCOA-3。
Background
Covalent Organic Polymers (COPs), an emerging porous covalent organic material, are linked by stable covalent bonds. It has received attention due to its characteristics of stable structure, high specific surface area, large porosity, modifiable structure and easy functionalization and is widely used in the fields of energy, medicine and environment. COPs are generally constructed by two types of monomers through one covalent bond, which severely limits the structural complexity and functional diversity, and the preparation of novel COPs with multifunctional structures is a problem to be solved urgently.
The invention prepares the three-component hydrogen bond covalent organic aerogel H by a simple solvothermal methodCOA-3. The advantages are that: (1) introducing aromatic hydrocarbon with sulfonic acid group to synthesize HCOA-3 has active sites of hydrogen bond action while having the advantages of covalent bond, and the existence of the hydrogen bond is favorable for increasing HCAdsorption properties of OA-3; (2) the dipole-dipole interaction caused by the polarization of oxygen and sulfur atoms allows the H producedCOA-3 has higher adsorption affinity; (3) the combined action of the hydrogen bond and the covalent bond breaks through the limitation of a single covalent bond, and provides more possibility for constructing COPs materials with multi-level sub-pore channels.
Disclosure of Invention
The invention aims to provide a hydrogen bond covalent organic aerogel HCA synthesis method of OA-3 comprises the following steps:
the method comprises the following steps: dissolving benzene-1, 3, 5-triacyl hydrazine in an organic solvent dimethyl sulfoxide, keeping the concentration of the solution at 0.04mol/L, and naming the solution as A;
step two: dissolving 1, 5-naphthalene disulfonic acid in the solution A, keeping the concentration of the solution at 0.12mol/L and naming the solution B as the solution B;
step three: 4, 4-biphenyl dicarboxaldehyde is dissolved in the solution B, the concentration of the solution B is kept to be 0.06mol/L, and the solution B is named as solution C;
the molar ratio of the solution C is as follows: benzene-1, 3, 5-trihydrazide: 1, 5-naphthalenedisulfonic acid: 4, 4-biphenyldicarbaldehyde ═ 2: 6: 3;
step four: placing the solution C in a constant-temperature oil bath pan, and heating and reacting at 100 ℃ for 30 minutes to obtain a bright yellow polymer;
step five: putting the bright yellow polymer obtained in the step four into a dialysis bag, taking distilled water as dialysate, removing the organic solvent, and taking out after obvious layering appears in the dialysis bag after 2-3 days to obtain an obtained product;
step six: pouring the obtained substance obtained in the fifth step into a beaker, freezing at low temperature, and then freeze-drying to obtain the hydrogen bond covalent organic aerogel material HCOA-3。
The invention has the beneficial effects that:
the hydrogen bond covalent organic polymer material H obtained by the synthetic method of the inventionCOA-3 has high chemical stability, simple synthesis method, multi-level pore channels, rich functional groups and shape plasticity.
Drawings
FIG. 1 is H of the present inventionCA schematic for the synthesis of OA-3;
FIG. 2 is H synthesized according to the present inventionCA powder X-ray diffraction pattern of OA-3;
FIG. 3 is H synthesized according to the present inventionCScanning electron micrographs of OA-3;
FIG. 4 is H synthesized by the present inventionCFourier transform-infrared spectrogram of OA-3;
FIG. 5 is H synthesized according to the present inventionCThermogravimetric curves of OA-3 under nitrogen atmosphere;
FIG. 6 is H synthesized by the present inventionCNitrogen desorption curve of OA-3;
FIG. 7 is H synthesized by the present inventionCX-ray photoelectron spectroscopy analysis of OA-3.
Detailed Description
Synthesis of HCThe starting materials used for OA-3 are all commercially available products.
As shown in figure 1, a hydrogen-bonded covalent organic polymer material HCA synthesis method of OA-3 comprises the following steps:
the method comprises the following steps: dissolving benzene-1, 3, 5-triacyl hydrazine in an organic solvent dimethyl sulfoxide, keeping the concentration of the solution at 0.04mol/L, and naming the solution as A;
step two: dissolving 1, 5-naphthalene disulfonic acid in the solution A, keeping the concentration of the solution at 0.12mol/L and naming the solution B as the solution B;
step three: 4, 4-biphenyl dicarboxaldehyde is dissolved in the solution B, the concentration of the solution B is kept to be 0.06mol/L, and the solution B is named as solution C;
the molar ratio of the solution C is as follows: benzene-1, 3, 5-trihydrazide: 1, 5-naphthalenedisulfonic acid: 4, 4-biphenyldicarbaldehyde ═ 2: 6: 3;
step four: placing the solution C in a constant-temperature oil bath pan, and heating and reacting at 100 ℃ for 30 minutes to obtain a bright yellow polymer;
step five: putting the bright yellow polymer obtained in the step four into a dialysis bag, taking distilled water as dialysate, removing the organic solvent, and taking out after obvious layering appears in the dialysis bag after 2-3 days to obtain an obtained product;
step six: pouring the obtained substance obtained in the fifth step into a beaker, freezing at low temperature, and then freeze-drying to obtain the hydrogen bond covalent organic aerogel material HCOA-3。
H synthesized by the inventionCThe powder X-ray diffraction pattern of OA-3 is shown in FIG. 2.
H synthesized by the inventionCA scanning electron micrograph of OA-3 is shown in FIG. 3.
H synthesized by the inventionCThe Fourier transform-infrared spectrum of OA-3 is shown in FIG. 4.
H synthesized by the inventionCThe thermogravimetric curve of OA-3 in a nitrogen atmosphere is shown in the figure5, respectively.
H synthesized by the inventionCThe nitrogen desorption curve of OA-3 is shown in FIG. 6.
H synthesized by the inventionCThe X-ray photoelectron spectroscopy analysis of OA-3 is shown in FIG. 7.