Preparation method of nano organic porous material
By mixing 1,3,5-triazine-2,4,6-triformaldehyde and TAPP in solution and heating reaction at room temperature, nano-organic porous materials with excellent CO2 and iodine steam adsorption properties were prepared, which solved the shortcomings of existing materials in adsorption properties and showed wide application prospects.
Patent Information
- Application Number
- CN202411871777.5
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-12-18
- Publication Date
- 2025-06-27
AI Technical Summary
There is room for improvement in the adsorption performance of existing nano-organic porous materials in CO2 and iodine steam, especially in terms of nitrogen content and microporous structure.
1,3,5-triazine-2,4,6-triformaldehyde and TAPP were mixed in ortho-dichlorobenzene solution at room temperature, glacial acetic acid was added as a catalyst, and the reaction was carried out at 80-120°C for 3-5 days to obtain nano-organic porous material. The material has a microporous structure and nitrogen-rich active site, enhancing its adsorption capacity of CO2 and iodine steam.
The prepared nano-organic porous materials show excellent CO2 and iodine steam adsorption capabilities and have a wide range of applications.
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Abstract
Description
Technical Field
[0001] The present invention relates to the technical field of porous materials, and particularly relates to a preparation method of a nano-organic porous material. Background Art
[0002] Organic porous materials are a class of porous materials composed of organic structural units, mainly including porous organic cages (POCs) and porous organic polymers (POPs). The diversity of structural units and easy modifiability endow these materials with unique structural designability and multifunctionality, showing good application potential in many fields such as gas storage, catalysis, energy environment, etc.
[0003] The Liao research group first synthesized three nitrogen-rich conjugated microporous materials (NCMPs) with structures similar to traditional polyaniline by chemical oxidative polymerization of multi-connected aniline precursors. The nitrogen content in NCMPs is as high as 11.84 wt%, its ultramicroporosity is less than 1 nm, and the specific surface area reaches 485 m 2 g -1 ². It was found through research that NCMPs have excellent CO₂ adsorption performance. The experimental results show that the CO₂ absorption amount is 11 wt%, the H₂ storage amount is 1.0 wt%, and the iodine vapor absorption amount under ambient pressure is 215 wt%. This research indicates that the porous structure and nitrogen content in nano-organic porous materials affect the CO₂ adsorption performance. On this basis, the present invention provides another nitrogen-containing nano-organic porous material. Summary of the Invention
[0004] 1. Technical problems to be solved: In view of the above technical problems, the present invention provides a preparation method of a nano-organic porous material.
[0005] 2. Technical solution: A preparation method of a nano-organic porous material includes the following steps: Dissolve 1,3,5-triazine-2,4,6-tricarbaldehyde and TAPP in o-dichlorobenzene to form solutions at room temperature, mix the two solutions evenly according to the molar ratio of 1,3,5-triazine-2,4,6-tricarbaldehyde to TAPP being 4:3, then add glacial acetic acid as a catalyst, react at 80 - 120 °C for 3 - 5 d, obtain a solid after the reaction, and dry the solid after washing to obtain the nano-organic porous material.
[0006] Further, the structural formula of the TAPP is as follows: .
[0007] Further, the structural formula of 1,3,5-triazine-2,4,6-tricarbaldehyde is as follows: .
[0008] Further, the concentration of the solution prepared from 1,3,5-triazine-2,4,6-tricarbaldehyde and TAPP in ortho-dichlorobenzene is 0.1 - 0.3 mol / L.
[0009] Further, the reaction temperature is preferably 100 - 120 °C.
[0010] Further, the solid obtained after the reaction is washed three times with DMF and THF successively, and then dried at 80 - 100 °C for 12 - 24 h.
[0011] 3. Beneficial effects: The present invention provides a preparation method of a nano-organic porous material. The synthesized nano-organic porous material has a microporous structure, and there are a large number of nitrogen-rich active sites on the surface and pore walls of the material skeleton. It has excellent iodine vapor adsorption capacity and CO2 adsorption capacity, and has a wide application prospect. Specific embodiments
[0012] The present invention will be specifically described below.
[0013] Example 1: A preparation method of a nano-organic porous material, comprising the following steps: At room temperature, 16.5 mg of 1,3,5-triazine-2,4,6-tricarbaldehyde and 50.6 mg of TAPP are respectively dissolved in ortho-dichlorobenzene to form 0.1 mol / L solutions. Then the two solutions are mixed evenly, and glacial acetic acid is added as a catalyst. The reaction is carried out at 80 °C for 5 d. After the reaction, a solid is obtained. The solid is washed three times with DMF and THF successively, and then dried at 80 °C for 18 h to obtain the nano-organic porous material.
[0014] Example 2: A preparation method of a nano-organic porous material, comprising the following steps: At room temperature, 16.5 mg of 1,3,5-triazine-2,4,6-tricarbaldehyde and 50.6 mg of TAPP are respectively dissolved in ortho-dichlorobenzene to form 0.1 mol / L solutions. Then the two solutions are mixed evenly, and glacial acetic acid is added as a catalyst. The reaction is carried out at 100 °C for 5 d. After the reaction, a solid is obtained. The solid is washed three times with DMF and THF successively, and then dried at 80 °C for 18 h to obtain the nano-organic porous material.
[0015] Example 3: A preparation method of a nano-organic porous material, comprising the following steps: Dissolve 16.5 mg of 1,3,5-triazine-2,4,6-tricarbaldehyde and 50.6 mg of TAPP in ortho-dichlorobenzene to form 0.1 mol / L solutions respectively at room temperature, then mix the two solutions evenly, add glacial acetic acid as a catalyst, react at 120 °C for 5 d, obtain a solid after the reaction, wash the solid three times with DMF and THF successively, and then dry at 80 °C for 18 h to obtain the nano-organic porous material.
[0016] Example 4: A preparation method of a nano-organic porous material, comprising the following steps: Dissolve 16.5 mg of 1,3,5-triazine-2,4,6-tricarbaldehyde and 50.6 mg of TAPP in ortho-dichlorobenzene to form 0.2 mol / L solutions respectively at room temperature, then mix the two solutions evenly, add glacial acetic acid as a catalyst, react at 100 °C for 5 d, obtain a solid after the reaction, wash the solid three times with DMF and THF successively, and then dry at 80 °C for 18 h to obtain the nano-organic porous material.
[0017] Example 5: A preparation method of a nano-organic porous material, comprising the following steps: Dissolve 16.5 mg of 1,3,5-triazine-2,4,6-tricarbaldehyde and 50.6 mg of TAPP in ortho-dichlorobenzene to form 0.3 mol / L solutions respectively at room temperature, then mix the two solutions evenly, add glacial acetic acid as a catalyst, react at 100 °C for 5 d, obtain a solid after the reaction, wash the solid three times with DMF and THF successively, and then dry at 80 °C for 18 h to obtain the nano-organic porous material.
[0018] Test example: The iodine adsorption and capture experiment is mainly measured by the mass method. The steps for iodine capture are as follows: Weigh a certain mass (about 20 mg) of the nano-organic porous material sample and put it into a 2 mL open glass bottle, then place the glass bottle into another wide-mouth bottle containing 500 mg of iodine, and seal it after placement. After heating the whole device at 85 °C for a period of time, iodine sublimes and is adsorbed by the internal organic porous material. Take out the internal sample bottle and weigh it at regular intervals to calculate the adsorption amount. The iodine capture value in the sample is calculated according to formula (1): α = (m2 - m1) / m1 (1).
[0019] In the formula: α is the adsorption capacity; m1 and m2 are the masses of the material before and after adsorbing iodine.
[0020] During the 60-hour iodine vapor adsorption process of the nano-organic porous materials prepared in Examples 1-5, the maximum adsorption amounts were 1.8 g / g, 2.1 g / g, 2.2 g / g, 2.0 g / g, and 2.3 g / g, respectively. The nano-organic porous materials have a microporous structure, which increases the iodine adsorption area. Moreover, due to the large number of nitrogen-rich active sites on the surface and pore walls of the material skeleton, the adsorption force between iodine and the material is enhanced, so iodine can be captured quickly and efficiently.
[0021] The CO2 adsorption capacity was further tested. The adsorption amounts of the nano-organic porous materials prepared in Examples 1-5 at 273 K and 100 KPa were 55.6 3 .g -1 , 63.1 cm 3 .g -1 , 65.7 cm 3 .g -1 , 64.1 cm 3 .g -1 and 66.3 cm 3 .g -1 .
[0022] Although the present invention has been disclosed above with preferred embodiments, they are not used to limit the present invention. Any person skilled in this art can make various changes or modifications without departing from the spirit and scope of the present invention. Therefore, the protection scope of the present invention should be defined by the protection scope of the claims of this application.
Claims
1. A method for preparing a nano-organic porous material, characterized in that: The following steps are involved: Under room temperature conditions, 1,3,5-triazine-2,4,6-tricarboxaldehyde and TAPP are respectively dissolved in o-dichlorobenzene to form solutions, the two solutions are evenly mixed according to a molar ratio of 1,3,5-triazine-2,4,6-tricarboxaldehyde to TAPP of 4:3, glacial acetic acid is added as a catalyst, and the reaction is carried out at 80-120° C. for 3-5 days to obtain a solid after the reaction, and the solid is washed and dried to obtain the nano organic porous material.
2. The method for preparing a nano-organic porous material according to claim 1, characterized in that: The structural formula of TAPP is as follows: 。 3. The method for preparing a nano-organic porous material according to claim 1, characterized in that: The structural formula of the 1,3,5-triazine-2,4,6-tricarbaldehyde is as follows: 。 4. The method for preparing a nano-organic porous material according to any one of claims 1 to 3, characterized in that: The concentration of the solution prepared by using o-dichlorobenzene for 1,3,5-triazine-2,4,6-tricarbaldehyde and TAPP is 0.1-0.3 mol / L.
5. The method for preparing a nano-organic porous material according to claim 4, characterized in that: The reaction temperature is preferably 100-120°C.
6. The method for preparing a nano-organic porous material according to claim 5, characterized in that: The solid obtained after the reaction was washed three times with DMF and THF, and then dried at 80-100° C. for 12-24 h.