Porous adsorption material based on reutilization of alcohol-soluble waste in production process of polyphenyl ether and synthesis method of porous adsorption material
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A porous adsorption material and production process technology, applied in separation methods, other chemical processes, chemical instruments and methods, etc., can solve the problems of easily polluting the environment, increasing the toxicity of asphalt, etc., achieving large micropore volume, excellent performance, high ratio The effect of surface area
Active Publication Date: 2022-05-03
ZHEJIANG UNIV OF TECH
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However, the most toxic part of asphalt that pollutes water is phenols, adding phenols to asphalt will increase the toxicity of asphalt and make it more likely to pollute the environment
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Embodiment 1
[0027] Add purification waste (1g), 1,2-dichloroethane (20ml), anhydrous ferric chloride (1.3517g, 0.0083mol) to the reactor in turn, stir until fully dissolved, then add p-dichlorobenzyl (0.7294 g, 0.0042 mol), nitrogen-vacuum pumping 3 times, nitrogen bubbling for 15 min, and reacting at 60°C for 12 hours.
[0028] After the reaction, the brown solid product was obtained by suction filtration under reduced pressure, washed with methanol three times, and extracted with methanol in a Soxhlet extractor for 24 hours. Finally, vacuum-dry at 80°C for 24 hours to obtain the final product.
Embodiment 2
[0030] Add purification waste (1g), 1,2-dichloroethane (20ml), anhydrous ferric chloride (6.7583g, 0.0417mol) to the reactor in turn, stir until fully dissolved, then add p-dichlorobenzyl (3.6471 g, 0.0208 mol), nitrogen-vacuum pumping 3 times, nitrogen bubbling for 15 minutes, and reacting at 80°C for 36 hours.
[0031] After the reaction, the brown solid product was obtained by suction filtration under reduced pressure, washed with methanol three times, and extracted with methanol in a Soxhlet extractor for 24 hours. Finally, vacuum dry at 80°C for 24h to obtain the final product
Embodiment 3
[0033] Add purification waste (1g), 1,2-dichloroethane (20ml), anhydrous ferric chloride (4.055g, 0.025mol) to the reactor in turn, stir until fully dissolved, then add p-dichlorobenzyl (2.1883 g, 0.0125 mol), nitrogen gas-vacuum pumping 3 times, nitrogen gas bubbling for 15 min, and reaction at 80°C for 24 hours.
[0034] After the reaction, the brown solid product was obtained by suction filtration under reduced pressure, washed with methanol three times, and extracted with methanol in a Soxhlet extractor for 24 hours. Finally, vacuum-dry at 80°C for 24 hours to obtain the final product.
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Abstract
The invention discloses a porous adsorption material based on reutilization of alcohol-soluble waste in a polyphenyl ether production process and a synthesis method thereof, and the method comprises the following steps: dissolving the alcohol-soluble waste in the polyphenyl ether production process in a solvent, filtering to remove insoluble substances, evaporating out the solvent, and drying to obtain a recycled material; dissolving the recycled material in a reaction solvent, sequentially adding a cross-linking agent and a catalyst, carrying out stirring reaction in a nitrogen atmosphere, and carrying out reduced pressure suction filtration to obtain a solid product; and washing the solid product with a precipitant, extracting with the precipitant, and drying to obtain the porous adsorption material. The porous adsorption material is prepared by effectively utilizing industrial waste in production of polyphenyl ether, sustainable development is realized, the world environment is protected, and the cross-linking agent containing rigid structures such as benzene and naphthalene is adopted, so that the network structure of the porous adsorption material shows high rigidity, and the porous adsorption material has a relatively high specific surface area and a relatively large micropore volume; the material has excellent performance in the aspects of gas adsorption, separation and the like.
Description
technical field [0001] The invention belongs to the technical field of material preparation, and relates to a synthesis method for preparing porous adsorption materials based on the reuse of polyphenylene ether production engineering waste, specifically a method based on Friedel-Crafts alkylation to realize super-crosslinking, recycle poly Alcohol-soluble waste, one of the by-products in the production process of phenyl ether, is used to prepare porous adsorption materials. Background technique [0002] Polyphenylene ether has strong applicability in electronic appliances, automobile industry, engineering equipment, etc. due to its characteristics of non-toxic and harmless, low relative density, and excellent mechanical and electrical properties. In the existing polyphenylene ether production process, the last process is to precipitate the polymer with methanol. After the polyphenylene ether product is filtered and separated, the small amount of residual waste left in methan...
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