Preparation method of high-acid-content carbon-based solid acid
A technology of carbon-based solid acid and high acid content, which is applied in the preparation of carboxylic acid esters, the preparation of organic compounds, chemical instruments and methods, etc. It can solve the problems of poor thermal stability of carbon materials, low acid strength, and limited acid content. Achieve the effect of simple equipment, easy process, and extended industrial chain
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Embodiment approach 1
[0017] Take 20g of medium-temperature coal tar pitch, add 40ml of xylene, stir to dissolve, then add 50g of trichloroacetic acid and 60ml of 30% H 2 o 2 , ultrasonicated for 50 minutes at a temperature of 80°C, filtered and dried to obtain chlorinated coal tar pitch containing 20 wt% chlorine; then pulverized the chlorinated coal tar pitch, sieved 200 mesh (74 microns), and put it into a beaker , add 100g of concentrated sulfuric acid, place it in a heat-conducting oil bath, control the reaction temperature to 165°C, react for 12 hours, cool to room temperature, filter with a sand core funnel, and then wash the sulfonated product with distilled water until the pH of the filtrate is neutral In order to obtain a solid acid with a surface acid content of 7.3 mmol / g, it was dried in a drying oven at 110°C for 4 hours.
Embodiment approach 2
[0019] Take 20g of high-temperature coal tar pitch, add 60ml of xylene, stir to dissolve, then add 60g of dichloroacetic acid and 80ml of 30% H 2 o 2 , ultrasonicated for 60 minutes at a temperature of 90°C, filtered and dried to obtain chlorinated coal tar pitch containing 18.6 wt% chlorine; then crushed chlorinated coal tar pitch, sieved to 200 mesh (74 microns), and put into a beaker , add 172g of concentrated sulfuric acid, place it in a heat-conducting oil bath, control the reaction temperature to 170°C, react for 12 hours, cool to room temperature, filter with a sand core funnel, and then wash the sulfonated product with distilled water until the pH of the filtrate is neutral In order to obtain a solid acid with a surface acid content of 7.5 mmol / g, it was dried in a drying oven at 110°C for 4 hours.
Embodiment approach 3
[0021] Take 20g of high-temperature coal tar pitch, add 80ml of xylene, stir to dissolve, then add 50g of monochloroacetic acid and 100ml of 30% H 2 o 2 , ultrasonicated for 40 minutes at a temperature of 70°C, filtered and dried to obtain chlorinated coal tar pitch with a chlorine content of 19.5 wt%; then pulverized the chlorinated coal tar pitch, sieved to 200 mesh (74 microns), and put it into a beaker , add 149.0g concentrated sulfuric acid, place it in a heat conduction oil bath, control the reaction temperature to 170°C, react for 12 hours, cool to room temperature, filter with a sand core funnel, and then wash the sulfonated product with distilled water until the pH of the filtrate is Neutral, placed in a drying oven at 110 ° C for 4 hours to obtain a solid acid with a surface acid content of 7.3 mmol / g.
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