Preparation method of two-acid catalytic synthesis of light-colored o-cresol-formaldehyde resin
A phenolic resin, acid-catalyzed technology, applied in the field of phenolic resin polymer synthesis, to achieve the effects of reducing chromaticity, controllable softening point, and increasing reaction rate
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Embodiment 1
[0025] Fill the 1000mL three-port reactor with nitrogen through repeated evacuation-nitrogen filling, then add 200g of o-cresol and 135g of 37% formaldehyde solution into the reaction vessel, heat to 40°C, use mechanical stirring to dissolve the o-cresol and mix evenly to obtain a transparent The reaction solution. Under the condition of nitrogen protection, a mixed organic acid catalyst (3 g of solid oxalic acid, 1 g of formic acid) was added to the reaction solution at normal pressure, the reaction temperature was controlled at 90 ° C, and the reaction was heated under reflux for 2 hours to obtain a milky white polymer solution. Under a nitrogen atmosphere, an inorganic acid catalyst (2.5 g of concentrated hydrochloric acid with a concentration of 37%) was added, and the reaction temperature was controlled at 90° C. to continue the reaction for 4 hours to obtain a milky white viscous liquid. Add organic solvent methyl isobutyl ketone, whose volume is 5 times the volume of th...
Embodiment 2
[0028] Fill the 1000mL three-port reactor with nitrogen through repeated evacuation-nitrogen filling, then add 210g of o-cresol and 150g of 37% formaldehyde solution into the reaction vessel, heat to 60°C and use mechanical stirring to dissolve the o-cresol and mix evenly to obtain a transparent reaction liquid. Under the condition of nitrogen protection, 6 g of solid oxalic acid was added to the reaction solution at normal pressure, the reaction temperature was controlled at 90° C., and the reaction was heated under reflux for 4 hours to obtain a milky white polymer solution. Then add 4 g of phosphoric acid mineral acid catalyst, and control the reaction temperature at 90° C. to continue the reaction for 4 hours to obtain a milky white viscous liquid. Add toluene as an organic solvent, whose volume is three times the volume of the milky white viscous liquid, to dissolve the crude resin product; then use a multi-stage series centrifugal extractor to extract and wash the crude ...
Embodiment 3
[0031] Fill the 1000mL three-port reactor with nitrogen through repeated evacuation-nitrogen filling, then add 160g of o-cresol and 126g of 37% formaldehyde solution into the reactor, heat to 60°C to dissolve the o-cresol and mix evenly to obtain a transparent reaction solution. Under the condition of nitrogen protection, 4g of formic acid was added to the reaction solution at normal pressure, the reaction temperature was controlled at about 100°C, and the reaction was heated to reflux for 3 hours. Under nitrogen atmosphere, 4.8g of 20% hydrochloric acid solution was slowly added dropwise. The reaction was continued at 100°C for 4 hours to obtain a milky white viscous liquid. Add cyclohexanone organic solvent, whose volume is 5 times the volume of milky white viscous liquid, so that the crude resin product is dissolved. The crude resin solution was extracted and washed with a multi-stage series centrifugal extractor, 200 mL of deionized water was added, and washed with water a...
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