Preparation method of ultrahigh molecular weight phenolic resin
An ultra-high molecular weight, phenolic resin technology, applied in the field of preparation of ultra-high molecular weight phenolic resin, can solve the problems of high raw material ratio, easy gelation, difficult control of the production process, etc., and achieves mild conditions, reasonable molecular weight distribution, and process Simple to use effects
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Embodiment 1
[0023] Embodiment 1 phenol / formaldehyde / hydrochloric acid
[0024] 500g of phenol, 350g of formaldehyde (37wt%), and 1.5g of hydrochloric acid (20wt%) were added to a stirring 1000ml four-necked flask with a condenser and mixed. Heat up to boiling reflux, react for 3 hours, heat up to 110°C for dehydration reaction, then cool down to 90°C, add 39g of formaldehyde (37wt%), 0.5g of hydrochloric acid (20wt%), and then reflux for reaction. When the melt viscosity of the resin reaches 3500MPa·s / 100°C, add 0.5g of sodium hydroxide, the pH of the resin reaches 6.4, and then continue to heat up and dehydrate until the temperature reaches 160°C to obtain ultra-high molecular weight phenolic resin. The resin has a number average molecular weight Mn of 1100 and a weight average molecular weight Mw of 14899. The softening point is 124°C, and the free phenol is 4.5%.
Embodiment 2
[0025] Embodiment 2 phenol / formaldehyde / sulfuric acid
[0026] Change hydrochloric acid into the sulfuric acid of 20wt%, other is the same as embodiment 1, still can obtain the phenolic resin of ultrahigh molecular weight. The number average molecular weight Mn of the resin is 1200, the weight average molecular weight Mw is 19980; the softening point is 130° C., and the free phenol is 4.3%.
Embodiment 3
[0027] Embodiment 3 cresol / formaldehyde / oxalic acid
[0028] 400g of cresol, 230g of formaldehyde (37wt%), 2.8g of oxalic acid (20wt%) were added to a 1000ml four-neck flask with a condenser and mixed. Heat up to boiling reflux, react for 3 hours, heat up to 110°C for dehydration reaction, then cool down to 95°C, add 25g of formaldehyde (37wt%), 0.5g of hydrochloric acid (20wt%), and then reflux for reaction. When the melt viscosity of the resin reaches 4500MPa·s / 100°C, add 0.9g of potassium hydroxide, the pH of the resin reaches 6, and then continue to heat up and dehydrate until the temperature reaches 160°C to obtain ultra-high molecular weight phenolic resin. The number average molecular weight Mn of the resin is 1350, and the weight average molecular weight Mw is 25400. Softening point 135°C, free cresol 4%.
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