Method for preparing high-ortho thermoplastic phenolic resin
A phenolic resin and thermoplastic technology, which is applied in the field of preparation of high-ortho-position thermoplastic phenolic resins, can solve the problems of unfavorable industrial production of thermoplastic high-ortho-position phenolic resins, increase production costs, and high requirements for equipment conditions, and achieve high-temperature reactions and easy gelation Curing, reducing the requirements for production equipment, and stabilizing the reaction process
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Embodiment 1
[0026] Put phenol and formaldehyde into the reactor according to the molar ratio of 1:0.72, add the catalyst zinc acetate according to 0.7% of the mass of phenol, then add the catalyst oxalic acid, the mass of oxalic acid is 0.3% of the phenol, stir and heat to 70°C and at this temperature Keep it under low temperature for 1 hour, then heat up to 100°C and boil and reflux for 5 hours; start distillation and dehydration after the reaction is completed, and continue heating and heating after the temperature rises to 110°C to stabilize for 1.5 hours, and finally vacuum dehydration at 150°C ~ 160°C Phenol, when the negative pressure reaches 0.97MPa, it can be discharged after 1 hour of dephenolization.
[0027] According to HG5 1342, measure the free phenol content in the phenolic resin, the free phenol content of the thermoplastic resin obtained by the above method is 2.1% after testing; the resin molecular weight (Mw) is 4415; the ortho-to-para ratio obtained from the infrared tr...
Embodiment 2
[0029] Put phenol and formaldehyde into the reaction kettle according to the molar ratio of 1:0.70, add catalyst zinc acetate according to 0.7% of the mass of phenol, then add catalyst oxalic acid, the mass of oxalic acid is 0.3% of phenol, stir and heat to 70°C Keep at low temperature for 1 hour, then heat up to 100°C and boil and reflux for 3 hours; start distillation and dehydration after the reaction is completed, and heat up after the temperature rises to 120°C to stabilize for 1 hour. When the temperature reaches 150°C-160°C, vacuum dehydration Phenol, when the negative pressure reaches 0.97MPa, it can be discharged after 1 hour of dephenolization.
[0030] According to HG5 1342, the free phenol content in the phenolic resin is measured, and the free phenol content of the thermoplastic resin obtained by the above method is about 2.3% after testing; the molecular weight of the resin is 3951; the ortho-to-para ratio obtained from the infrared transmission spectrum is 6: 1; ...
Embodiment 3
[0032] Put phenol and formaldehyde into the reactor according to the molar ratio of 1:0.68, add the catalyst zinc acetate according to 0.7% of the mass of phenol, then add the catalyst oxalic acid, the mass of oxalic acid is 0.3% of the phenol, stir and heat to 70°C and at this temperature Keep it under low temperature for 1 hour, then heat up to 100°C and boil and reflux for 4 hours; start distillation and dehydration after the reaction is completed, when the temperature rises to 130°C, stabilize the temperature for 0.5 hours and then heat up, when the temperature reaches 150°C, vacuum dephenolization can be done , When the negative pressure reaches 0.97MPa, it can be discharged after 0.5 hours of dephenolization.
[0033] Measure free phenol content in phenolic resin according to HG5 1342, the free phenol content of the thermoplastic resin obtained by the above method is about 2.1% after testing; the resin molecular weight is 3320; the ortho-para ratio obtained from infrared ...
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