Production of modified phenolic resin with high boron content
A technology of phenolic resin and boron modification, applied in the field of materials, to achieve the effect of simple and easy preparation method and excellent thermal performance
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Embodiment 1
[0019] Step (1): According to the molar ratio of boric acid / phenol=1 / 3, 28.2g of phenol and 40ml of toluene solution were added into a four-necked flask equipped with a condenser, a thermometer, an electric stirrer and a thermocouple. Raise the temperature to 90°C, then add 6.2g of boric acid, and at the same time use 0.1mol / L NaOH solution to adjust the pH value of the solution in the four-necked flask. When the pH is between 6 and 8, make the solution react at a temperature range of 90°C , and vacuum dehydration at the same time, the reaction time is 3 hours, and the vacuum degree is 0.1-1KPa; when the liquid is clear and slightly orange, and no water is produced after long-term pumping, stop pumping.
[0020] Step (2) Add 10.2 g of paraformaldehyde with a molecular weight of 450, make it react at 100° C. while stirring, and dehydrate under reduced pressure. As the dehydration proceeds, the liquid in the reaction bottle gradually becomes viscous. After 3-4 hours of reaction,...
Embodiment 2
[0023] Embodiment 2: the mol ratio of the boric acid / phenol of embodiment 1 step (1) is changed into 1 / 2 by 1 / 3, by the mol ratio of boric acid / phenol=1 / 2, the phenol of 18.8g and 30ml ethanol solution Add it to a four-necked flask equipped with a condenser, a thermometer, an electric stirrer and a thermocouple. Raise the temperature to 60°C, then add 6.2g of boric acid, and at the same time adjust the pH value of the solution in the four-necked flask with 0.1mol / L potassium hydroxide solution. The reaction time is 6 hours, and the vacuum degree is 0.1-1KPa. When the liquid is clear and slightly orange, and when there is no water after long-term pumping, stop pumping.
[0024] Step (2) Add 10.2 g of paraformaldehyde with a molecular weight of 200, make it react at 80° C. while stirring, and dehydrate under reduced pressure. As the dehydration proceeds, the liquid in the reaction bottle gradually becomes viscous. After 5-6 hours of reaction, when it is yellow-green, stop the r...
Embodiment 3
[0025] Embodiment 3: the mol ratio of the boric acid / phenol of embodiment 1 step (1) is changed into 2 / 1 by 1 / 3, by the mol ratio of boric acid / phenol=2 / 1, the phenol of 9.4g and 20ml tetrahydrofuran solution Add it to a four-necked flask equipped with a condenser, a thermometer, an electric stirrer and a thermocouple. Raise the temperature to 90°C, then add 12.4g of boric acid, and at the same time use 0.1mol / L calcium carbonate solution to adjust the pH value of the solution in the four-necked flask. Reaction, vacuum decompression and dehydration at the same time, the reaction time is 4 hours, the vacuum degree is 0.1 ~ 1KPa; when the liquid is clear and slightly orange, and when there is no water after long-term pumping, stop pumping;
[0026] Step (2) Add 10.2 g of paraformaldehyde with a molecular weight of 200, make it react at 80° C. while stirring, and dehydrate under reduced pressure. As the dehydration proceeds, the liquid in the reaction bottle gradually becomes vi...
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