formaldehyde;phenol

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: 48.0 g of phenol and 82.6 g of 37%-formalin were placed in a separable flask equipped with a Dimroth condenser, and stirred for mixing therein, followed further by addition of 3.8 g of 29% ammonia water and stirring for mixing. The resultant solution was reacted at a temperature of 70-80° C. for 6.5 hours on a mantle heater. After the reaction, the reaction product was cooled to room temperature to obtain 78 g of phenol-formaldehyde initial condensate. The initial condensate was placed in a vessel formed by a copper foil and cured at 150° C. for 12 hours in a drier to obtain 60 g of a phenolic resin. Then, the phenolic resin was crushed to diameters of ca. 1-2 cm, heated to 600° C. at a rate of 200° C./h in a nitrogen gas atmosphere (normal pressure) and held at 600° C. for 1 hour for pre-calcination to obtain a carbon precursor. The carbon precursor was pulverized to form a powdery carbon precursor having an average particle size of 25 μm. Then, the powdery carbon precursor was charged in a vacuum calcination furnace, heated to 1200° C. at a rate of 5° C./min and held at 1200° C. for 1 hour for main calcination under a reduced pressure maintained at 1 kPa or below, followed by cooling to obtain a powdery carbonaceous material. equipped with a Dimroth condenser for mixing stirring for mixing After the reaction

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: 94.2 g of phenol (reagent-grade, available from Kanto Kagaku K.K.) and 80.6 g of 37%-formalin were placed in a separable flask equipped with a Dimroth condenser, and stirred for mixing therein, followed further by addition of 14.0 g of 20% sodium hydroxide aqueous solution and stirring for mixing. The resultant solution was reacted at a temperature of 85-95° C. for 6 hours on a mantle heater. After the reaction, the reaction product was cooled to room temperature to obtain 152 g of phenol-formaldehyde initial condensate. The initial condensate was placed in a vessel formed by a copper foil and cured at 150° C. for 12 hours in a drier (“EYELA NED-300”, available from Tokyo Rika Kiki K.K.) to obtain 95 g of a phenolic resin. Then, the phenolic resin was crushed to diameters of ca. 1-2 cm, heated to 600° C. at a rate of 200° C./h in a nitrogen gas atmosphere (normal pressure) and held at 600° C. for 1 hour for pre-calcination to obtain a carbon precursor. The carbon precursor was pulverized to form a powdery carbon precursor having an average particle size of 25 μm. Then, the powdery carbon precursor was charged in a vacuum calcination furnace, heated to 1100° C. at a rate of 5° C./min and held at 1100° C. for 1 hour for main calcination under a reduced pressure maintained at 1 kPa or below, followed by cooling to obtain a powdery carbonaceous material. equipped with a Dimroth condenser for mixing stirring for mixing After the reaction

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: The liquid phenol-formaldehyde resin (Resin 5L) was first treated with formaldehyde scavengers, then mixed with resorcinol, and spray-dried into powder resin. spray-dried into powder resin

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: A resole resin is made using from 1.5:1.0 up to 2.0:1.0 chemical equivalents ratio of formaldehyde:phenol catalyzed with KOH. When this reaction has proceeded to the desired viscosity, it is cooled and retarded by addition of formic acid. To this resin is added about 3 Phr of Epon epoxy resin, 3 Phr of DMP plasticizer, and about 2 Phr of a silicone surfactant. To about 70 Parts by weight (Pbw) of this mixture is added about 14 Pbw of a mixed blowing agent system such as described above, about 1.5 Pbw Arlatone "G" surfactant, about 0.1 Pbw L-5340 surfactant, and about 16 Pbw toluene sulfonic acid catalyst. This reacts to form a suitable closed cell phenolic foam. is cooled To about 70 Parts by weight (Pbw) of this mixture is added about 14 Pbw of a mixed This reacts to form a suitable closed cell phenolic foam

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: Into a 4 liter resin flask equipped with a mechanical stirrer, reflux condenser and thermometer is placed 2000 gms (21.28 moles) USP phenol; 882 gms (15.28 moles) aqueous formaldehyde (52%); 200 gms water and 12 gms (0.10 mole) phosphoric acid (85%). The pH of the resulting mixture is 1.05. This mixture is then heated to reflux and refluxed a total of 5 hours. The free formaldehyde content of the mixture at this point is found to be 0.84%. At this point the reflux condenser is replaced with a distillation condenser and batch distilled under atmospheric pressure for one hour until the batch temperature reaches 160° C. At this point a mixture of 173 gms (3.0 moles) of 52% aqueous formaldehyde, mixed with 70 gms of water is slowly added to the mixture over a period of 36 minutes. During the addition, the batch temperature drops to 142° C. When all the aqueous formaldehyde has been added, the batch is held at 142°-150° C. for 15 minutes. Then the receiver on the distillation condenser is replaced with a vacuum receiver to allow completion of the batch under vacuum. The resin is then dehydrated to a batch temperature of 165° C. under vacuum of 28 inches of mercury. The vacuum is released and the resin discharged from the vessel to yield 2027 gms of product, which exhibits a gradient bar melting point of 223° F. and a glass transition temperature as measured by differential scanning calorimetry of 70° C. (158° F.). This resin is a non-curing Novolak as shown when tested on a hot plate at 330° F. However, when thoroughly blended with 10 parts per hundred (pph) of hexa, it has a set time of 24-25 sec. when heated at 330° F. (166° C.). Into a 4 liter resin flask equipped with a mechanical stirrer reflux condenser This mixture is then heated to reflux refluxed a total of 5 hours At this point the reflux condenser is replaced with a distillation condenser batch distilled under atmospheric pressure for one hour until the batch temperature reaches 160° C is slowly added to the mixture over a period of 36 minutes During the addition drops to 142° C is then dehydrated to a batch temperature of 165° C. under vacuum of 28 inches of mercury

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: reacting phenol and formaldehyde to form a phenol-formaldehyde condensate;

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: A phenol formaldehyde resole was prepared in the laboratory in accordance with the procedure set forth in Example 3 except the molar ratio of formaldehyde to phenol was 2.4:1.

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: A phenol formaldehyde resole was prepared in the laboratory in accordance with the procedure set forth in Example 3 except the molar ratio of formaldehyde to phenol was 1.6:1.

Conditions: temp:80.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: An apparatus as described in Example 1 was charged with diphenyl ether (0.1 mol), phenol (0.1 mol) and sulfuric acid (0.5 g). The reagents were heated to 80° C. and stirring started. Formaldehyde (13 mL, 0.17 mol) was added dropwise resulting in the rapid formation of a solid product. After the addition was complete, the mixture was heated under reflux for 1 hour. The resulting product was a solid, insoluble mass. resulting in the rapid formation of a solid product After the addition the mixture was heated under reflux for 1 hour

Conditions: temp:80.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: An apparatus as described in Example 1 was charged with diphenyl ether (0.1 mol), phenol (0.1 mol) and sulfuric acid (0.5 g). The reagents were heated to 80° C. and stirring started. Formaldehyde (13 mL, 0.17 mol) was added dropwise resulting in the rapid formation of a solid product. After the addition was complete, the mixture was heated under reflux for 1 hour. The resulting product was a solid, insoluble mass. resulting in the rapid formation of a solid product After the addition the mixture was heated under reflux for 1 hour

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: A 250-mL 3-neck flask equipped with a mechanical stirrer and an addition port was charged with diphenyl ether (34 gm, 0.2 mol), acetic acid (35 mL) containing sulfuric acid (5 mL), and aqueous formaldehyde (37% solution, 46 mL, 0.61 mol). The flask was placed in a 100° C. oil bath and rapid mixing was started. After the reaction between the diphenyl ether and formaldehyde had proceeded for 24 hours phenol (40 mL, 0.46 mol) was added in uniform portions over a 15-minute period. A 250-mL 3-neck flask equipped with a mechanical stirrer was placed in a 100° C. rapid mixing

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: A 250-mL 3-neck flask equipped with a mechanical stirrer and an addition port was charged with diphenyl ether (34 gm, 0.2 mol), acetic acid (35 mL) containing sulfuric acid (5 mL), and aqueous formaldehyde (37% solution, 46 mL, 0.61 mol). The flask was placed in a 100° C. oil bath and rapid mixing was started. After the reaction between the diphenyl ether and formaldehyde had proceeded for 24 hours phenol (40 mL, 0.46 mol) was added in uniform portions over a 15-minute period. A 250-mL 3-neck flask equipped with a mechanical stirrer was placed in a 100° C. rapid mixing