Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Formaldehyde | HCID 712 | — |
| Reactant | Phenol | HCID 996 | — |
| Reactant | Melamine | HCID 7955 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Product | HCID 21285052 | HCID 21285052 | — |
Reaction Steps
The process for Example 5 was initiated by charging 593.5 g phenol (6.31 moles), 4.3 g of acetic acid (0.72% of phenol) and 75.2 g melamine (0.60 moles) into a reaction vessel to form a reaction mixture. The reaction mixture was heated to 80° C., and 64.1 g of 50.3% aqueous formaldehyde (60% of total charge) was added in over 20 minutes. The reaction mixture went under atmospherically distilling to 123° C., then maintained at 123° C. for 2 hours followed by reducing the reaction mixture temperature to 80° C. 42.5 g of 50.3% aqueous formaldehyde (40% of total charge) was added over about 20 minutes to the reaction mixture, followed by atmospherically distilling the reaction mixture to 123° C., then maintaining the temperature at 123° C. for 1.6 hours, and finally increasing the temperature over 60 minutes to 165° C. and continuing to distill atmospherically. Next, the reaction mixture was under a gradually increasing vacuum over 2 hours to full vacuum of at least 27 inches while maintaining a temperature of 163°-165° C., and then heating the reaction mixture to 175° C. under full vacuum. Further, the process is concluded by removing the vacuum distillate (417.8 g) and discharging the product (263.0 g) from the reaction vessel.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US09249251B2 |
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| Source dataset | uspto-grants-2016_02 |
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| ORD ID | ord-eab2ea239c334b9186ae9776a8d32d77 |
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| Source note | uspto-grants-2016_02 |
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