Formaldehyde → Dihydrobenzoxazine

HRID 615916

Reaktionsgleichung

Reaktionsgleichung von HRID 615916
O[C:2]1C=C[C:5]([C:8]([C:11]2[CH:16]=CC(O)=CC=2)(C)C)=[CH:4][CH:3]=1.[NH2:18]C1C=CC=CC=1.[CH2:25]=[O:26]>C1(C)C=CC=CC=1>[O:26]1[C:25]2[CH:2]=[CH:3][CH:4]=[CH:5][C:8]=2[CH2:11][CH2:16][NH:18]1

Komponenten

5

Edukt 3

HCID 712Formaldehyde2×HCID 6115AnilineHCID 6623Bisphenol A

Produkt 1

HCID 21887592Dihydrobenzoxazine

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1140TolueneLösungsmittel

Reaktionsbedingungen

Temperatur
65 °C

Versuchsvorschrift

To a suitably equipped glass resin reactor equipped with stirrer are charged 100 parts bisphenol A, 70 parts toluene and 81.5 parts of aniline. The slurry is warmed and agitated to form a uniform solution. An inert nitrogen atmosphere is maintained over the reaction mixture. The temperature of the reaction mixture is adjusted to 50° C. and 108 parts of 50% formalin are added slowly, while the temperature is maintained at 50° to 55° C. After formalin addition is complete the batch is refluxed at 65° C. for 1 hour under reduced pressure. The batch is then heated to atmospheric reflux and the reflux condensate is permitted to separate into an aqueous phase and organic phase in an oil/water separator. The organic phase of the condensate is returned to the reactor and the aqueous phase is removed. After about 83 parts of water are removed and the reaction temperature reaches 116° C., the clear product solution is cooled while 21 parts of 2-butoxyethanol are added. The clear pale yellow solution of poly(dihydrobenzoxazine) had the following composition and properties: percent closed dihydrobenzoxazine ring 83%, equiv. wt. 278, solids 71.6%, Brookfield viscosity 305 cps.

Aufarbeitung

  1. customTo a suitably equipped glass resin reactor equipped with stirrer
  2. temperatureThe slurry is warmed
  3. customto form a uniform solution
  4. temperatureAn inert nitrogen atmosphere is maintained over the reaction mixture
  5. customis adjusted to 50° C.
  6. temperatureis maintained at 50° to 55° C
  7. temperatureThe batch is then heated
  8. temperatureto atmospheric reflux
  9. customto separate into an aqueous phase and organic phase in an oil/water separator
  10. customthe aqueous phase is removed
  11. customAfter about 83 parts of water are removed
  12. customreaches 116° C.
  13. temperaturethe clear product solution is cooled while 21 parts of 2-butoxyethanol
  14. additionare added
  15. custompercent closed dihydrobenzoxazine ring 83%, equiv. wt. 278, solids 71.6%, Brookfield viscosity 305 cps

Quellen und Nachweise

ORD-Eintrag
ord-e5105f7e75e24c42915b2639b684f2b1
Quelldatensatz
uspto-grants-1985_02
Patentnummer
US04501864

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