Trimethylolpropane → Cyclohexane tertiary butyl isophthalate

HRID 2376811

Reaktionsgleichung

Reaktionsgleichung von HRID 2376811
[CH:1]1([C:10]([OH:12])=[O:11])[CH2:6][CH2:5][CH:4](C(O)=O)[CH2:3][CH2:2]1.[C:13](C1C(C(O)=O)=CC=CC=1C(O)=O)([CH3:16])([CH3:15])[CH3:14].C1(CO)CCC(CO)CC1.OCC(C)(CO)C.C(C(CO)(CO)CC)O.[C:55]([O-:58])(=[O:57])C.[Sb+3].C([O-])(=O)C.C([O-])(=O)C>C(O)CO>[CH2:1]1[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.[C:10]([O:12][C:13]([CH3:16])([CH3:15])[CH3:14])(=[O:11])[C:1]1[CH:2]=[CH:3][CH:4]=[C:5]([C:55]([O-:58])=[O:57])[CH:6]=1

Komponenten

8

Edukt 6

HCID 6510TrimethylolpropaneHCID 77351,4-CyclohexanedimethanolHCID 141061,4-Cyclohexanedicarboxylic acidHCID 23354Antimony triacetateHCID 31344Neopentyl glycolHCID 19762767t-Butyl isophthalic acid

Produkt 1

HCID 86604590Cyclohexane tertiary butyl isophthalate

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 174Ethylene GlycolLösungsmittel

Reaktionsbedingungen

Temperatur
254 °C

Versuchsvorschrift

Synthesis of the co-cyclohexane-tbia was carried out in a batch reactor which was charged with the following raw materials: 1,4 cyclohexane dicarboxylic acid (37 kg), tertiary butyl isophthalic acid (59.9 kg), 1,4 cyclohexane dimethanol (37.8 kg), neopentyl glycol (11.2 kg), ethylene glycol (60.3 kg), trimethylol propane (0.5 kg), and antimony (III) acetate (90 g). Under a pressure of 2 atmospheres (2×105 N/m2), this mixture was heated to 254 degrees C. while removing the reaction by-product, water. After completing this reaction and removing the water, the pressure was gradually reduced to 1 torr (263 N/m2) while heating to 290° C. The condensation by-product, ethylene glycol, was continuously removed until a polymer with intrinsic viscosity of 0.72 dl/g, as measured in 60/40 wt % phenol/o-dichlorobenzene, was produced. The polymer had a glass transition temperature of about 67° C. as measured by DSC with a temperature ramp of 20° C./min. This CCH-tbia had a refractive index of 1.519 as measured with a Metricon refractometer at 632 nm.

Aufarbeitung

  1. customwas carried out in a batch reactor
  2. customwhile removing the reaction by-product, water
  3. customthis reaction
  4. customremoving the water
  5. temperaturewhile heating to 290° C
  6. customThe condensation by-product, ethylene glycol, was continuously removed until a polymer with intrinsic viscosity of 0.72 dl/g
  7. customwas produced

Quellen und Nachweise

ORD-Eintrag
ord-9c5fc90ff6974e1790d86d72c47aef93
Quelldatensatz
uspto-grants-2008_12
Patentnummer
US07468204B2

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