Trimethylolpropane → Cyclohexane tertiary butyl isophthalate

HRID 2376810

반응식

HRID 2376810 반응식
C[O:2][C:3]([CH:5]1[CH2:10][CH2:9][CH:8](C(OC)=O)[CH2:7][CH2:6]1)=[O:4].[CH:15]1([CH2:23][OH:24])[CH2:20][CH2:19][CH:18](CO)[CH2:17][CH2:16]1.OC[C:27]([CH3:31])([CH2:29]O)[CH3:28].C(C(CO)(CO)CC)[OH:33].C([O-])(=O)C.[Sb+3].C([O-])(=O)C.C([O-])(=O)C>C([O-])(=O)C.[Co+2].C([O-])(=O)C.C([O-])(=O)C.[Zn+2].C([O-])(=O)C.C(O)CO>[CH2:5]1[CH2:10][CH2:9][CH2:8][CH2:7][CH2:6]1.[C:23]([O:24][C:27]([CH3:28])([CH3:29])[CH3:31])(=[O:33])[C:15]1[CH:16]=[CH:17][CH:18]=[C:19]([C:3]([O-:4])=[O:2])[CH:20]=1

참가 물질

9

반응물 5

HCID 6510TrimethylolpropaneHCID 7198Dimethyl 1,4-cyclohexanedicarboxylateHCID 77351,4-CyclohexanedimethanolHCID 23354Antimony triacetateHCID 31344Neopentyl glycol

생성물 1

HCID 86604590Cyclohexane tertiary butyl isophthalate

시약·촉매·용매 3

HCID 6277Cobalt diacetate촉매HCID 11192Zinc Acetate촉매HCID 174Ethylene Glycol용매

반응 조건

온도
254 °C

실험 절차

Synthesis of the co-cyclohexane-tbia was carried out in a batch reactor which was charged with the following raw materials: 1,4 dimethyl cyclohexane dicarboxylate (8.45 kg), 1,4 cyclohexane dimethanol (8.98 kg), neopentyl glycol (1.8 kg), ethylene glycol (7.95 kg), trimethylol propane (0.2 kg), cobalt (II) acetate (3.6 g), zinc acetate (5.0 g), and antimony (III) acetate (6.5 g). Under a pressure of 2 atmospheres (2×105 N/m2), this mixture was heated to 254 C while removing the reaction by-product, methanol. After completing this reaction and removing the methanol, tertiary butyl isophthalate (9.48 kg) was charged to the reactor. Under a pressure of 2 atmospheres (2×105 N/m2), the mixture was heated to 254° C. until the reaction by-product, water, was removed. Triethyl phosphonoacetate (7.0 g) was then charged to the reactor and 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.

후처리

  1. customwas carried out in a batch reactor
  2. temperatureUnder a pressure of 2 atmospheres (2×105 N/m2), this mixture was heated to 254 C
  3. customwhile removing the reaction by-product, methanol
  4. customthis reaction
  5. customremoving the methanol, tertiary butyl isophthalate (9.48 kg)
  6. additionwas charged to the reactor
  7. customwas removed
  8. additionTriethyl phosphonoacetate (7.0 g) was then charged to the reactor
  9. temperaturewhile heating to 290° C
  10. customThe condensation by-product, ethylene glycol, was continuously removed until a polymer with intrinsic viscosity of 0.72 dl/g
  11. customwas produced

출처 및 근거

ORD 기록
ord-b6005aaaca8a4c84b62f341e3c9753bd
출처 데이터셋
uspto-grants-2008_12
특허 번호
US07468204B2

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