Trimethylolpropane → Cyclohexane tertiary butyl isophthalate

HRID 2376810

反応式

HRID 2376810 の反応式
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

参加物

9

反応物 5

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

生成物 1

HCID 86604590Cyclohexane tertiary butyl isophthalate

試薬・触媒・溶媒 3

HCID 6277Cobalt diacetate触媒HCID 11192Zinc Acetate触媒HCID 174Ethylene Glycol溶媒

反応条件

温度
254 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-b6005aaaca8a4c84b62f341e3c9753bd
出典データセット
uspto-grants-2008_12
特許番号
US07468204B2

関連ノート

読み込み中…