Ethylene Glycol → Bis(2-hydroxyethyl) terephthalate

HRID 856870

反応式

HRID 856870 の反応式
[C:1]([OH:12])(=[O:11])[C:2]1[CH:10]=[CH:9][C:5]([C:6]([OH:8])=[O:7])=[CH:4][CH:3]=1.[CH2:13]([OH:16])[CH2:14]O.C(N([CH2:22][CH3:23])CC)C.[OH2:24]>>[C:1]([O:12][CH2:14][CH2:13][OH:16])(=[O:11])[C:2]1[CH:10]=[CH:9][C:5]([C:6]([O:8][CH2:23][CH2:22][OH:24])=[O:7])=[CH:4][CH:3]=1

参加物

5

反応物 4

HCID 174Ethylene GlycolHCID 962WaterHCID 7489Terephthalic AcidHCID 8471Triethylamine

生成物 1

HCID 13739Bis(2-hydroxyethyl) terephthalate

実験手順

A heat transfer medium-circulating 2-L stainless steel autoclave equipped with a stirrer was charged with high-purity terephthalic acid and ethylene glycol in the molar ratio of 1:2, and triethylamine was added in an amount of 0.3 mol-% relative to the acid component, and the mixture was subjected to esterification reaction for 120 minutes at a pressure of 0.25 MPa at 245° C. while water was distilled away from the system, whereby a mixture of bis(2-hydroxyethyl) terephthalate (BHET) and oligomers (referred to hereinafter as BHET mixture) was obtained. To this BHET mixture were added the above-described aluminum salt B in an amount of 0.015 mol-% in terms of aluminum atom relative to the acid component in the polyester, and the mixture was stirred at 245° C. for 10 minutes in a nitrogen atmosphere at normal pressure. Then, the temperature was increased to 275° C. over 50 minutes while the pressure in the reaction system was gradually reduced to 0.1 Torr, and the polymerization reaction was further conducted at 275° C. at 0.1 Torr. The polymerization time (AP) necessary for the IV of the polyethylene terephthalate to reach 0.65 dl/g is shown in Table 16.

後処理

  1. additionwas added in an amount of 0.3 mol-% relative to the acid component
  2. distillationwas distilled away from the system, whereby
  3. additiona mixture of bis(2-hydroxyethyl) terephthalate (BHET)

出典と根拠

ORDレコード
ord-77ff60a83bc04937b7b1a1b92af16def
出典データセット
uspto-grants-2006_12
特許番号
US07144614B2

関連ノート

読み込み中…