Propylene Glycol → 1,2-Propylene-dipropylene terephthalate

HRID 1633440

反応式

HRID 1633440 の反応式
[C:1]([O-:12])(=[O:11])[C:2]1[CH:10]=[CH:9][C:5]([C:6]([O-:8])=[O:7])=[CH:4][CH:3]=1.S([C:17]1[C:25]([C:26]([O-])=O)=[CH:24][CH:23]=[CH:22][C:18]=1[C:19]([O-])=O)(O)(=O)=O.[Na+].[Na+].[CH2:31](O)C(O)C.COC(=O)C1C=CC(C(OC)=O)=CC=1.S(C1C(C(OC)=O)=CC=CC=1C(OC)=O)(O)(=O)=O.[Na]>CCCC[Sn](O)=O.C(O)COCCO>[C:1]1(=[O:12])[O:11][CH:22]([CH3:31])[CH2:23][CH2:24][CH:25]([CH3:26])[CH2:17][CH:18]([CH3:19])[O:8][C:6](=[O:7])[C:5]2[CH:9]=[CH:10][C:2]1=[CH:3][CH:4]=2

参加物

8

反応物 5

HCID 1030Propylene Glycol2 回HCID 8441Dimethyl terephthalateHCID 1542691,4-BenzenedicarboxylateHCID 21895896Sodium sulfoisophthalateHCID 87098651Sodium dimethyl sulfoisophthalate

生成物 1

HCID 684281411,2-Propylene-dipropylene terephthalate

試薬・触媒・溶媒 2

HCID 16767Butylstannonic acid触媒HCID 8117Diethylene Glycol溶媒2 回

反応条件

温度
165 °C

実験手順

A linear sulfonated random copolyester resin comprising 46.5 mole percent terephthalate, 3.5 mole percent sodium sulfoisophthalate, 47.5 mole percent 1,2-propanediol, and 2.5 mole percent diethylene glycol is prepared as follows. Into a 5 gallon Parr reactor equipped with a bottom drain valve, double turbine agitator, and distillation receiver with a cold water condenser are charged 3.98 kilograms of dimethylterephthalate, 451 grams of sodium dimethyl sulfoisophthalate, 3.104 kilograms of 1,2-propanediol (1 mole excess of glycol), 351 grams of diethylene glycol (1 mole excess of glycol), and 8 grams of butyltin hydroxide oxide catalyst. The reactor is then heated to 165° C. with stirring for 3 hours whereby 1.33 kilograms of distillate are collected in the distillation receiver, and which distillate comprises about 98 percent by volume methanol and 2 percent by volume 1,2-propanediol as measured by the ABBE refractometer available from American Optical Corporation. The reactor mixture is then heated to 190° C. over a one hour period, after which the pressure is slowly reduced from atmospheric pressure to about 260 Torr over a one hour period, and then reduced to 5 Torr over a two hour period with the collection of approximately 470 grams of distillate in the distillation receiver, and which distillate comprises approximately 97 percent by volume 1,2-propanediol and 3 percent by volume methanol as measured by the ABBE refractometer. The pressure is then further reduced to about 1 Torr over a 30 minute period whereby an additional 530 grams of 1,2-propanediol are collected. The reactor is then purged with nitrogen to atmospheric pressure, and the polymer product discharged through the bottom drain onto a container cooled with dry ice to yield 3.5 mole percent sulfonated polyester resin, sodio salt of (1,2-propylene-dipropylene-5-sulfoisophthalate)-copoly (1,2-propylene-dipropylene terephthalate).

後処理

  1. customis prepared
  2. customInto a 5 gallon Parr reactor equipped with a bottom drain valve
  3. distillationdouble turbine agitator, and distillation receiver with a cold water condenser
  4. distillationare collected in the distillation receiver, and which distillate
  5. temperatureThe reactor mixture is then heated to 190° C. over a one hour period
  6. waitafter which the pressure is slowly reduced from atmospheric pressure to about 260 Torr over a one hour period
  7. distillationreduced to 5 Torr over a two hour period with the collection of approximately 470 grams of distillate in the distillation receiver, and which distillate
  8. waitThe pressure is then further reduced to about 1 Torr over a 30 minute period
  9. customwhereby an additional 530 grams of 1,2-propanediol are collected
  10. customThe reactor is then purged with nitrogen to atmospheric pressure
  11. temperaturecooled with dry ice

出典と根拠

ORDレコード
ord-397b7d5f92b74849840511625a4fe18d
出典データセット
uspto-grants-2003_01
特許番号
US06503678B1

関連ノート

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