Ethylene → HCID 86759008、化合物

HRID 1369047ノート

反応式

HRID 1369047 の反応式
[C:1]([O:4][CH:5]=[CH2:6])(=[O:3])[CH3:2].C=C.[C:9](OO)(C)(C)[CH3:10].OCS([O-])=O.[Na+].[C:21]([O:25][C:26]12[CH2:32][CH:29]([CH2:30][CH2:31]1)[CH2:28][CH2:27]2)(=[O:24])[CH:22]=[CH2:23]>O.S([O-])([O-])(=O)=O.[NH4+].[Fe+]>[C:1]([O:4][CH:5]=[CH2:6])(=[O:3])[CH3:2].[C:21]([O:25][C:26]12[CH2:32][CH:29]([CH2:28][CH2:27]1)[CH2:30][CH2:31]2)(=[O:24])[CH:22]=[CH2:23].[CH2:9]=[CH2:10]

参加物

8

反応物 5

HCID 6325Ethylene2 回HCID 6410tert-Butyl hydroperoxideHCID 7904Vinyl Acetate2 回HCID 23509218Bicyclo[2.2.1]heptan-1-yl prop-2-enoateHCID 23689980Sodium Formaldehyde Sulfoxylate

生成物 1

HCID 86759008HCID 86759008、化合物

試薬・触媒・溶媒 2

HCID 178527670HCID 178527670、化合物触媒HCID 962Water溶媒2 回

反応条件

温度
60 °C

実験手順

932 g of water, 466 g of a 20% strength, aqueous solution of a polyvinyl alcohol having a degree of hydrolysis of 88 mol % and a Höppler viscosity of 4 mPas, 5 g of iron ammonium sulfate (1% strength in water) and 1170 g of vinyl acetate were initially introduced into a polymerization vessel having a volume of 5 liters and were heated to 60° C. At the same time, 40 bar of ethylene were forced in. tert-Butyl hydroperoxide (3% strength in water) and brüggolite (sodium hydroxymethanesulfinate) (5% strength in water) were then metered in continuously, each at 14 g/h. From the beginning of the polymerization, detectable from the increase in the internal temperature, the internal temperature was increased to 80° C. 30 minutes later, the remaining monomer mixture comprising 466 g of norbornyl acrylate and 699 g of vinyl acetate was metered in continuously in 2 h at 585 g/h. Simultaneously with the monomer metering, 755 g of a 12.3% strength polyvinyl alcohol solution (polyvinyl alcohol as above) were metered at 358 g/h in the course of 2 h. The ethylene pressure was kept at 40 bar up to the end of the monomer metering. Polymerization was effected until no more heat of polymerization could be observed. To remove residual monomers, postpolymerization was effected with 15 g of tert-butyl hydroperoxide (10% strength in water) and 15 g of brüggolite (10% strength in water) after cooling to 30° C.

後処理

  1. customFrom the beginning of the polymerization, detectable from the
  2. temperatureincrease in the internal temperature
  3. temperaturethe internal temperature was increased to 80° C
  4. custom30 minutes
  5. customcontinuously in 2 h
  6. customwere metered at 358 g/h in the course of 2 h
  7. customPolymerization
  8. temperatureno more heat of polymerization
  9. customTo remove residual monomers, postpolymerization
  10. temperatureafter cooling to 30° C.

出典と根拠

ORDレコード
ord-3e97fb027abc4788b0e7bf9612664e87
出典データセット
uspto-grants-2003_06
特許番号
US06576698B1

反応ノート

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