Acrylic Acid → alpha-Methylene-gamma-butyrolactone acrylic acid pentaerythritol allyl ether

HRID 83936

반응식

HRID 83936 반응식
[CH2:1]=[C:2]1[CH2:7][CH2:6][O:5][C:3]1=[O:4].[C:8]([OH:12])(=[O:11])[CH:9]=[CH2:10].[CH2:13]([O:16][CH2:17][C:18]([CH2:23][OH:24])([CH2:21][OH:22])[CH2:19][OH:20])[CH:14]=[CH2:15].S([O-])(OCCCCCCCCCCCC)(=O)=O.[Na+].S(OOS([O-])(=O)=O)([O-])(=O)=O.[Na+].[Na+].[OH-].[Na+]>O>[CH2:1]=[C:2]1[CH2:7][CH2:6][O:5][C:3]1=[O:4].[C:8]([OH:12])(=[O:11])[CH:9]=[CH2:10].[CH2:13]([O:16][CH2:17][C:18]([CH2:21][OH:22])([CH2:23][OH:24])[CH2:19][OH:20])[CH:14]=[CH2:15]

참가 물질

8

반응물 6

HCID 6581Acrylic Acid2회HCID 14798Sodium HydroxideHCID 62655Sodium PersulfateHCID 68352alpha-Methylene butyrolactone2회HCID 3086330Allyl pentaerythritol2회HCID 3423265Sodium Lauryl Sulfate2회

생성물 1

HCID 131731900alpha-Methylene-gamma-butyrolactone acrylic acid pentaerythritol allyl ether

시약·촉매·용매 1

HCID 962Water용매2회

반응 조건

온도
75 °C

실험 절차

The crosslinked polymer poly(α-methylene-γ-butyrolactone-acrylic acid-pentaerythritol allyl ether) was prepared by emulsion polymerization of α-methylene-γ-butyrolactone and acrylic acid with the crosslinking monomer pentaerythritol allyl ether. To a four neck round bottom glass flask, equipped with a mechanical stirrer and a thermocouple with a nitrogen inlet at the side of the inlet-tube and two dropping funnels was added the initial charge of 44.03 g of water and 0.51 g of a 20% solution of sodium dodecyl sulfate surfactant. Into the monomer dropping funnel a mixture of 20.8 g of α-methylene-γ-butyrolactone, 1.1 g of acrylic acid and 0.16 g of pentaerythritol allyl ether were added. Into the second dropping funnel the aqueous mixture consisting of 83.43 g water, 1.32 g 20% sodium dodecylsulfate, 0.14 g sodium persulfate and 0.17 g 20% sodium hydroxide solution were added. The initial charge was heated to 75° C. dropwise addition of the monomer was started. Dropwise addition of the aqueous mixture started 5 minutes later. The monomer feed ended 120 minutes after the start of monomer addition, and the aqueous stream ended 5 minutes after the monomer stream ended. After a cook-down time of one hour, the reaction mixture was cooled to room temperature.

후처리

  1. customTo a four neck round bottom glass flask, equipped with a mechanical stirrer
  2. additiona thermocouple with a nitrogen inlet at the side of the inlet-tube and two dropping funnels was added the
  3. additionwere added
  4. additionwere added
  5. additionThe initial charge
  6. additiondropwise addition of the monomer
  7. additionDropwise addition of the aqueous mixture
  8. waitThe monomer feed ended 120 minutes
  9. additionafter the start of monomer addition
  10. waitthe aqueous stream ended 5 minutes
  11. temperatureAfter a cook-down time of one hour, the reaction mixture was cooled to room temperature

출처 및 근거

ORD 기록
ord-40aa735a4fc642b2855ba315df9fa102
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08846817B2

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