반응 #324348

ord-605f8938786442bf98d55b881050907d

반응 방정식

CCC=C(C)C(=O)OOc1ccccc1
phenoxy ethylmethacrylate
C=C(C)C(=O)O
methacrylic acid
C=C(C)C(=O)OC
methyl methacrylate
C=C(C)C(=O)OC.C=C(C)C(=O)[O-].CCC=C(C)C(=O)OOc1ccccc1
phenoxy ethylmethacrylate methylmethacrylate methacrylate
수율 163.3%

반응 조건

온도
72°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타equipped with an agitator and a condenser
  2. 2
    workup.ADDITIONwas added dropwise over 3 hours
  3. 3
    workup.ADDITIONOnce the dropwise addition
  4. 4
    기타the mixture was reacted for one more hour
  5. 5
    workup.ADDITIONwas added
  6. 6
    온도The temperature was raised to 78° C.
  7. 7
    온도the mixture was heated for 4 hours
  8. 8
    기타The obtained reaction solution
  9. 9
    기타was precipitated two times in large excess of hexane
  10. 10
    기타the precipitated resin was dried

실험 절차

(Synthesis of Water-Insoluble Polymer Dispersant P-1) 88 g of methyl ethyl ketone was added to a 1000 ml three-necked flask equipped with an agitator and a condenser, and was heated to 72° C. under a nitrogen atmosphere. To this, a solution of 0.85 g of dimethyl 2,2′-azobisisobutyrate, 50 g of phenoxy ethylmethacrylate, 13 g of methacrylic acid and 37 g of methyl methacrylate dissolved in 50 g of methyl ethyl ketone was added dropwise over 3 hours. Once the dropwise addition was completed, the mixture was reacted for one more hour, and then a solution of 0.42 g of dimethyl 2,2′-azobisisobutyrate dissolved in 2 g of methyl ethyl ketone was added. The temperature was raised to 78° C., and the mixture was heated for 4 hours. The obtained reaction solution was precipitated two times in large excess of hexane, and the precipitated resin was dried to obtain 96.5 g of phenoxy ethylmethacrylate/methylmethacrylate/methacrylate (copolymerization ratio [% by mass ratio]=50/37/13) copolymer (resin dispersant P-1).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08641181B2uspto-grants-2014_02