Acrylic Acid → Butyl prop-2-enoate;styrene

HRID 424323

Reaktionsgleichung

Reaktionsgleichung von HRID 424323
[C:1]([O:5][CH2:6][CH2:7][CH2:8][CH3:9])(=[O:4])[CH:2]=[CH2:3].Cl.Cl.N(C(C)(C)C(N)=N)=NC(C)(C)C(N)=N.[CH2:26]=[CH:27][C:28]1[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=1.C(O)(=O)C=C.C(S)CCCCCCCCCCC>CCCCCCCCCCCCCC[N+](C)(C)C.[Br-].O>[CH2:26]=[CH:27][C:28]1[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=1.[C:1]([O:5][CH2:6][CH2:7][CH2:8][CH3:9])(=[O:4])[CH:2]=[CH2:3]

Komponenten

8

Edukt 5

HCID 6581Acrylic AcidHCID 7501StyreneHCID 81951-DodecanethiolHCID 8846Butyl Acrylate2×HCID 763442,2'-Azobis(2-methylpropanimidamide) dihydrochloride

Produkt 1

HCID 168422Butyl prop-2-enoate;styrene

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 14250Tetradecyltrimethylammonium bromideKatalysator2×HCID 962WaterLösungsmittel3×

Reaktionsbedingungen

Temperatur
65 °C

Versuchsvorschrift

In a round glass flask are charged 300 parts by weight of deionized water and 1.5 parts by weight of TTAB (tetradecyltrimethylammonium bromide, product of Sigma Aldrich) and nitrogen bubbling is performed for 20 minutes. The temperature is raised to 65° C. under stirring. To the reaction mixture is added 40 parts by weight of an n-butyl acrylate monomer, followed by stirring for further 20 minutes. After 0.5 part by weight of a initiator “V-50” (trade name of 2,2′-azobis(2-methylpropionamidine)dihydrochloride, product of Wako Pure Chemicals) is dissolved in 10 parts by weight of deionized water in advance, the resulting solution is charged in the flask. After maintaining the temperature at 65° C. for 3 hours, an emulsion obtained by emulsifying 55 parts by weight of a styrene monomer, 15 parts by weight of an n-butyl acrylate monomer, 2.5 parts by weight of acrylic acid and 0.8 part by weight of dodecanethiol in 100 parts by weight of deionized water having 0.5 part by weight of TTAB dissolved therein is charged in the flask continuously through a metering pump over 2 hours. The temperature is raised to 70° C. and it is maintained for 2 hours, whereby the polymerization is completed. A core-shell resin particle dispersion liquid (A1) having a weight-average molecular weight Mw of 25,000, an average particle size of 150 nm and a solid content of 25 wt. % is obtained.

Aufarbeitung

  1. stirringby stirring for further 20 minutes
  2. additionthe resulting solution is charged in the flask
  3. temperatureAfter maintaining the temperature at 65° C. for 3 hours
  4. customan emulsion obtained
  5. dissolutiondissolved
  6. additiontherein is charged in the flask continuously through a metering pump over 2 hours
  7. temperatureThe temperature is raised to 70° C.
  8. temperatureit is maintained for 2 hours
  9. customan average particle size of 150 nm and a solid content of 25 wt. % is obtained

Quellen und Nachweise

ORD-Eintrag
ord-65134ed6fb8844fe99f6a2b320ab6e2a
Quelldatensatz
uspto-grants-2012_01
Patentnummer
US08105744B2

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