Acrylic Acid → Butyl prop-2-enoate;styrene

HRID 424323

反応式

HRID 424323 の反応式
[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]

参加物

8

反応物 5

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

生成物 1

HCID 168422Butyl prop-2-enoate;styrene

試薬・触媒・溶媒 2

HCID 14250Tetradecyltrimethylammonium bromide触媒2 回HCID 962Water溶媒3 回

反応条件

温度
65 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-65134ed6fb8844fe99f6a2b320ab6e2a
出典データセット
uspto-grants-2012_01
特許番号
US08105744B2

関連ノート

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