tert-Butyl hydroperoxide → Butyl acrylate vinyl acetate

HRID 35979

반응식

HRID 35979 반응식
C(N1CCCC1=O)=C.C(OO)(C)(C)C.S([O-])[O-].C=O.[Na+].[Na+].[C:22]([O:25][CH:26]=[CH2:27])(=[O:24])[CH3:23].[C:28]([O:32][CH2:33][CH2:34][CH2:35][CH3:36])(=[O:31])[CH:29]=[CH2:30]>O>[C:22]([O:25][CH:26]=[CH2:27])(=[O:24])[CH3:23].[C:28]([O:32][CH2:33][CH2:34][CH2:35][CH3:36])(=[O:31])[CH:29]=[CH2:30]

참가 물질

7

반응물 5

HCID 6410tert-Butyl hydroperoxide2회HCID 6917N-vinyl-2-pyrrolidone2회HCID 7904Vinyl AcetateHCID 8846Butyl AcrylateHCID 21225536CID 212255362회

생성물 1

HCID 23373234Butyl acrylate vinyl acetate

시약·촉매·용매 1

HCID 962Water용매4회

반응 조건

온도
55 °C

실험 절차

0.3 parts by weight (ppw) of the anionic polyelectrolyte dispersant used in Example 1, 1.6 ppw of the non-ionic surfactant solution quoted at the foot of Table 4, 0.1 ppw of the cellulose "Cellosize" QP 300 and 2.8 ppw vinyl pyrrolidone were dissolved at ambient temperature (20° to 25° C.) in 54.8 ppw water contained in a glass polymerisation vessel fitted with a stirrer, reflux condenser and inlets for reactants. The vessel was fluxed with nitrogen and then maintained under an atmosphere of nitrogen. The stirrer was started and the solution was heated to 55° C. 0.05 ppw of tertiary butyl hydroperoxide free radical initiator dissolved in 0.05 ppw water were added to the heated solution followed by 0.06 ppw of sodium formaldehyde sulphoxylate dissolved in 0.5 ppw water and the temperature of the contents of the vessel rose to 60° C. indicating exothermic polymerisation of the vinyl pyrrolidone. The temperature was maintained at 60° C. for 50 minutes and then 19.1 ppw vinyl acetate, 8.2 ppw butyl acrylate and 0.6 ppw tertiary butyl hydroperoxide were each added at a steady rate over a period of two hours simultaneously with a steady addition of a solution of 0.6 ppw sodium formaldehyde sulphoxylate and 3 ppw of the nonionic surfactant used in Example 1 dissolved in 7.3 ppw water. A copolymerisation occurred which formed a colloidally stable dispersion of film-forming particles of vinyl acetate/butyl acrylate copolymer with which chains of polyvinyl pyrrolidone had chemically bonded. The dispersion was allowed to cool to ambient temperature, stirring was stopped and the cooled dispersion was filtered. The filtrate was found to consist of the colloidally (at least partially sterically) stable dispersion of film-forming copolymer particles bonded to polyvinyl pyrrolidone water-soluble compound. The filtrate which will be referred to as Latex 6. The copolymer particles in Latex 6 had a number average particle size of 90 nm, a minimum film-forming temperature of 285K and at least one or other of the amino or carbonyl groups of the polyvinyl pyrrolidone were adsorbable onto the titanium dioxide particles of Millbase 6. The pH of Latex 6 was adjusted to 8 as in Example 1.

후처리

  1. customcontained in a glass polymerisation vessel
  2. customfitted with a stirrer
  3. temperaturereflux condenser and inlets for reactants
  4. temperaturemaintained under an atmosphere of nitrogen
  5. additionwere added to the heated solution
  6. customrose to 60° C.
  7. temperatureThe temperature was maintained at 60° C. for 50 minutes

출처 및 근거

ORD 기록
ord-c54135f1785442ec859de7d350f12c8d
출처 데이터셋
uspto-grants-1995_05
특허 번호
US05412019

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