Methyl Methacrylate → Butyl prop-2-enoate--methyl 2-methylprop-2-enoate (1/1)

HRID 35152

반응식

HRID 35152 반응식
[C:1]([O:5][CH2:6][CH2:7][CH2:8][CH3:9])(=[O:4])[CH:2]=[CH2:3].[C:10]([O:15][CH3:16])(=[O:14])[C:11]([CH3:13])=[CH2:12].C(=O)([O-])[O-].[Na+].[Na+]>O.[N+]([O-])(O)=O>[C:1]([O:5][CH2:6][CH2:7][CH2:8][CH3:9])(=[O:4])[CH:2]=[CH2:3].[C:10]([O:15][CH3:16])(=[O:14])[C:11]([CH3:13])=[CH2:12]

참가 물질

6

반응물 3

HCID 6658Methyl MethacrylateHCID 8846Butyl AcrylateHCID 10340Sodium Carbonate

생성물 1

HCID 62802Butyl prop-2-enoate--methyl 2-methylprop-2-enoate (1/1)

시약·촉매·용매 2

HCID 944Nitric Acid용매HCID 962Water용매

실험 절차

Cellulose (200 g, Harmac fully bleached Douglas Fir pulp available from MacMillan Bloedel, Stamford, CT) was dispersed in water (9.5 l) by mechanical agitation under nitrogen purging for two hours. A mixture of butyl acrylate (200 g) and methyl methacrylate (20 g) was vigorously stirred into the pulp for one-half hour. Graft copolymerization was initiated by addition of ceric ammonium nitrate (11 g, 0.02M) in 1M nitric acid (500 ml). The graft copolymerization was allowed to proceed for four hours, during which the color of the aqueous portion went from yellow (Ce4) to colorless (Ce3) indicating the oxidation of cellulose and initiation of polymerization. The reaction was neutralized with sodium carbonate (26.5 g, 0.25 M), filtered by suction, and washed with water (5 l). The sample was dried overnight at 90° C. to give a white fiber product (405 g, 93% conversion). The cellulose graft copolymer was extracted by refluxing with tetrahydrofuran (9 l) for three hours to remove homopolymer, filtered and dried to yield cellulose/butyl acrylate/methyl methacrylate fibers (200 g/177 g, 53 wt. % cellulose/47 wt. % butyl acrylate/methyl methacrylate, 86% graft efficiency).

후처리

  1. customGraft copolymerization
  2. customThe graft copolymerization
  3. filtrationfiltered by suction
  4. washwashed with water (5 l)
  5. customThe sample was dried overnight at 90° C.
  6. customto give a white fiber product (405 g, 93% conversion)
  7. extractionThe cellulose graft copolymer was extracted
  8. temperatureby refluxing with tetrahydrofuran (9 l) for three hours
  9. customto remove homopolymer
  10. filtrationfiltered
  11. customdried

출처 및 근거

ORD 기록
ord-2548f1f26ad649c8805369e662cb133a
출처 데이터셋
uspto-grants-1988_08
특허 번호
US04765982

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