反应 #63430

ord-2548f1f26ad649c8805369e662cb133a

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他Graft copolymerization
  2. 2
    其他The graft copolymerization
  3. 3
    过滤filtered by suction
  4. 4
    洗涤washed with water (5 l)
  5. 5
    其他The sample was dried overnight at 90° C.
  6. 6
    其他to give a white fiber product (405 g, 93% conversion)
  7. 7
    萃取The cellulose graft copolymer was extracted
  8. 8
    温度by refluxing with tetrahydrofuran (9 l) for three hours
  9. 9
    其他to remove homopolymer
  10. 10
    过滤filtered
  11. 11
    其他dried

实验过程

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).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US04765982uspto-grants-1988_08