반응 #8947

ord-5b5d74676e844a0585699235e1e1654c

반응 조건

온도
110°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타to prepare a treating agent solution
  2. 2
    workup.ADDITIONtreated
  3. 3
    세척washed with water
  4. 4
    기타dried
  5. 5
    기타to uniformly absorb the total amount of the above treating agent solution
  6. 6
    기타air-dried for 3 hours at room temperature
  7. 7
    workup.ADDITIONThe dried cloth was heat-treated for 20 minutes at 140° C. in a batch type hot air oven (“IPHH-2000”, an inert oven manufactured by Tabaiesbeck Co., Ltd.)
  8. 8
    세척washed with water
  9. 9
    세척It was further washed with 5% aqueous sodium bicarbonate solution
  10. 10
    세척rinsed three times with water
  11. 11
    세척subsequently washed with 10% aqueous citric acid solution
  12. 12
    세척rinsed three times with water
  13. 13
    세척finally washed with household
  14. 14
    세척washing detergent solution
  15. 15
    세척rinsed with water
  16. 16
    기타air-dried
  17. 17
    workup.WAITFurthermore, 0.5 g of the cloth was immersed in 10 ml of pure water for an hour at room temperature
  18. 18
    세척was not eluted

실험 절차

4.66 Grams (20 mmol) of L-lysine methyl ester dihydrochloride, 2.22 g (6.2 mmol) of disodium phosphate 12 hydrate and 0.2 g of polyoxyethylene lauryl ether (“Newcol 1100”, nonionic surfactant produced by Nippon Nyukazai Co., Ltd.) were dissolved in 10.0 ml of water to prepare a treating agent solution. A cotton cloth (200 mm×200 mm, 7.5 g) was in advance treated to be immersed in 25% aqueous sodium hydroxide solution for an hour at room temperature, washed with water and dried. This treated cotton cloth_was allowed to uniformly absorb the total amount of the above treating agent solution and then air-dried for 3 hours at room temperature. The dried cloth was heat-treated for 20 minutes at 140° C. in a batch type hot air oven (“IPHH-2000”, an inert oven manufactured by Tabaiesbeck Co., Ltd.) and washed with water. It was further washed with 5% aqueous sodium bicarbonate solution and rinsed three times with water and subsequently washed with 10% aqueous citric acid solution and rinsed three times with water, and finally washed with household washing detergent solution, rinsed with water and air-dried. The identification of the formed L-lysine cellulose ester was conducted by the following method. A part of the cloth was cut and a solution of ninhydrin in butanol was sprayed on it. Thereafter, it was heated for 10 minutes in an oven of 110° C. to cause coloring thereby the presence of the amino acid was confirmed. Also, a part of the cloth was cut and subjected to an infrared spectroscopic analysis whereby there was confirmed a peak based on ester bond at 1720–1740 cm−1. Furthermore, 0.5 g of the cloth was immersed in 10 ml of pure water for an hour at room temperature and then the immersed water was analyzed by HPLC whereby it was confirmed that free L-lysine methyl ester was not eluted. As a result of determination for the amount of the L-lysine bonded, it was 0.17 mmol per g of the cloth. The degree of esterfication was 0.028. Also, the amount of citric acid was 0.15 mmol.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07091221B2uspto-grants-2006_08