Method for detecting ancient silk fabric
A technology of silk fabrics and silk fibroin, which is applied in the field of cultural relics detection, can solve problems such as low sensitivity, unsuitability for cultural relics detection, and large influence of impurities, and achieve high sensitivity, excellent sensitization and modifiability, and enhanced sensitivity.
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Embodiment 1
[0028] 1) Weigh 5g of mulberry silk and place it in 180mL of 0.018M sodium carbonate solution, in a water bath for 55 minutes, and the temperature of the water bath is 80°C, take it out and wash it with deionized water three times, and put it in an oven to dry.
[0029] 2) Take 2g of dried silk fibroin, 2.3g of calcium nitrate, add 48mL of formic acid, magnetically stir for 80min, filter and add sodium bicarbonate until the solution is neutral, and use a cellulose dialysis bag with a molecular weight cut-off of 8000 to remove the resulting solution. After dialysis in ionized water for 2 days, and changing the water every 5 hours, the silk fibroin solution was freeze-dried in a vacuum freeze dryer for 2 days, and the obtained silk fibroin was ground into powder for use.
[0030] 3) Take 2.8mL of graphene oxide with a concentration of 5mg / mL, soak it in 0.2M propylenediamine and reflux for 2.8h at 65℃; then, add 5ml of 0.1% (w / v) sodium hexachloroplatinate to the previous After conti...
Embodiment 2
[0040] 1) Weigh 5g of mulberry silk and place it in 200mL of 0.02M sodium carbonate solution, in a water bath for 60 minutes, the temperature of the water bath is 80℃, take it out and wash it with deionized water four times, and put it in an oven to dry.
[0041] 2) Take 2g of dried silk fibroin, 2.5g of calcium nitrate, add 50mL of formic acid, stir with a magnetic force for 90 minutes, filter and add sodium bicarbonate until the solution is neutral, and use a cellulose dialysis bag with a molecular weight cut-off of 9000 to remove the resulting solution. Dialysis in ionized water for 2.5 days and changing the water every 6 hours. After freeze-drying the silk fibroin solution in a vacuum freeze dryer for 2.5 days, the resulting silk fibroin is ground into powder for use.
[0042] 3) Take 3mL of graphene oxide with a concentration of 6mg / mL, soak it in 0.3M propylenediamine and reflux for 3h at 70℃; then, add 5.5ml of 0.1% (w / v) sodium hexachloroplatinate to the previous In the mix...
Embodiment 3
[0052] 1) Weigh 5g of mulberry silk and place it in 220mL of 0.022M sodium carbonate solution, in a water bath for 65 min, and the temperature of the water bath is 80°C, take it out and wash it with deionized water five times, and put it in an oven to dry.
[0053] 2) Take 2g of dried silk fibroin, 2.7g of calcium nitrate, add 52mL of formic acid, stir with a magnetic force for 100min, filter and add sodium bicarbonate until the solution is neutral, and use a cellulose dialysis bag with a molecular weight cut-off of 10,000 to remove the resulting solution. After dialysis in ionized water for 3 days, and changing the water every 7 hours, the silk fibroin solution was freeze-dried in a vacuum freeze dryer for 3 days, and the obtained silk fibroin was ground into powder for use.
[0054] 3) Take 3.2mL of graphene oxide with a concentration of 7mg / mL, soak it in 0.4M propylenediamine and reflux for 3.2h at 75℃; then, add 6ml of 0.1% (w / v) sodium hexachloroplatinum to the previous After...
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