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PROJECT: LIFE12 ENV/IT/352 «BIONAD»

PROJECT: LIFE12 ENV/IT/352 «BIONAD». << Naturalised  dyes replacing commercial colorants for environmentally friendly leather dyeing and water recycle>>. DAVIDE PELLEGRINI ICCOM-CNR, Pisa. 6 Months Progress Meeting – BIOKIMICA premises , Santa Croce sull’Arno (PI), June 13th 2014.

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PROJECT: LIFE12 ENV/IT/352 «BIONAD»

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  1. PROJECT: LIFE12 ENV/IT/352 «BIONAD» <<Naturalised dyes replacing commercial colorants for environmentally friendly leather dyeing and water recycle>> DAVIDE PELLEGRINI ICCOM-CNR, Pisa 6 Months Progress Meeting – BIOKIMICA premises, Santa Croce sull’Arno (PI), June 13th 2014

  2. Actions  B.1BIOKIMICA, INESCOP, ICCOM-CNR (0-6 months) Demonstration of the use of traditionalchemicalaciddyes in leatherdyeing B.2BIOKIMICA, INESCOP, (ICCOM-CNR) (0-6 months) Demonstration of the qualityfeatures of dyedleatherwithaciddyes B.4BIOKIMICA, (ICCOM-CNR) (3-9 months) Demonstration of naturaliseddyes in leatherdyeingatlaboratorylevel

  3. Naturalised dyes  DO30 DB27 LACTOSE DR202 DY42

  4. Commercial acid dyes  O37 Y49 B113 R249

  5. Leather dyeing procedure B.1, B.4 1. Formic acid at 55°C Heating at 55°C 400 µL MilliQ + 4 mgformic acid Magnetic stirring for 0.5 h 4 mg/2 mL 2% (dye/leather) 0.2 g Washing with 4 mLMilliQ for 3 times Magnetic stirring at 20°C for 1 h

  6. Leather dyeing procedure B.1, B.4 2. Neutralization Heating at 55°C 400 µL MilliQ + 4 mgformic acid Magnetic stirring for 0.5 h 4 mg/2 mL 2% (dye/leather) 0.2 g Neutralization with 50µL K2CO3 (pH = 7-8) Magnetic stirring for 10 min Magnetic stirring at 20°C for 1 h Washing with 4 mLMilliQ for 3 times

  7. Dyes characterization UV-Vis B.1, B.2, B.4 FORMIC ACID PROCEDURE Naturalised dyes Commercial acid dyes 1  Dyeing bath 2  Washing 1 3  Washing 2 4  Washing 3

  8. Dyes characterization UV-Vis B.1, B.2, B.4 NEUTRALIZATION PROCEDURE Naturalised dyes Commercial acid dyes 1  Dyeing bath 2  Washing 1 3  Washing 2 4  Washing 3

  9. Dyes characterization UV-Vis B.1, B.2, B.4 DO30 dyeingbath DO30 washing 1 1.3 DO30 washing 2 DO30 washing 3 1.2 442 1.1 0.5 1 0.9 -61% 0.8 A -79% -83% 0.7 Absorbance 0.6 0.5 0.0 0.4 Tanning solution Washing water 2 0.3 Washing water 1 Washing water 3 0.2 0.1 0 -0.1 200 250 300 350 400 450 500 550 600 650 700 750 800 Wavelength [nm]

  10. Dyed leather characterization B.1, B.2, B.4 Naturalised dyes Commercial acid dyes 2% 5% 10% 15%

  11. Dyed leather characterization B.1, B.2, B.4 Naturalised dyes Commercial acid dyes Formic acid Neutralization

  12. Dyed leather characterization Colorimetry B.1, B.2, B.4 CM2600d KONICA MINOLTA 360-740 nm α = 10° D65 d. 5 mm

  13. FT-IR CHARACTERIZATION B.1, B.2, B.4 AMIDE II CNν, NHδ ~1550 cm-1 0.12 AMIDE I C=Oν ~1650 cm-1 0.1 0.08 Absorbance 0.06 COOHν ~1730 cm-1 0.04 ATR spectrum 128 scans Untreated leather 0.02 0 3500 3000 2500 2000 1500 1000 500 0 Wavenumbers [1/cm]

  14. FT-IR CHARACTERIZATION B.1, B.2, B.4 AMIDE I1 ~1654 cm-1 AMIDE II CN ν, NHδ ~1550 cm-1 0.12 AMIDE I2 ~1636 cm-1 AMIDE I C=Oν ~1650 cm-1 0.1 0.08 Absorbance 0.06 COOHν ~1730 cm-1 0.04 ATR spectrum 128 scans Untreated leather 0.02 0 3500 3000 2500 2000 1500 1000 500 0 Wavenumbers [1/cm]

  15. FT-IR CHARACTERIZATION B.1, B.2, B.4 Naturalised dyes 1.02 1.014 1.008 1654 cm-1 1650 cm-1 1634 cm-1 1637 cm-1 1.002 0.996 0.99 Absorbance BLANK 0.984 DO30-HCl 0.978 DY42-HCl 0.972 DR202-HCl 0.966 DB27-HCl 0.96 0.954 1660 1655 1650 1645 1640 1635 1630 1625 1620 Wavenumbers [1/cm]

  16. FT-IR CHARACTERIZATION B.1, B.2, B.4 Commercial dyes 1.01 1.005 1 0.995 BLANK Absorbance 0.99 ORANGE 37 0.985 YELLOW 49 0.98 RED 249 0.975 BLUE 113 0.97 0.965 1670 1665 1660 1655 1650 1645 1640 1635 1630 1625 1620 Wavenumbers [1/cm]

  17. FT-IR CHARACTERIZATION Principal Component Analysis B.1, B.2, B.4 AMIDE I1 ~1654 cm-1 AMIDE II CN ν, NHδ ~1550 cm-1 0.12 AMIDE I2 ~1636 cm-1 AMIDE I C=Oν ~1650 cm-1 0.1 VARIABLES Peak heights of AI1/AII AI2/AII COOH/AII 0.08 Absorbance 0.06 COOHν ~1730 cm-1 0.04 0.02 0 3500 3000 2500 2000 1500 1000 500 0 Wavenumbers [1/cm]

  18. FT-IR CHARACTERIZATION Principal Component Analysis B.1, B.2, B.4 Score plot Formic acid procedure Neutralization procedure Loading plot DY42-HCl 1.5 Orange 1 DR202-HCl AI2/AII Red Red PC2 0 AI1/AII -1 0 1 Orange PC2 (29%) Leather 0.0 DB27-HCl DY42-HCl -2 0 2 4 -1 COOH/AII DR202-HCl Yellow Blue PC1 Blank Blue PCA Variables: AI1/AII, AI2/AII, COOH/AII Var. tot. = 98% Matrix: covariance Blank DO30-HCl DO30-HCl DB27-HCl Yellow -1.5 PC1 (69%)

  19. FT-IR CHARACTERIZATION Principal Component Analysis B.1, B.2, B.4 Score plot Formic acid procedure Neutralization procedure Loading plot 2 DY42-HCl 1 1.5 Orange 1 DR202-HCl AI2/AII Red Red PC2 0 AI1/AII -1 0 1 Orange PC2 (29%) Leather 0.0 DB27-HCl DY42-HCl -2 0 2 4 -1 COOH/AII DR202-HCl Yellow Blue PC1 Blank Blue PCA Variables: AI1/AII, AI2/AII, COOH/AII Var. tot. = 98% Matrix: covariance Blank DO30-HCl DO30-HCl DB27-HCl Yellow -1.5 PC1 (69%)

  20. FT-IR CHARACTERIZATION Principal Component Analysis B.1, B.2, B.4 Score plot Formic acid procedure Neutralization procedure Loading plot 2 DY42-HCl 1 1.5 Orange 1 DR202-HCl AI2/AII 1  High AI1/AII, AI2/AII Formic Acid procedure (and RED neutralization) Red Red PC2 0 AI1/AII -1 0 1 Orange PC2 (29%) Leather 0.0 DB27-HCl DY42-HCl -2 0 2 4 -1 COOH/AII 2  Low AI1/AII, AI2/AII Neutralization procedure (and DB27-HCl and blue formic acid procedure) DR202-HCl Yellow Blue PC1 Blank Blue PCA Variables: AI1/AII, AI2/AII, COOH/AII Var. tot. = 98% Matrix: covariance Blank DO30-HCl DO30-HCl DB27-HCl Yellow -1.5 PC1 (69%)

  21. FT-IR CHARACTERIZATION Principal Component Analysis B.1, B.2, B.4 DY42-HCl Formic acid DY42-HCl Neutralization AMIDE II INCREASES

  22. COLLAGEN CROSS-LINKING FT-IR B.1, B.2, B.4 ~1654 cm-1/~1690 cm-1 Collagen cross-linking type Dehydro-dihydroxy-norleucine (deH-DHLNL) Pyridinoline (Pyr)

  23. COLLAGEN CROSS-LINKING FT-IR B.1, B.2, B.4 Commercial Naturalised Naturalised dyes Rich in Pyr type cross-linking

  24. COLLAGEN CROSS-LINKING FT-IR B.1, B.2, B.4 Naturalised dyes 5%, 10%, 15% Same behavior of commercial dyes 2%

  25. COLLAGEN CROSS-LINKING TGA B.1, B.2, B.4 Gas: N2 200 mL/min Heating: 30-700°C, 10 °C/min

  26. COLLAGEN CROSS-LINKING TGA B.1, B.2, B.4 T02 Tonset T01 % fin

  27. COLLAGEN CROSS-LINKING TGA B.1, B.2, B.4 Naturalised 2% T02 Commercial 2% Tonset Naturalised 15% T01 % fin

  28. FUTURE ACTIONS B.1BIOKIMICA, INESCOP, ICCOM-CNR (0-6 months) Demonstration of the use of traditionalchemicalaciddyes in leatherdyeing HPLC-DAD  characterization of dyes bath and washing solutions GC-MS characterization of the volatile fraction of the dyedleather C.1ICCOM-CNR, UNIFI, INESCOP, BIOKIMICA (0-12 months) Monitoring on the enviromental impact of aciddyeswithinleather manufacture Atomicspectroscopy determination of the metal content of dyeingwastewaters (Cr, Co, Cu, Fe)

  29. BIONAD PEOPLE @ ICCOM-CNR, PISA Emilia Bramanti Alessandro D’Ulivo EmanuelaPitzalis DavidePellegrini Massimo Onor Manuela Cempini

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