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1 !"# $ %&' ("""$! )&' ("""$! Test report Direct Dyes Reactive Dyes

2 1 Direct Dyes Direct Dyes Development of reliable and safe processes To evaluate the effectiveness of the system as a support for the optimum processes investigation, we executed the trials using a standard recipe with different dyeing processes. Standard recipe: Direct Orange 2GL (CI 39) 0,2% Direct Rubine BL (CI 83) 0,3% Direct Grey GLL (CI 112) 0,5% Trial 5 Direct Dyes on cotton, salt three times at low 1/3 th salt added, running for 10 1/3 th salt added, running for 10 1/3 th salt added, running for 10 Heating to 100 C, gradient 1 C/1, for 30 Cooling at 80 C Trial 7 Direct Dyes on cotton, salt dosed in 20 at high Heating to 100 C, gradient 1 C/1 Salt added in 20, running 10 Pause for 30 Cooling at 80 C Trial 6 Direct Dyes on cotton, salt three times at high Heating to 100 C, gradient 1 C/1 1/3 th salt added, running for 10 1/3 th salt added, running for 10 1/3 th salt added, running for 10 Pause for 30 Cooling at 80 C Trial 8 Direct Dyes on cotton, dosing salt at high until maximum exhaustion is obtained. Heating to 100 C, gradient 1 C/1 Salt added in 40, running 10 Pause for 30 Cooling at 80 C

3 Understanding the relations between dyes To evaluate the behaviour of a trycromie under different concentrations of the dyes of the recipe we used the following recipes: Recipe 9: Direct Orange 2GL (CI 39) 0,2% Direct Rubine BL (CI 83) 0,3% Direct Grey GLL ( CI 112) 1.0% Recipe 10: Direct Orange 2GL (CI 39) 1,0% Direct Rubine BL (CI 83) 0,3% Direct Grey GLL (CI )112 0,2% Trial 9 Direct Dyes on cotton, salt three times at low 1/3 th salt added, running for 10 1/3 th salt added, running for 10 1/3 th salt added, running for 10 Heating to 100 C, gradient 1 C/1, for 30 Cooling at 80 C Trial 10 Direct Dyes on cotton, salt three times at low 1/3 th salt added, running for 10 1/3 th salt added, running for 10 1/3 th salt added, running for 10 Heating to 100 C, gradient 1 C/1, for 30 Cooling at 80 C

4 Graph 1 Direct Dyes on cotton, salt three times at low Graph 4 Direct Dyes on cotton, dosing salt at high until maximum exhaustion is obtained Graph 2 Direct Dyes on cotton, salt three times at high Graph 5 Direct Dyes on cotton, salt three times at low Graph 3 Direct Dyes on cotton, salt three times at high Graph 6 Direct Dyes on cotton, salt three times at low

5 2 Conclusion These dyeing demonstrate how different introductions of salt can strongly influence the dyebath behaviour. Dosing the salt before heating seems to conduct to a better exhaustion development during the process. Nevertheless also the other trials suggest interesting considerations, the dosing at high leads in the 6 th case to a violent exhaustion that could be dangerous, also dosing the salt bring to really high exhaustion rates, so the dosing at high should be done with extreme care. The 8 th test shows that a higher quantity of salt can increase the recipe s strength. At last the trials 9 and 10 demonstrate that different ratio between the dyes of the recipe can conduce to different exhaustion, this can be interesting to understand if a colour is effectively more or less substantive in different conditions of concentration and if the thermal cycle is effective with that recipe. Comparing the 9 th and the 10 th graphs we can deduce, looking at the exhaustion ratios at the ending of the dyeing, that the thermal cycle is not suitable in the first case while is optimal in the second.

6 3 Reactive Dyes Reactive Dyes Development of reliable and safe processes To evaluate the effectiveness of the system as a support for the optimum processes investigation, we executed the trials using a standard recipe with different dyeing processes. Standard recipe: YellowSumifix Supra HF-3R 1,0% Red Sumifix Supra HF-2B 0,8% Bleu Sumifix Supra HF-BG 1,5% The quantity of Sodium chloride utilized was 50g/l. Trial 11 Reactive Dyes on cotton, dyeing at 70 C, fixation with sodium carbonate at 60 C. Salt added, running for 10 Increase to70 C, gradient 3 C/1 for 30 Cooling at 60 C, pause for 10 Soda Ash 2g/l for 10 Soda Ash 5g/l for 10 Soda Ash 13 g/l for 60 Washing after dyeing: 1 Cool rinse 5 g/l of Acetic Acid, 1 Rinse at 70 C for 5, 1 Washing at 98 C for 10 with 1g/l of Zaiterol Final rinse Trial 12 Reactive Dyes on cotton, dyeing at 70 C, fixation with sodium carbonate and sodium hydroxide at 60 C. Salt added, running for 10 Increase to70 C, gradient 3 C/1 for 30 Cooling at 60 C, pause for 10 Soda Ash 1g/l for 10 Caustic Soda 1g/l for 10 Caustic Soda 2 g/l for 60 Washing after dyeing: 1 Cool rinse with 5 g/l of Acetic Acid, 1 Rinse at 70 C for 5, 1 Washing at 98 C for 10 with 1g/l of Zaiterol Final rinse

7 Trial 13 Reactive Dyes on cotton, dyeing at 70 C, fixation with alkaline buffer at 60 C Salt added, running for 10 Increase to70 C, gradient 3 C/1 for 30 Cooling at 60 C, pause for 10 Alkaline buffer Washing after dyeing: 1 Cool rinse with 5 g/l of Acetic Acid, 1 Rinse at 70 C for 5 1 Washing at 98 C for 10 with 1g/l of Zaiterol Final rinse Trial 14 Reactive Dyes on cotton, dyeing at 70 C, fixation with alkaline buffer at 60 C Salt added, running for 10 Increase to70 C, gradient 3 C/1 for 30 Cooling at 60 C, pause for 10 Dosing Alkaline buffer in 20 pause for 60 Washing after dyeing: 1 Cool rinse with 5 g/l of Acetic Acid, 1 Rinse at 70 C for 5 1 Washing at 98 C for 10 with 1g/l of Zaiterol Final rinse. Trial 15 Reactive dyes on cotton, dyeing at 70 C, fixation with Sodium carbonate at 70 C Salt added, running for 10 Increase to70 C, gradient 3 C/1 for 30 Soda ash 2g/l for 10 Soda ash 5g/l for 10 Soda ash 13g/l for 60 Washing after dyeing: 1 Cool rinse with 5 g/l of Acetic Acid, 1 Rinse at 70 C for 5 1 Washing at 98 C for 10 with 1g/l of Zaiterol Final rinse. Trial 16 Reactive dyes on cotton, Dyeing at 70 C, salt added and fixation at 70 C Increase to70 C, gradient 3 C/1 for 30 Salt added in 20, running for 10 Dosing of soda ash gradually in 20 Washing after dyeing: 1 Cool rinse with 5 g/l of Acetic Acid, 1 Rinse at 70 C for 5 1 Washing at 98 C for 10 with 1g/l of Zaiterol Final rinse.

8 Graph 7 Exhaustion graph trial 11 reactive dyes Observations: This process underlines the bleu dye substantivity respect the other dyes of the trichromie, nevertheless during the fixation phase all the trichromie works in a better way getting to a exhaustion ratio comprised between 92% and 84%. During the soaping process it is pointed out that the bleu component is effectively less fixed. Graph 8 Exhaustion graph trial 12 reactive dyes Observations: Also this process underlines the bleu dye substantivity respect the other dyes of the trichromie. The soaping phase point out that the quantity of fixed dye is slightly higher, in fact the quantity of dye discharged during the soaping is lower.

9 Graph 9 Exhaustion graph trial 13 reactive dyes Observations: The fast addiction, due to a mistake, of the alkaline solution carries to a violent exhaustion of the dyes presents in bath this could cause a differential fixation of the dyes between the inside and the outside of the bobbin. Graph 10 Exhaustion graph trial 14 reactive dyes Observations: As is outlined in this process the dosing of the alkaline solution helps to get to a more uniform exhaustion during the fixation period.

10 Graph 11 Exhaustion graph trial 15 reactive dyes Observations: With this trial it has been demonstrated the low influence of over the fixation ratio. Graph 12 Exhaustion graph trial 16 reactive dyes Observations: This test demonstrates how the process variables affect the exhaustion. As it s clear the exhaustion is really homogeneous and continue during the dyeing process further more it is possible to reduce the time of dyeing heating to 70 C at the highest speed conceded by the dyeing machine. Anyway this is not the perfect process because of the high substantivity exhaustion ratio reached with the addiction of salt, this result suggests to dose the salt with an exponential curve.

11 4 Conclusion The most significant data for the analysis of the system are the fixation degree and the homogeneity of the dyes build up. If with robustness of the dyeing class we intend the low influence to the dyeing variables (ph, Temperature ) variations around the ideal conditions, we can say that the degree of fixation is mainly function of the robustness of the dyeing class utilized and of the final values of the dyeing variables. The homogeneity of the build up is strictly dependent by the dermal proceeding of the dyeing and by the addictions of electrolytes and of basis during the dyeing process. Tests Relative disparity 16 0, , , , , Table: relative difference in process exhaustion. In this graph and in this table is lined out that the 16 th trial is better than the other as homogeneity.

12 5 Experiences Other cases Development of reliable and safe processes Follow other practical examples: Really substantive Blue Wrong type yellow

13 Other class of reactive dyes Wrong Type Red and soaping time

14 Low soluble acid dyes

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