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Journal of the Textile Institute
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Bio-scouring process optimization of wool fiber and wastewater utilization
Laijiu Zheng , Bing Du & Lili Wang
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Key Laboratory of Eco‐Textiles of Liaoning Province, Dalian Polytechnic University, Dalian 16034, China Available online: 24 Jun 2011

To cite this article: Laijiu Zheng, Bing Du & Lili Wang (2012): Bio-scouring process optimization of wool fiber and wastewater utilization, Journal of the Textile Institute, 103:2, 159-165 To link to this article: http://dx.doi.org/10.1080/00405000.2011.559023

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The Journal of The Textile Institute Vol. 103, No. 2, February 2012, 159–165

Bio-scouring process optimization of wool fiber and wastewater utilization
Laijiu Zheng*, Bing Du and Lili Wang
Key Laboratory of Eco-Textiles of Liaoning Province, Dalian Polytechnic University, Dalian 16034, China
Taylor and Francis

(Received 24 July 2010; final version received 26 January 2011 ) This paper is aimed at developing a method to optimize the wool-scouring process with bio-enzymes of Bacillus subtilis and Candida lipolytica. Good experimental conditions, first determined by single factor test, were the ratio of B. subtilis to C. lipolytica 1:4, temperature 40°C, pH 7.0, enzyme consumption 6%, bath ratio 1:35, and time 16 h. Based on these conditions, the Plackett–Burman design (P–B design) was used to determine the main influencing factors such as bath ratio, temperature, and time for enzymatic scouring. Then, a Response Surface Method (RSM) was used to optimize these factors, and the optimum parameters were solved with the quadratic regression equation: bath ratio 1:33.28, temperature 40.44°C, and time 18.11 h. Under these optimum conditions, the residual fat content in bio-scoured wool was 0.75%. Furthermore, the wool surface was smoother and cleaner than the non-optimized one. In addition, the lanolin was reclaimed as a valuable material in industry by centrifugation from wastewater, and it could reduce the content of organic substance to decrease the environmental pollution. Moreover, the residual lanolin, perspiration, dung, chaffy, short wool, and silt were utilized to make ecological organic fertilizer by compost treating. It could achieve the complex utilization of bio-scouring wastewater. Keywords: bio-scouring; wool fiber; Plackett–Burman design; Response Surface Method; wastewater utilization

10.1080/00405000.2011.559023

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Introduction Water- and organic-solvent-scouring methods had been widely applied in textile preliminary working. However, the high scouring temperature (60–90°C) wasted too much heat energy in an aqueous-scouring process, and there was too much organic solvent to disposal in the solvent-scouring wastewater (Atichart, Citapar, Kejvalee, & Mali, 2008; Christoe, 2006). Moreover, the content of lanolin in some kinds of lamb homegrown was very low, so it was difficult to be reclaimed from the scouring wastewater. Scouring with organic solvent could reclaim lanolin effectively, but it was not popularized due to the high investment for device (Pool & CordRuwisch, 2004). Recently, there were some reports about ultrasonic technology used in scouring process, but the scouring fiber was poor in whiteness and smoothness, and the production cost was very high (Guo & Zhang, 2006). In the present work, enzyme was widely applied in the wool textile industry, and results on bio-anti-shrinking, bio-modifying, bio-finishing, etc. were obtained (El-Sayed, Hamed, Kantouch, & Heine, 2002; El-Sayed, Kantouch, & Heine, 2001; Gaffar, Maria, Guillem, & Tzankov, 2009; Wang et al., 2009). However, little attention was put on the research of bioscouring due to few alternative enzymes, low enzyme activity, and poor stability. In order to solve above
*Corresponding author. Email: fztrxw@dlpu.edu.cn
ISSN 0040-5000 print/ISSN 1754-2340 online Copyright © 2012 The Textile Institute http://dx.doi.org/10.1080/00405000.2011.559023 http://www.tandfonline.com

problems, the present work proposed a new bio-scouring process in which Bacillus subtilis (the enzyme produced by it was named as Enzyme 1 in the following) and Candida lipolytica (the enzyme produced by it was named Enzyme 2 in the following) were used as scouring bacteria. Both enzyme solutions in scouring process were obtained in our biochemical laboratory. We screened the bacteria and fermented them to secret enzyme, and then separated them by centrifugation. The supplement amount of enzymes and the ratio of Enzymes 1 to 2 were optimized. The optimum condidtion for bio-scouring would be determined by the Plackett–Burman design (P–B design) in combination with the response surface method (RSM), and this could provide some data for pilot and commercial scouring scale in the further research.

Experimentals The wool fiber was Australian wool (60 s), provided by Fuxin Chaoyi Co. Ltd. The fiber (20 g) was put in enzymatic washing solution in 2000-ml beaker and vibrated at 58°C for infiltration, and then was transferred to another beaker containing the washing solution for scouring. After that, the scoured wool fiber was rinsed at 52–56°C. The different ratios of Enzymes 1 and 2

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Table 1. Term RFC (%) Fracture strength (cN) Whiteness Effect of wool fiber treated by enzyme.
Enzyme 1

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were supplemented in the washing solution and different percent of enzyme was selected for detection. The single factor tests were carried out to investigate the influences of temperature, pH, bath ratio, and time on the bio-scouring. The ranges of temperature, pH, bath ratio, and time were 25–50°C, 5–10, 1:20– 1:45, and 4–24 h, respectively. Then, the scouring process was further optimized by using P–B design in combination with RSM. P–B design was a statistical methodology, which was used to determine significance of all factors to response variable. Hadamard Matrix was used in P–B design, and there were N–1 factors in an N times test, in which N–4 were actual factors and three fictional variables to calculate the error. In this research, X1 − X5 were actual factors, and X6 − X8 were fictional variables. The influence of enzyme addition, temperature, pH, bath ratio, and time on Residual Fat Content (RFC, Chinese National Standard, GB6977-86, 1986c) was investigated with P–B design. Each independent factor was tested at a high (+1) level and a low (−1) level. The two levels are enzyme amount (X1): 6% and 8%; pH (X2): 6.0 and 7.0; bath ratio (X3): 1:30 and 1:35; temperature (X4): 38°C and 40°C; time (X5): 16 and 20 h. Eight experimental runs were carried out. Two dummy factors were used to estimate the experimental error and check the adequacy of the first-order model. The calculation software SPSS (version 17.0) was used for the regression analysis of the experimental data. The quality of fit of the first-order model equation was expressed by the coefficient of determination R2, and its statistical significance was determined by an F-test. The significance of the regression coefficients was tested by a t-test. Results and discussion Complex enzymes for bio-scouring The Enzyme 1, Enzyme 2, and Enzymes 1 + 2 were tested for its scouring and the results were shown in Table 1. Enzyme 1 was produced by B. subtilis that mainly had protease and lipase activity to remove contaminants of protein and fat, and Enzyme 2 was produced by C. lipolytica that was used mainly for degreasing. The results indicate that the fiber treated by the complex of Enzymes 1 and 2 both had the lowest RFC, and no significant differences happened in fracture strength while the whiteness was increased. So the complex of Enzymes 1 + 2 was better for scouring wool fiber. Further, the different ratios of Enzymes 1 and 2, listed in Table 2, were used to scour wool fiber. It could be seen that the highest efficiency of wool cleaning was obtained at the ratio of Enzyme 1 to Enzyme 2 being 1:4, which indicated that the enzyme produced by C. lipolytica played a dominant role in bio-scouring process.

Enzyme 2 2.34 7.45 67.8

Enzyme 1+2 1.79 7.39 68.9

2.86 7.42 66.5

Note: Whiteness: testing method of whiteness of wool fiber (GB/T 5885-1986; Chinese National Bureau of Standard, 1986a). Fracture strength: Testing method of whiteness of wool fiber (GB/T 12411.290; Chinese National Bureau of Standard, 1986b).

Table 2.

Effect of mixture ratio on the RFC. 1:1 1:2 1:3 1:4 1:5 1:6

Enzyme 1:Enzyme 2

RFC (%) 1.78 1.45 1.27 1.13 1.19 1.24 Enzyme 2:Enzyme 1 1:1 2:1 3:1 4:1 5:1 6:1 RFC (%) 1.78 1.56 1.48 1.61 1.73 1.89

Figure 1.

Effect of enzyme consumption on the RFC.

The effect of enzyme amount on RFC was also investigated (Figure 1). The RFC was inversed along with the enzyme amount added in washing solution. From the viewpoint of production cost, enzyme consumption was 6% (volume ratio of enzyme and water), was chosen as the suitable enzyme amount.
Figure 1. Effect of enzyme consumption on the RFC.

Single factor test A series of single factor tests were carried on at different conditions by changing temperature, pH, bath ratio, and time. It is indicated from Figure 2 that the RFC of cleaned wool was lowest when scoured at 40°C and pH 7.0. Furthermore, the RFC increased with the bath ratio or time at the beginning and then did not keep this tendency until bath ratio and time reached 1:35 and 16 h, respectively. Therefore, this better condition was determined through single factor test.
Figure 2. Scouring effect of single factor test.

Bio-scouring process optimization Base on the single factor test, P–B design was applied to study on of the RFC, where enzyme consumption

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Table 3. Run X1 1 2 3 4 5 6 7 8 1 −1 −1 1 −1 1 1 −1 X2 1 1 −1 −1 1 −1 1 −1 X3 1 1 1 −1 −1 1 −1 −1 Plackett–Burman design and its results, Factors X4 −1 1 1 1 −1 −1 1 −1 X5 1 −1 1 1 1 −1 −1 −1 X6 −1 1 −1 1 1 1 −1 −1 X7 −1 −1 1 −1 1 1 1 −1 X8 1 −1 −1 1 −1 1 1 −1

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Y (%) 0.89 0.91 0.96 0.98 0.94 0.84 0.93 0.87

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Notes: X1, enzyme consumption; X2, pH; X3, bath ratio; X4, temperature; X5, time; X6−X8, vacant factors.

scoured wools. It was obtained by a first-order model equation fitting, and was expressed as: Y = 0.915 – 0.005X1 + 0.003X2 – 0.015X3 + 0.030X4 + 0.028X5 This fit of the model was checked by the coefficient of determination R2, which was calculated to be 0.9935, indicating that 99.35% of the variability in the response could be explained by the model. The t-test was further used to identify the effect of every factor on fat content (Table 4). It indicated that X3, X4, and X5 are the greatest important factors that should be further optimized. While the factor X1 was selected as a low level (−1) and X2 was chosen as a high level (+1) according to the experiment results, which were 6% of enzyme consumption and 7.0 of pH. The relationship between predicted response Y and process variables Xi was unknown in most of RSM problems. Here, the process variables and fast optimize response could be carried out by a minimum of experiments. It could be seen that the surface of scoured wool was cleaner and smoother than that of the traditional process. Based on the first-order model equation obtained and the three important factors above, the path of steepest ascent was determined to find proper direction of changing variables increasing or decreasing the concentration according to the sign of the main effects to
Table 4. Figure 2. Scouring effect of single factor test. Factor Enzyme dosage pH Bath ratio Temperature Time Regression analysis of the effect of every factor. t-value −2.0000 1.0000 −6.0000 12.0000 11.0000 p > |t| 0.1835 0.4227 0.0267 0.0069 0.0082 Significant level (%) 81.65 57.74 97.33 99.31 99.18

(X1), pH (X2), bath ratio (X3), temperature (X4), and time (X5) were considered. Each factor had two levels: high level represented by +1 and low level by −1, as listed in Table 3, where X6 − X8 represented vacant factors and Y was the reponse value representing fat content of

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Experimental design and results of steepest ascent. Table 7. No. 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 Central composite design and results. X1 −1 −1 −1 −1 1 1 1 1 −1.682 1.682 0 0 0 0 0 0 0 0 0 0 X2 −1 −1 1 1 −1 −1 1 1 0 0 −1.682 1.682 0 0 0 0 0 0 0 0 X3 −1 1 −1 1 −1 1 −1 1 0 0 0 0 −1.682 1.682 0 0 0 0 0 0 Y 0.93 0.91 0.88 0.87 0.95 0.92 0.83 0.85 0.89 0.87 0.96 0.83 0.85 0.81 0.82 0.79 0.81 0.78 0.75 0.76

Step Bath ratio Temperature (°C) Time (h) Fat content (%) −2 −1 0 1 2 3 1:27 1:30 1:33 1:36 1:39 1:42 36 38 40 42 44 46 14 16 18 20 22 24 0.96 0.89 0.83 0.92 1.18 2.36

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improve fat content. The designed results of the path of steepest ascent experiments are shown in Table 5, from which the lowest response is 0.83% under the bioscouring conditions of bath ratio 1:33, temperature 40°C, and time 18 h. The central composite design (CCD) was conducted in the optimum vicinity to locate the true optimum concentrations of bath ratio (X1), temperature (X2), and time (X3) for fat content. CCD was a second-order design of response method in common usage. It made up by cube point, center point, and star point, which seemed as five-level factorial test. The test time was increased exponentially by the increasing of number of factors. The levels of the variables for the CCD were shown in Table 6. The design matrix and the corresponding experimental data were shown in Table 7. The response value Y of fat content of CCD design was fitted with the second-order equation: Y2 = 0.784 – 0.0054X1 – 0.0365X2 – 0079X3 + 0.0376X12 + 0.0429X22 + 0.0199X32 – 0.0125X1X2 + 0.0025X1X3 – 0.0075X2X3 The fit of the model was also checked by the determination coefficient R2 that is equal to 0.9257, indicating that 92.57% of the variability in the response could be explained by the model. The significance of the regression coefficients of the model is shown in Table 8. The temperature and quadratic term had high significance on fat content. The interaction effects of each factor, however, had no significance. The relationship between the three factors wasn’t a simple linear relationship but the second relationship, and the interaction between each factor was very small that basically not affected each other in the
Table 6. Level and code of experiment variables. Coded level Factor Bath ratio Temperature Time Coded −1.682 Xl X2 X3 −1 0 1 1.682

experiment. The contour plots described by the model equation (Y2) were represented in Figure 3. The minimum fat content reached 0.8% approximately. Finally, the optimal scouring conditions were 1:33.28, 40.44°C, and 18.11 h for bath ratio, temperature, and time, respectively, at which a minimum response of 0.78% fat content was given. This optimum condition was then verified, and the experimental result showed that the fat content of scoured wools was 0.75%. The well correlation between predicted and measured values justifies the validity of the response model. The clarity of wool surface was observed with scanning electronic microscope (SEM), as shown in Figure 4. It could be seen that the scoured surface was
Figure 3. The 3D and contour plot of response surface.

Table 8. Parameter X1 X2 X3 X12 X22 X32 X1X2 X1X3 X2X3

Regression coefficients of the regression equation. Value −0.0054 −0.0365 −0.0079 0.0376 0.0429 0.0199 −0.0125 0.0025 0.0075 SD 0.0062 0.0062 0.0062 0.0061 0.0061 0.0061 0.0082 0.0082 0.0082 t-value −0.863622 −5.848095 −1.258139 6.190131 7.062666 3.281681 −1.532365 0.306473 0.919419 Prob > |t| 0.408032 0.000162 0.236924 0.000103 0.000034 0.008265 0.156436 0.765530 0.379520

1:29.636 1:31 1:33 1:35 1:36.364 38.318 39 40 41 41.682 16.318 17 18 19 19.682

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Figure 3.

The 3D and contour plot of response surface.

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Complex utilization of bio-scouring wastewater The bio-scouring wastewater contained much lanolin, perspiration, dung, chaffy, short wool, and silt, with the content of lanolin 5–20 g/L and COD 4 × 104 to 6 × 104 mg/L. Because the lanolin was a valuable material in many industries, it was necessary to extract lanolin from the wastewater, and it could reduce the content of organic substance to decrease the environmental pollution. We reclaimed the lanolin by centrifugation. Firstly, we separated the big solid particles from wastewater by centrifugal machine and heated it to 80–85°C in heating kettle, and then reclaimed the lanolin by supercentrifuge. The extraction rate was 50–60% by this method. After lanolin extraction, there were some remaining lanolin, perspiration, dung, chaffy, short wool, and silt. We utilized them to make ecological organic fertilizer by compost treating, and optimized the content of nutrient substantce through the metabolism of microorganism. It could achieve the complex utilization of bioscouring wastewater.
Figure 4. SEM comparison of wool fiber.

Conclusions Bio-scouring process of wool fiber was optimized with the Plackett–Burman design and the RSM. The enzyme with good bio-scouring effect was a combination of B. subtilis and C. lipolytica, and the ratio of the former to latter was 1:4. The optimum process parameters were determined using this combined enzymes, and they were 6% of enzyme consumption, 7.0 of pH, 1:33.28 of bath ratio, 40.44°C of temperature, and 18.11 h of time. Under this condition, the fat content of bioscoured wools was only 0.75%, which reduced to 0.31% compared to that of non-optimized condition. Furthermore, the lanolin was reclaimed as a valuable material in industry by centrifugation from wastewater. In addition, the residual lanolin, perspiration, dung, chaffy, short wool, and silt were utilized to make ecological organic fertilizer by compost treating. It could achieve the complex utilization of bio-scouring wastewater.

Figure 4.

SEM comparison of wool fiber.

Acknowledgements
This project was funded by Liaoning Accented Project (2009223005) and Liaoning Innovative Team Project (LT2010010).

very clean and smooth, and the definition was comparable with that scoured with traditional process. It was noted that there still exist crack and tilte at the wool scales (Figure 4(c)). Due to that, they were subjected to be damaged and blunted with enzyme treatment. But both surface performance and capillarity effect of wool fiber under this bio-scouring were improved greatly.

References
Atichart, T., Citapar, K., Kejvalee P., & Mali, H. (2008). Process modification in the scouring process of textile industry. Journal of Cleaner Production, 16, 152–158.

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