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Silk reeling of silkworm cocoon in strongly alkaline electrolyzed water as a sericin swelling
agent at low temperature
Ting-Ting Cao, Yuan-Jing Wang and Yu-Qing Zhang*
Silk Biotechnology Laboratory, School of Biology and Basic Medical Sciences, Soochow University, Suzhou, P.R. China
(Received 25 April 2013; accepted 15 July 2013)
Strongly alkaline electrolyzed water (SAEW) was used as a sericin swelling agent for silk reeling from cocoons of the
silkworm Bombyx mori. Tap water was electrolyzed with a laboratory-made combined water electrolyzer to generate
SAEW with pH 11.50. The hardness of SAEW was 30% less than that of the tap water, whereas the concentrations of
Na+ in SAEW were 18% higher than those in the tap water. The pH of the SAEW was stable for at least a month in an
airtight container. Cocoons were immersed in pH 11.50 SAEW for 15 min with shaking, which replaces one step of the
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complex cocoon cooking process in the traditional reeling method (TRM) where penetration is achieved by repeatedly
alternating high and low temperatures. The swollen cocoons were transferred into fresh pH 11.50 SAEW for reeling at
the same, or slightly lower, temperature. The sericin loss from the whole cocoon in pH 11.50 SAEW is about 3.5% and
the tensile property of the single silk fibroin filament is similar to or better than that of TRM. Silk reeling in SAEW
involves only one step of cocoon swelling in pH 11.50 SAEW (70°C), which replaces a series of complex processes
including water penetration, water absorption, swelling, and then silk reeling in the TRM. A novel low-temperature and
simple reeling technology suitable for development by the silk industry is described.
Keywords: silk reeling; cocoon cooking; sericin; strongly alkaline electrolyzed water; low temperature
complex process of cocoon drying and cooking (Hisashi, diagramatically in Figure 1. The tap water runs directly
1984). However, cocoon cryopreservation substantially into the electrolyzer for the preparation of SAEW and
increases the cost of silk reeling. A pineapple extract rich the pH is adjusted by controlling the flow rate of the tap
in cysteine proteinases was used as an effective agent for water. The SAEW is purified by passage through a filter
the cocoon cooking and reeling of oak tasar (Antheraea to remove the white precipitate and any suspended
proylei J.) (Singh, Devi & Devi, 2003). There have been substance before storage in an airtight container.
studies of Antheraea mylilla cocoonase and its use in
silk preparation (Prasad, Pandey, & Sinha, 2012). Chen,
Li, Shen, Wei, and Xu (2010) bred a new variety of Traditional reeling method
mulberry cocoon with less sericin in the cocoon and The traditional reeling method (TRM) is basically the
tried to achieve cocoon cooking and reeling at a lower same as that used by an automated reeling machine in a
temperature of 80°C. No method of cocoon cooking and modern silk industry. The process involves water absorp-
reeling raw silk superior to that currently used commer- tion or penetration into the cocoon layer for sericin
cially has been reported. A decade ago, Japanese work- swelling. Therefore, TRM was selected as the control for
ers investigated the use of tap water and the addition of a reeling experiment with a hand-reeled method often
an electrolytic accelerator or mineral salts to tap water to used in the laboratory. Male cocoons were selected for
generate alkaline electrolyzed water for silk degumming the experiment (Zhang et al., 2010). The steps in the
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(Junich, 1998; Kie, 2001; Kim, Chung, & Lee, 2005; TRM are shown in Figure 2. Silkworm cocoons were
Kim, Kwon, Lee, & Woo, 2001; Tsukasa & Takashi, immersed in boiling water (500–800 mL) and incubated
2007), but there has been no report of the use of at 100°C for 1.5 min with shaking (80–100 rpm) to
electrolyzed tap water for cocoon cooking and reeling. remove air from the cocoon shells, transferred into water
In the present study, a laboratory-made combined water at 65°C and kept there for 2.5 min, transferred into water
electrolyzer was used for the electrolysis of tap water to at 100°C and kept there for 2.0 min, and transferred to
generate alkaline pH-stable electrolyzed water in which an 80–90°C waterbath and kept there for 9.0 min.
the ordinary commercial cocoon layer can be swollen Finally, the cocoons were transferred into a 70°C
and penetrated rapidly at a lower temperature for a short waterbath for reeling. When reeling, the priorities of the
length of time before reeling. silk fiber were numbered by 100 cycles into one group
(100 cycles/group, 1125 m/cycle), and the reeled silk
Pt Anode
Ceramic Film
Pt Cathode
1st , 2 nd , 3 rd , 4 th , 5 th …… 10 th Group
SAEW Purification
Tap Water
SAEW pH11.50
Tensile property measurements of single filaments
An average values of 10 single filaments
Figure 1. A diagram of the laboratory-built water electrolyzer. Figure 2. TRM and sampling method.
504 T.-T. Cao et al.
fiber (often called raw silk) was initially marked by 1st, conditions for more than a month with very little change
2nd, 3rd … 10th groups. The values for the raw silk of pH. Elementary analysis showed that the hardness of
properties were calculated as: the filtered SAEW (pH 11.50) was reduced by 30% and
the Na+ concentration was 18% higher compared to
(1) Reelability (%) = [1/(number of thread troubles the values for the tap water. Therefore, the strong alka-
+ 1)] 100; linity of SAEW is mainly due to the high concentration
(2) Fineness of silk filament (Denier) = [raw silk of OH resulting from water electrolysis.
weight (dry)/ raw silk length (m)] 9000;
(3) Raw silk recovery (%) = [raw silk weight (dry)/
cocoon shell weight (dry)] 100; Effect of the pH of SAEW on silk reeling performance
(4) Reelable length (m) = reelability raw silk Cocoons were divided into five test groups (10 cocoons/
length (m). group) and immersed in SAEW with a pH of 10.00,
10.50, 11.00, 11.50, or 12.00, placed into a shaking
SAEW reeling method (120 rpm) water bath at 70°C, and kept there for 15 min
to allow water to penetrate rapidly into the cocoon shell
Silkworm cocoons were immersed in pH 11.50 SAEW
and induce sericin swelling. After transfer into SAEW
(1:30/W:V) at 70°C and incubated for 15 min with
with the same pH and temperature, the silk was reeled
shaking (120 rpm). The detailed steps are as follows. The
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Temperature effect
Tensile test
In order to find the optimum temperature for water
The three groups (3rd, 4th, and 5th groups) of marked penetration, cocoons in pH 11.50 SAEW were divided
raw silk were degummed in neutral soap solution as into five groups and one group was incubated at each
described (Gulrajani, 1992). The numbered order in test temperature, 60, 65, 70, 75, and 80°C, in a bath
cocoon would be not disrupted. Ten single silk fibroin fil- ratio (cocoons/SAEW) of 1:40 (w/v) with shaking.
aments (length 50 mm) taken randomly from 200 single After immersion for 15 min, the swollen cocoons were
filaments of each group were measured with a universal transferred into fresh pH 11.50 SAEW at the same
testing machine (VNCLSYJ-001, Instron model 3365; temperature and reeling was started. Table 2 gives the
Instron, Industrial Product Group, Grove, PA, USA). The effect of swelling temperature on the silk reeling results;
maximum load and the shift, energy, and tensile strain at it can be seen that the reeling scores at four temperatures
maximum load were calculated. (60–75°C) increased with increased temperature. At
70°C, reelability, fineness of silk filament, raw silk
recovery, and reelability length were maximal at 83.2%,
Results and discussion
SAEW preparation and water quality
Table 1. Effect of SAEW pH on silk reeling performance.
Tap water (pH 8) was electrolyzed to produce a total
of 36 L of pH 3.00 acidic electrolyzed water as washing Fineness of Raw silk
water with various antimicrobial properties (Fabrizio, SAEW Reelability silk filament recovery Reelability
Sharma, Demirci, & Cutter, 2002; Hotz, Linneweber, pH (%) (denier) (%) length (m)
Dohmen, & Konertz, 2004) and 20 L of pH 11.50 10.00 52.8 1.086 57.2 389.72
SAEW. The SAEW was passed through a filter to 10.50 66.1 1.807 73.7 553.48
remove the residue consisting of salts such as calcium 11.00 70.0 1.913 87.2 550.22
carbonate that are insoluble or only poorly soluble in 11.50 78.7 2.198 94.2 834.78
12.00 75.5 2.186 91.3 797.47
SAEW. The filtered SAEW was as transparent and clear
as the tap water and could be stored under airtight Note: The values are the average of reeling scores of 10 cocoons.
The Journal of The Textile Institute 505
Table 2. Effect of swelling temperature on silk reeling Bath ratio for cocoon swelling
performance.
In order to determine the effect of the volume of SAEW
Fineness on the swelling of sericin in the cocoon layer, the
of silk Raw silk cocoons were immersed in pH 11.50 SAEW at 70°C for
Temperature Reelability filament recovery Reelability 15 min at bath ratios of 1:10, 1:20, 1:30, 1:40, and 1:50
(°C) (%) (denier) (%) length (m) (w/v) and the results are given in Table 4. The effect of
60 44.8 1.156 74.5 375.68 the bath ratio on cocoon reeling scores was not clear.
65 66.0 1.906 89.6 638.79 There was no significant difference between the reelabili-
70 83.2 2.189 97.2 898.18 ty, fineness of silk filament, raw silk recovery, and reela-
75 80.3 1.975 90.2 801.82
bility length for bath ratios of 1:10 (w/v) or 1:50 (w/v).
80 72.2 1.865 87.6 708.52
Thus, the selection of the selected bath ratio of 1:20–40
Note: The values are the average of reeling scores of 10 cocoons. (w/v) should be properly justified in view of the values
shown in Table 4. Generally, we choose a slightly larger
bath ratio as a test to avoid frequently changing the
2.189 denier, 97.2%, and 898 m, respectively. Therefore,
SAEW reeling soup due to the accumulation of sericin
a swelling temperature of 70°C in pH 11.50 SAEW was
in SAEW. Therefore, a bath ratio of 1:40 was selected to
used in all reeling experiments except where noted
be used in the experiment except where noted otherwise.
otherwise.
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Fineness of Raw silk Note: The values are the average of reeling scores of 10 cocoons.
Time Reelability silk filament recovery Reelability
(min) (%) (denier) (%) length (m)
Table 5. Comparison of cocoon reeling scores between TRM
5 78.74 1.986 87.2 767.29 and SAEW reeling methods.
10 79.03 2.207 93.7 834.38
15 81.78 2.213 94.2 831.08 Fineness of Raw silk
30 80.04 2.209 93.6 846.37 Reeling Reelability silk filament recovery Reelability
60 80.62 2.189 93.8 850.86 method (%) (denier) (%) length (m)
120 79.75 2.203 92.9 842.63
180 79.46 2.167 90.7 838.80 TRM 76.85 1.97 87.24 717.89
240 78.88 2.106 91.2 831.26 SAEW 78.30 2.00 93.71 818.90
Note: The values are the average of reeling scores of 10 cocoons. Note: The values are the average of reeling scores of 10 cocoons.
506 T.-T. Cao et al.
Table 6. Loss of sericin and water absorption in the cocoon cooking and reeling process.
Reeling method Dry cocoon (g) Cooked cocoon (g) Water absorption (g) Sericin loss (g) Sericin loss (%)
TRM 8.94 ± 0.06 83.40 ± 5.75 74.46 ± 5.80 0.30 ± 0.06 3.36 ± 0.60
SAEW 8.85 ± 0.64 19.15 ± 0.21 10.30 ± 0.85 0.35 ± 0.07 3.95 ± 0.52
Table 7. Tensile property of single degummed fibroin filament swollen and reeled in SAEW.
SAEW/NS 3rd 6.007 0.518 4.300 0.136 0.178 0.023 45.601 1.662
SAEW/NS 4th 6.212 0.924 4.205 0.096 0.172 0.013 44.730 0.842
SAEW/NS 5th 5.790 0.247 5.526 1.499 0.196 0.027 52.188 5.664
SAEW/NS Mean 6.003 0.563 4.677 0.577 0.182 0.021 47.506 2.722
Note: TRM: traditional reeling method; SAEW: pH 11.50 SAEW reeling method; NS: neutral soap degumming method.
3.5% of the whole cocoon weight, which is less than a was not carried out. So, the duration of cocoon cooking
quarter of the total amount of sericin surrounding the at a lower temperature of SAEW is the key factor.
fibroin in the cocoon. This is why the tensile properties
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described here is that water penetrates into the cocoon Naik, S. V. & Somashekar, T. H. (2008). Effect of degree of
shell at a temperature lower than that used in the TRM. cocoon drying and cocoon cooking conditions on reeling
performance and quality of raw silk of Indian bivoltine
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