A method for low-strength loss modification finishing of cotton fabric by combining des with cellulase

By combining DES with cellulase, the problem of strength reduction in cotton fabrics during enzymatic modification was solved, achieving a cotton fabric modification and finishing method that efficiently improves softness and minimizes strength loss.

CN120099794BActive Publication Date: 2025-11-25JIANGNAN UNIV
View PDF 2 Cites 0 Cited by

Patent Information

Application Number
CN202510209739.1
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2025-02-25
Publication Date
2025-11-25
Estimated Expiration
2045-02-25

AI Technical Summary

Technical Problem

When using bio-enzymes to modify cotton fabrics, the cellulose molecular chains break, causing damage to the internal fiber structure of the fabric, resulting in a decrease in fabric strength and affecting subsequent use.

Method used

Cotton fabrics were treated with a combination of biodegradable eutectic solvent (DES) and cellulase. The process involved preparing a DES/buffer solution, soaking the cotton fabric in it, adding cellulase for enzymatic finishing, and then inactivating the enzyme at high temperature to obtain the modified cotton fabric.

Benefits of technology

While maintaining the surface modification effect of the fabric, it significantly reduces the fabric strength loss rate, improves softness and smoothness, and reduces the structural damage to the fabric by cellulase.

✦ Generated by Eureka AI based on patent content.

Smart Images

  • Figure CN120099794B_ABST
    Figure CN120099794B_ABST
Patent Text Reader

Abstract

A low-strength loss modification finishing method of cotton fabric combined with DES and cellulase, characterized in that the method comprises the following steps: mixing a buffer solution with a DES solvent, and preparing a DES / buffer solution through ultrasonic treatment, wherein the DES solvent is one of a neutral DES solvent, an acidic DES solvent and an alkaline DES solvent; immersing the cotton fabric in the DES / buffer solution, adding a cellulase preparation, and performing biological enzyme modification finishing; then, the obtained cotton fabric is subjected to high-temperature inactivation in a water bath, washed, and dried; the method uses a low eutectic solvent combined with cellulase to perform one-bath biological enzyme modification finishing on the cotton fabric, removes short fibers and hair on the surface of the fabric, improves the anti-pilling ability, is mild and efficient, and has a low fabric strength loss rate; compared with the cellulase treatment alone, the method has a shorter time consumption and a lower strength loss rate; the DES solvent used has a low cost, is biodegradable, and can be recycled, and meets the production requirements of environmental protection and sustainability.
Need to check novelty before this filing date? Find Prior Art

Description

TECHNICAL FIELD

[0001] The application relates to a low-strength-loss modification finishing method of cotton fabric combined with DES and cellulase, and belongs to the technical field of surface biological modification of cotton fabric by enzyme treatment. BACKGROUND

[0002] Cotton is an important variety of natural fiber, and is in the first place in the consumer market due to good moisture absorption and air permeability, softness, easy care and other characteristics, is the most widely used product in daily life, and varieties and styles have realized gradation, and are widely used in various clothing, bedding and home decoration products and the like. However, in daily wearing, due to the mutual friction of the fabric, short fibers on the surface of the fabric are easily broken and pulled out to form pilling, which affects the aesthetic property and comfort of the clothing. In order to further improve the softness and comfort of the pure cotton fabric, surface modification finishing (such as polishing, softening and the like) is adopted on the cotton fabric.

[0003] Due to the wide application of the cotton fabric and the continuous improvement of the living standard of people, the wearing comfort of the fabric, especially the touch comfort of the bedding, has become an important topic of basic research and application research. In recent years, the method for surface modification finishing of the cotton fabric mainly includes the following several ways: physical method, such as mechanical polishing, ultrasonic finishing and the like; chemical method, such as surface coating, softener treatment and the like; biological method, such as enzyme modification and the like. The physical and chemical methods not only have complex process, long treatment period, low production efficiency, large energy consumption, and the generated waste chemicals and waste water are difficult to recycle and pollute the environment, but also the severe mechanical action or the penetration of the chemicals will cause certain damage to the fabric and affect the performance. In comparison, the biological enzyme as a kind of green ecological and environmental protection material has mild catalytic reaction condition, high efficiency and specificity, can save a large amount of energy, and can be biodegraded, and is widely used in textile industrial processing in recent years. The surface modification finishing of the cotton fabric by the biological enzyme can make the surface of the treated fabric smooth, soft, smooth and delicate, and greatly improves the product added value. However, the biological enzyme will also penetrate into the inside of the fabric while breaking the surface cellulose molecular chain, which will affect the internal fiber structure of the fabric and cause the overall strength of the fabric to decrease, and greatly affects the subsequent use. SUMMARY

[0004]

Technical problem

[0005] The modification finishing of the cotton fabric by the biological enzyme will cause the biological enzyme to penetrate into the inside of the fabric while breaking the surface cellulose molecular chain, which will affect the internal fiber structure of the fabric and cause the overall strength of the fabric to decrease, and greatly affects the subsequent use. Therefore, there is an urgent need for a biological enzyme modification finishing method with small damage to the strength of the cotton fabric.

[0006]

Technical scheme

[0007] In order to solve the above technical problems, the application adopts biodegradable solvent DES combined with cellulase to modify and finish the cotton fabric, so as to reduce the strength loss of the fabric and meet the requirements of subsequent processing while ensuring a certain surface polishing or softening effect.

[0008] The first object of the application is to provide a method for modifying and finishing cotton fabric with low strength loss by combining DES with cellulase, comprising the following steps:

[0009] (1) Preparation of DES / buffer solution

[0010] The buffer solution is mixed with the DES solvent, and then ultrasonic treatment is performed to obtain the DES / buffer solution.

[0011] (2) Enzyme treatment

[0012] The cotton fabric is immersed in the DES / buffer solution, and then cellulase preparation is added to perform biological enzyme finishing, so as to obtain the finished cotton fabric.

[0013] (3) High-temperature inactivation

[0014] The modified and finished cotton fabric is subjected to high-temperature inactivation in a water bath, and then washed, dried and obtained.

[0015] In an embodiment of the application, the DES is one of neutral DES solvent, acidic DES solvent and alkaline DES solvent.

[0016] In an embodiment of the application, the preparation method of the DES solvent is as follows: the hydrogen bond donor and the hydrogen bond acceptor are mixed and heated and stirred until clear and transparent, so as to obtain the DES solvent; the temperature of heating and stirring is 80-100 DEG C; and the time of heating and stirring is 2-6 h.

[0017] The hydrogen bond donor is a compound capable of providing hydrogen atoms to form hydrogen bonds, and usually contains N-H or O-H bonds. The hydrogen atoms of the hydrogen bond donor can be covalently combined with atoms with strong electronegativity to form polar bonds. Due to the attraction of the electronegative atoms to the electrons, the hydrogen atoms of the hydrogen bond donor have a partial positive charge, so as to produce electrostatic interaction with the lone pair electrons in the hydrogen bond acceptor to form hydrogen bonds.

[0018] The hydrogen bond acceptor is a compound or element capable of accepting hydrogen bonds, and usually contains atoms with high electronegativity (such as oxygen, nitrogen or fluorine). These atoms contain lone pair electrons, which can attract the hydrogen atoms in the hydrogen bond donor through electrostatic interaction, so as to form hydrogen bonds.

[0019] In an embodiment of the application, the hydrogen bond acceptor of the neutral DES is one of choline chloride and betaine, and the hydrogen bond donor is one of glycerol, polyethylene glycol 200 and polyethylene glycol 600.

[0020] In one embodiment of the present application, the hydrogen bond acceptor of the acidic DES is one of choline chloride, betaine, and the hydrogen bond donor is one of acetic acid, formic acid, p-toluenesulfonic acid.

[0021] In one embodiment of the present application, the hydrogen bond acceptor of the basic DES is one of choline chloride, betaine, and the hydrogen bond donor is one of urea, ethylene glycol, 1,3-propanediol.

[0022] In one embodiment of the present application, in step (1), the molar ratio of the hydrogen bond acceptor to the hydrogen bond donor is 1:2 or 1:5.

[0023] In one embodiment of the present application, in step (1), the pH of the buffer solution is 4.3-6.3.

[0024] In one embodiment of the present application, in step (1), the pH of the buffer solution is preferably 5.3.

[0025] In one embodiment of the present application, in step (1), the buffer solution is selected from one of acetic acid-sodium acetate buffer (AA-SA), citric acid-sodium citrate buffer.

[0026] In one embodiment of the present application, in step (1), the DES solvent concentration of the DES / buffer solution is 5-30 wt%.

[0027] In one embodiment of the present application, in step (1), the ultrasonic treatment is until the buffer solution is uniformly mixed with the DES solvent.

[0028] In one embodiment of the present application, in step (2), the bath ratio (mass ratio) of the cotton fabric to the DES / buffer solution is 1:8-1:14.

[0029] In one embodiment of the present application, in step (2), the enzyme activity of the cellulase preparation is 500-1000 EGU / g, and the amount of the cellulase preparation is 2-4% o.w.f. of the cotton fabric.

[0030] In one embodiment of the present application, in step (2), the bio-enzyme finishing is performed at 45-55°C for 30-60 min.

[0031] In one embodiment of the present application, in step (2), the bio-enzyme finishing is performed by using a high-temperature colorimeter at a rotation speed of 20-40 r / min.

[0032] In one embodiment of the present application, in step (3), the temperature of the water bath high-temperature inactivation is 90-100°C, and the treatment time of the water bath high-temperature inactivation is 8-20 min.

[0033] The second object of the present application is to provide the modified cotton fabric prepared by the above method.

[0034] The third object of the present application is to provide the application of the above modified cotton fabric in the field of textiles.

[0035] In one embodiment of the present application, the field of textiles includes clothing and home textiles.

[0036] Advantages:

[0037] (1) The present application uses deep eutectic solvent (DES) combined with cellulase to modify and finish cotton fabric by one-bath bio-enzyme method. The preparation method of the deep eutectic solvent is simple and low in cost. The prepared deep eutectic solvent is biodegradable and can be recycled, which has the advantages of environmental protection and sustainability.

[0038] (2) The present application uses cellulase to catalyze the hydrolysis of cellulose molecular chains on the surface of cotton fabric, so that the cellulose molecular chains in the fabric are broken, the short fibers and hair on the surface of the fabric are removed, the anti-pilling ability of cotton is improved on the basis of keeping the performance unchanged, the softness of the fabric is improved, the stiffness is reduced, and the smoothness is improved, so as to improve the hand feeling style and touch comfort of the fabric, and further improve the wearability of the fabric.

[0039] (3) The present application uses DES combined with cellulase to modify and finish cotton fabric by bio-enzyme method. Compared with the fabric treated by single cellulase, the softness of the fabric is improved more obviously, and the strength loss rate of the fabric is lower in the same modification and finishing time, which is mild and efficient.

[0040] (4) The present application uses DES combined with cellulase to modify and finish cotton fabric by one-bath method. The softness effect is similar to that of 60 min of single enzyme treatment within 30 min, and the strength loss rate is reduced by about 5%. After 60 min of treatment, the strength loss rate of the fabric can be reduced by about 20%. BRIEF DESCRIPTION OF DRAWINGS

[0041] Figure 1 The test results of fabric softness and weft strength loss rate of cotton fabric treated in Example 1, Control Example 1, Control Example 2, Example 2, Control Example 3, Control Example 4.

[0042] Figure 2 The test results of fabric softness and weft strength loss rate of fabric treated by different types of DES combined with cellulase in Example 1, Example 3, Example 4, Example 5 and Example 6.

[0043] Figure 3 The test results of fabric softness and weft strength loss rate of fabric treated by different concentrations of DES combined with cellulase in Example 1 and Examples 7-9.

[0044] Figure 4The results of softness and weft strength loss rate test of cotton fabric treated by example 1, 10, 11 and control example 1, 2, 5, 6.

[0045] Figure 5 The scanning electron microscope images of the fabric obtained from example 1, control example 1 and control example 2; wherein (a) is control example 1, (b) is control example 2, and (c) is example 1.

[0046] Figure 6 The content of hydrolysis product in the reaction solution of example 1, control example 2, example 2 and control example 4. DETAILED DESCRIPTION

[0047] The fabric raw material used in the examples and comparative examples of the present application is pure cotton fabric. The cellulase preparation used is selected from Novozyme Celluclast 1.5L cellulase, Novozyme 8000L cellulase and Genencor CAN neutral cellulase.

[0048] The test method involved in the present application is as follows:

[0049] 1. Fabric style test method

[0050] The cotton fabric to be tested is equilibrated at a temperature of 21±1℃ and a relative humidity of 65±2% for 24 hours, and a circular sample with an area of 100cm 2 is cut. A PhabrOmeter fabric style instrument is used for testing. According to the thickness and mass of the sample, an additional pressure block is added. The softness, smoothness and stiffness indexes of the fabric are obtained by setting the test according to the thickness and area density of the fabric.

[0051] 2. Fabric mechanical property test

[0052] A YG(B)02226ET electronic fabric strength machine is used for strength test of the cotton fabric to be tested. The pre-tension is 2N, the starting tension value is 100N, the sample width is 50mm, the test clamping distance is 200mm, the tensile speed is 100mm / min, each sample is tested 5 times, and the average value is taken as the final result.

[0053] 3. Hydrolysis product release amount test

[0054] 250mg of anhydrous glucose is dissolved in deionized water to make up to 250ml. 2.0ml, 4.0ml, 6.0ml, 8.0ml and 10.0ml of the solution are taken and made up to 50ml respectively. 2.5ml of each of the above solutions is taken in a test tube. 2.5ml of 3, 5-dinitrosalicylic acid is added to each, and boiled for 5min. After cooling, the absorbance values of the above glucose solutions with different concentrations are measured at 520nm by ultraviolet spectrophotometry. The standard curve is drawn with absorbance and glucose content as the vertical and horizontal coordinates respectively.

[0055] The reaction residue after enzyme inactivation was centrifuged, 2.0 ml of the supernatant was taken, 3.0 ml of DNS reagent was added, boiled for 5 min, placed in a cold water bath, and diluted to 25 ml with deionized water. The absorbance was measured at 520 nm wavelength using a UV spectrophotometer. The obtained absorbance value was brought into the standard curve to obtain the corresponding release amount of hydrolysis product (reducing sugar).

[0056] 4. Fabric apparent morphology characterization

[0057] Before testing, the sample was sprayed with gold, and the changes in the surface morphology of the fabric before and after modification were observed using a SU1510 type scanning electron microscope. The accelerating voltage during the electron microscope scanning test was 5.0 kV, and the magnification was 35x, 900x and 2000x, respectively.

[0058] Example 1

[0059] A method for low-strength loss modification of cotton fabric by DES combined with cellulase, comprising the following steps:

[0060] (1) Preparation of DES solvent

[0061] The hydrogen bond donor and the hydrogen bond acceptor were mixed and heated and stirred at 80°C until clear and transparent, obtaining a neutral DES solvent ChCl-PEG 200 ; the hydrogen bond donor is polyethylene glycol 200, the hydrogen bond acceptor is choline chloride, and the molar ratio of the hydrogen bond acceptor to the hydrogen bond donor is 1:5;

[0062] (2) Preparation of DES / AA-SA solution

[0063] 0.05M acetic acid-sodium acetate buffer (pH=5.3) was mixed with the prepared DES solvent, and was treated by oscillation and ultrasonic treatment until homogeneous, to prepare a DES / AA-SA solution with a DES solvent concentration of 20wt%;

[0064] (3) Enzyme treatment

[0065] The cotton fabric was immersed in the DES / AA-SA solution, the bath ratio of the cotton fabric to the DES / AA-SA solution was 1:10, and 3.0%o.w.f of cellulase preparation (Novozymes Celluclast 1.5L cellulase, 700 EGU / g) was added, which was placed in a steel cup matched with a high-temperature colorimeter, and was subjected to biological enzyme modification by using a high-temperature colorimeter at 50°C and a rotation speed of 30r / min for 30min, to obtain the modified cotton fabric;

[0066] (4) High-temperature sterilization

[0067] The finished cotton fabric was taken out and put into deionized water, and then high-temperature inactivation was carried out in a water bath at 100°C for 10 min, and then the cotton fabric was washed under flowing water, and then dried at 60°C to constant weight, and then placed in a constant-temperature and constant-humidity chamber (21±1°C, 65±2%) for 24 h to obtain the modified cotton fabric.

[0068] Comparative Example 1

[0069] (1) The cotton fabric was immersed in the AA-SA solution, and the bath ratio of the cotton fabric to the AA-SA solution was 1:10, and then placed in a steel cup matched with the high-temperature colorimeter, and then treated by the high-temperature colorimeter at 50°C and a rotation speed of 30 r / min for 30 min.

[0070] (2) The cotton fabric prepared in step (1) was taken out and put into deionized water, and then high-temperature inactivation was carried out in a water bath at 100°C for 10 min, and then the cotton fabric was washed under flowing water, and then dried at 60°C to constant weight, and then placed in a constant-temperature and constant-humidity chamber (21±1°C, 65±2%) for 24 h.

[0071] Comparative Example 2

[0072] The difference from Example 1 is that steps (1) and (2) are not performed, and the DES / AA-SA solution in step (3) is replaced by 0.05M acetic acid-sodium acetate buffer solution (pH=5.3).

[0073] The cotton fabrics obtained in Example 1 and Comparative Examples 1 and 2 were subjected to performance testing, and the test results are as follows:

[0074] Table 1: Weft strength loss rate and style test results of the cotton fabrics obtained in Example 1 and Comparative Examples 1 and 2

[0075] Modified finished cotton fabric Example 1 Control Example 1 Control Example 2 Fabric weft strength loss rate (%) 15.09 1.59 22.73 Fabric softness 77.15 74.53 76.69 Fabric stiffness 26.38 29.00 27.46 Fabric smoothness 80.76 80.45 80.63

[0076] As can be seen from Table 1, the enzyme treatment (Comparative Example 2) improves the softness of the fabric to a certain extent, but further damages the weft strength. After the introduction of DES (Example 1), the structural damage caused by the cellulase to the inside of the fabric is weakened to a certain extent, and the strength loss rate of the fabric is reduced.

[0077] Example 2

[0078] The difference from Example 1 is that the reaction time of the biological enzyme modification finishing in step (3) is replaced by 60 min.

[0079] Comparative Example 3

[0080] The difference from Comparative Example 1 is that the treatment time of the high-temperature colorimeter is replaced by 60 min.

[0081] Comparative Example 4

[0082] The difference from Comparative Example 2 is that the high temperature colorimeter treatment time of 30 min is replaced by 60 min.

[0083] The obtained modified finishing cotton fabric is subjected to performance test, and the test results are as follows:

[0084] Table 2: Weft strength loss rate and style test results of cotton fabric obtained in Example 2 and Comparative Examples 3 and 4

[0085] Modified finished cotton fabric Example 2 Control Example 3 Control Example 4 Fabric weft strength loss rate (%) 20.68 2.16 38.85 Fabric softness 77.73 75.01 77.23 Fabric stiffness 25.91 28.87 25.37 Fabric smoothness 80.92 80.56 80.68

[0086] Table 2: Compared with Table 1, the treatment time is increased, the softening effect of the fabric is improved, and the strength loss is also greater. After the introduction of DES, similar softening results to the 60 min enzyme treatment alone can be achieved within 30 min, while the strength loss rate of the fabric is greatly reduced.

[0087] Figure 1 The breaking strength loss rate and softness of the cotton fabric obtained in Example 1, Comparative Example 1, Comparative Example 2, and Example 2, Comparative Example 3, and Comparative Example 4 are compared. As can be seen from the figure, the softness of the cotton fabric after enzyme treatment is improved, and the strength loss rate is significantly increased. After the introduction of DES, the softness of the fabric is improved, and the strength loss of the fabric is improved to a certain extent. Within 30 min, the strength loss rate is reduced by about 5%, and the modified finishing fabric after the introduction of DES can achieve similar softness to the 60 min enzyme treatment alone, and the strength loss rate of the fabric is reduced by nearly 25%. Within 60 min, the strength loss rate of the modified finishing cotton fabric treated is also reduced by about 20%. It can be seen that this method has a certain degree of improvement in treatment effect.

[0088] Example 3

[0089] A method for low strength loss modification and finishing of cotton fabric by DES combined with cellulase, comprising the following steps:

[0090] (1) Preparation of DES solvent

[0091] The hydrogen bond donor and the hydrogen bond acceptor are mixed and heated and stirred at 80°C until clear and transparent, obtaining a neutral DES solvent ChCl-PEG 600 ; the hydrogen bond donor is polyethylene glycol 600, the hydrogen bond acceptor is choline chloride, and the molar ratio of the hydrogen bond acceptor to the hydrogen bond donor is 1:5;

[0092] (2) Preparation of DES / AA-SA solution

[0093] 0.05M acetic acid-sodium acetate buffer (pH=5.3) is mixed with the prepared DES solvent, and is subjected to oscillation and ultrasonic treatment until mixed uniformly, to prepare a DES / AA-SA solution with a DES solvent concentration of 20wt%;

[0094] (3) Enzyme treatment

[0095] The cotton fabric was immersed in the DES / AA-SA solution, the bath ratio of the cotton fabric to the DES / AA-SA solvent was 1:10, and a cellulase preparation (Novozymes Celluclast 1.5L cellulase, 700 EGU / g) was added in an amount of 3.0% o.w.f of the cotton fabric, and the cotton fabric was placed in a steel cup matched with the high-temperature color matching machine, and the enzyme modification finishing was carried out at 50°C and a rotation speed of 30 r / min for 30 min by using the high-temperature color matching machine, to obtain the finished cotton fabric.

[0096] (4) High-temperature sterilization

[0097] The finished cotton fabric was taken out and placed in deionized water, and was high-temperature inactivated in a water bath at 100°C for 10 min, and was washed under flowing water, and was dried at 60°C to a constant weight, and was placed in a constant-temperature and constant-humidity chamber (21±1°C, 65±2%) for 24 h of balancing, to obtain the modified cotton fabric.

[0098] Example 4

[0099] A method for low-strength damage modification finishing of cotton fabric by using DES combined with cellulase, comprising the following steps:

[0100] (1) Preparation of DES solvent

[0101] The hydrogen bond donor and the hydrogen bond acceptor were mixed and heated and stirred at 80°C until clear and transparent, to obtain a neutral DES solvent Bet-Gly; the hydrogen bond donor was glycerol, the hydrogen bond acceptor was betaine, and the molar ratio of the hydrogen bond acceptor to the hydrogen bond donor was 1:2;

[0102] (2) Preparation of DES / AA-SA solution

[0103] 0.05M acetic acid-sodium acetate buffer (pH=5.3) was mixed with the prepared DES solvent, and was oscillated and ultrasonically treated until homogeneous, to prepare a DES / AA-SA solution with a DES solvent concentration of 20wt%;

[0104] (3) Enzyme treatment

[0105] The cotton fabric was immersed in the DES / AA-SA solution, the bath ratio of the cotton fabric to the DES / AA-SA solvent was 1:10, and a cellulase preparation (Novozymes Celluclast 1.5L cellulase, 700 EGU / g) was added in an amount of 3.0% o.w.f of the cotton fabric, and the cotton fabric was placed in a steel cup matched with the high-temperature color matching machine, and the enzyme modification finishing was carried out at 50°C and a rotation speed of 30 r / min for 30 min by using the high-temperature color matching machine, to obtain the finished cotton fabric.

[0106] (4) High-temperature sterilization

[0107] The finished cotton fabric was taken out and placed in deionized water, and then high-temperature inactivation was carried out in a water bath at 100°C for 10 min, and then washed under flowing water, and then dried at 60°C to constant weight, and then placed in a constant-temperature and constant-humidity chamber (21±1°C, 65±2%) for 24 h of balancing, to obtain the modified cotton fabric.

[0108] Example 5

[0109] The difference from Example 1 is that in step (1), the hydrogen bond donor is replaced by acetic acid to prepare the acidic DES solvent ChCl-AA, and the molar ratio of the hydrogen bond acceptor and the hydrogen bond donor is 1:2.

[0110] Example 6

[0111] The difference from Example 1 is that in step (1), the hydrogen bond donor is replaced by 1,3-propanediol to prepare the basic DES solvent ChCl-1,3-prop, and the molar ratio of the hydrogen bond acceptor and the hydrogen bond donor is 1:2.

[0112] Table 3: Weft strength loss rate and style test results of the cotton fabric obtained in Example 1 and Examples 3-6

[0113] Modified finished cotton fabric Example 1 Example 3 Example 4 Example 5 Example 6 Fabric weft strength loss rate (%) 15.09 20.52 14.98 20.38 18.73 Fabric softness 77.15 76.92 77.10 76.83 77.06 Fabric stiffness 26.38 26.07 27.02 27.11 26.26 Fabric smoothness 80.76 82.28 79.37 80.98 80.77

[0114] As can be seen from Table 3, the DES solvents prepared by using ChCl-PEG 200 (Example 1) and Bet-Gly (Example 4) have good softening effect and low strength loss rate in the one-bath bioenzymatic modification and finishing of cotton fabric, and Example 1 has the best effect.

[0115] Figure 2 Comparison of the breaking strength loss rate and softness of the cotton fabric obtained by the modification and finishing of different DES types combined with cellulase. As can be seen from the figure, ChCl-PEG 200 has the best comprehensive modification and finishing effect on the fabric.

[0116] Example 7

[0117] The difference from Example 1 is that in step (2), the DES solvent concentration of the DES / AA-SA solution is replaced from 20wt% to 5wt%.

[0118] Example 8

[0119] The difference from Example 1 is that in step (2), the DES solvent concentration of the DES / AA-SA solution is replaced from 20wt% to 10wt%.

[0120] Example 9

[0121] The difference from Example 1 is that the DES solvent concentration of the DES / AA-SA solution in step (2) is changed from 20wt% to 30wt%.

[0122] Table 4: Results of the loss rate of the strength and softness of the cotton fabric in the weft direction obtained by Examples 1 and 7-9

[0123]

[0124]

[0125] As can be seen from Table 4, with the increase of the DES concentration, the loss rate of the strength of the fabric gradually increases. When the concentration is 20%, the softness of the fabric increases higher and the loss rate of the strength is smaller. When the concentration is further increased, the softness has little difference and the loss rate of the strength increases. Therefore, the DES concentration of the DES / AA-SA solution is preferably 20%.

[0126] Figure 3 The loss rate of the breaking strength and the softness of the cotton fabric modified by the cellulase with different DES concentrations are compared. As can be seen from the figure, with the increase of the DES concentration, the loss rate of the strength also gradually increases and the softness also nearly shows a growth trend. When the concentration is increased from 20% to 30%, the loss rate of the strength shows a higher growth and the growth rate of the softness is slow.

[0127] Example 10

[0128] The difference from Example 1 is that the cellulase preparation Novozymes Celluclast 1.5L cellulase in step (3) is replaced by Novozymes 8000L cellulase.

[0129] Comparative Example 5

[0130] The difference from Comparative Example 2 is that the cellulase preparation Novozymes Celluclast 1.5L cellulase in step (3) is replaced by Novozymes 8000L cellulase.

[0131] Table 5: Results of the loss rate of the strength and softness of the cotton fabric in the weft direction obtained by Examples 1, 10, Comparative Examples 2 and 5

[0132] Modified finished cotton fabric Example 1 Control Example 2 Example 10 Control Example 5 Fabric weft strength loss rate (%) 15.09 22.73 17.95 20.11 Fabric softness 77.15 76.69 76.21 75.85 Fabric stiffness 26.38 27.46 28.01 28.41 Fabric smoothness 80.76 80.63 80.62 80.22

[0133] As can be seen from Table 5, although the Novozymes 8000L enzyme has a smaller damage to the strength of the fabric, the modification and finishing effect is also weaker. After the introduction of DES, the synergistic modification and finishing effect of the two is not as good as that of the Novozymes 1.5L cellulase. Therefore, the Novozymes Celluclast 1.5L cellulase is preferred.

[0134] Example 11

[0135] The difference from Example 1 is that the cellulase preparation Novozymes Celluclast 1.5L cellulase in step (3) is replaced by Genencor CAN neutral cellulase.

[0136] Comparative Example 6

[0137] The difference from Comparative Example 2 is that the cellulase preparation Novozymes Celluclast 1.5L cellulase in step (3) is replaced by Genencor CAN neutral cellulase.

[0138] Table 6 Cotton fabric weft direction strength loss rate and softness results obtained by Example 1, 11, Comparative Example 2, 6

[0139] Modified finished cotton fabric Example 1 Control Example 2 Example 11 Control Example 6 Fabric weft strength loss rate (%) 15.09 22.73 20.27 26.05 Fabric softness 77.15 76.69 77.25 76.03 Fabric stiffness 26.38 27.46 27.77 28.13 Fabric smoothness 80.76 80.63 80.51 80.38

[0140] As can be seen from Table 6, after the introduction of DES, the softness of Genencor CAN cellulase is improved higher, but the strength damage to the fabric is still large, and the improvement of strength and style cannot be well balanced, therefore, Novozymes Celluclast 1.5L cellulase is preferred.

[0141] Figure 4 The breaking strength loss rate and softness of the cotton fabric modified by different types of cellulase finishing are compared. As can be seen from the figure, after the introduction of DES, the strength loss rate of the fabric is decreased to a certain extent, and the softness is also improved. In terms of fabric style and strength loss, the improvement effect of Novozymes Celluclast 1.5L cellulase is the best.

[0142] But it can be seen that no matter which cellulase is introduced, the modification and finishing effect of cellulase on cotton fabric is improved to a certain extent, the strength loss rate is decreased, and the corresponding fabric style is also improved.

[0143] Figure 5 The scanning electron microscope images of Example 1, Comparative Example 1 and Comparative Example 2 are 35 times, 900 times and 2000 times respectively. As can be seen from the figure, the surface of the fabric without enzyme treatment is rough, and there are many short fibers distributed randomly. These short fibers are easy to rub and form pills during subsequent wearing. After cellulase modification and finishing, the short fibers on the surface of the cotton fabric are hydrolyzed, the protruding fibrils on the surface of the fabric are reduced, and the surface smoothness is improved. The improvement effect of the fabric surface after DES combined with cellulase treatment is more obvious.

[0144] Figure 6The amount of hydrolysis product after modification and finishing of Example 1 (DES-enzyme system, 0.5h), Control Example 2 (enzyme treatment alone, 0.5h) and Example 2 (DES-enzyme system, 1h), Control Example 4 (enzyme treatment alone, 1h) were compared. As can be seen from the figure, the content of reducing sugar in the reaction solution increased with the extension of enzyme treatment time, and the enzyme treatment reaction continued. The amount of reducing sugar produced by enzyme treatment alone within 30 min was higher, but as the reaction time increased, the difference between the two decreased, and the DES may have a stabilizing effect on cellulase. Due to the synergistic effect of DES and enzyme, the surface fiber short bristles can be more effectively hydrolyzed, the excessive hydrolysis during modification and finishing is reduced, the amount of hydrolysis product is reduced, and the internal structure of the fabric is effectively protected, reducing strength loss.

[0145] Example 12

[0146] The difference from Example 1 is that AA-SA is replaced by citric acid-sodium citrate buffer.

[0147] The strength loss rate and softening effect of the cotton fabric obtained in Example 12 are similar to those of acetic acid-sodium acetate buffer, and it can be seen that the type of buffer has less interference with the system, and only the corresponding pH environment needs to be provided. This scheme is suitable for various buffer systems.

[0148] The above examples provided are not intended to limit the scope covered by the present application, and the described steps are not intended to limit the order of execution. Those skilled in the art can make obvious improvements to the present application in combination with existing common knowledge, which also falls within the protection scope defined by the claims of the present application.

Claims

1. A method for low-strength loss modification finishing of cotton fabric with DES in combination with cellulase, characterized in that, It comprises the following steps: (1) Preparation of DES / buffer solution Mixing the buffer solution with DES solvent, and preparing DES / buffer solution by ultrasonic treatment; the DES solvent is one of neutral DES solvent, acidic DES solvent and basic DES solvent; (2) Enzyme treatment Immersion of the cotton fabric in the DES / buffer solution, and adding cellulase preparation to perform biological enzyme finishing to obtain the finished cotton fabric; (3) High-temperature inactivation Water bath high-temperature inactivation of the finished cotton fabric, washing, drying to obtain the modified cotton fabric.

2. The method of claim 1, wherein, In step (1), the preparation method of the DES solvent is mixing the hydrogen bond donor and the hydrogen bond acceptor, and heating and stirring until clear and transparent; The hydrogen bond acceptor is one of choline chloride and betaine; The hydrogen bond donor of the neutral DES solvent is one of glycerol, polyethylene glycol 200 and polyethylene glycol 600; The hydrogen bond donor of the acidic DES solvent is one of acetic acid, formic acid and p-toluenesulfonic acid; The hydrogen bond donor of the basic DES solvent is one of urea, ethylene glycol and 1,3-propanediol; The molar ratio of the hydrogen bond acceptor to the hydrogen bond donor is 1:2 or 1:

5.

3. The method of claim 2, wherein, In the preparation method of the DES solvent, the temperature of heating and stirring is 80-100℃; and the time of heating and stirring is 2-6h.

4. The method of claim 1, wherein, In step (1), the pH of the buffer solution is 4.3-6.3; the concentration of the DES solvent of the DES / buffer solution is 5-30wt%; and the buffer solution is one of acetic acid-sodium acetate buffer and citric acid-sodium citrate buffer.

5. The method of claim 1, wherein, In step (2), the bath ratio of the cotton fabric to the DES / buffer solution is 1:8-1:

14.

6. The method of claim 1, wherein, In step (2), the enzyme activity of the cellulase preparation is 500-1000 EGU / g; and the dosage of the cellulase preparation is 2-4% o.w.f of the cotton fabric.

7. The method of claim 1, wherein, In step (2), the biological enzyme finishing is performed at 45-55℃ for 30-60min.

8. The method of claim 1, wherein, In step (3), the temperature of water bath high-temperature inactivation is 90-100℃; and the treatment time of water bath high-temperature inactivation is 8-20min.

9. The modified cotton fabric prepared by the method of any one of claims 1-8.

10. The application of the modified cotton fabric of claim 9 in the field of textiles.

Citation Information

Patent Citations

  • Method for hydrophilic modification of polyester through DES ultrasonic pretreatment combined with enzyme

    CN117306241A

  • Acetylation-grade dissolving pulp as well as preparation method and application thereof

    CN118110053A