CN119121631B - Machine washable silk fabric and preparation method thereof - Google Patents

Machine washable silk fabric and preparation method thereof

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Publication number
CN119121631B
CN119121631B CN202411378347.XA CN202411378347A CN119121631B CN 119121631 B CN119121631 B CN 119121631B CN 202411378347 A CN202411378347 A CN 202411378347A CN 119121631 B CN119121631 B CN 119121631B
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China
Prior art keywords
silk
solution
machine washable
silk fabric
dopamine
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Active
Application number
CN202411378347.XA
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Chinese (zh)
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CN119121631A (en
Inventor
陈凤翔
童爱心
张玉
乔思杰
史芷丞
何安南
骆宇新
王梦琦
黄智宇
何俊
王斌昊
王佳馨
王庆淼
鱼水朋
王平
刘欣
徐卫林
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Yagor Fashion Co ltd
Wuhan Textile University
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Yagor Fashion Co ltd
Wuhan Textile University
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Priority to CN202411378347.XA priority Critical patent/CN119121631B/en
Publication of CN119121631A publication Critical patent/CN119121631A/en
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Publication of CN119121631B publication Critical patent/CN119121631B/en
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    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M15/00Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
    • D06M15/01Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with natural macromolecular compounds or derivatives thereof
    • D06M15/15Proteins or derivatives thereof
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M10/00Physical treatment of fibres, threads, yarns, fabrics or fibrous goods made from such materials, e.g. by ultrasonic waves, corona discharge, irradiation, electric currents or magnetic fields; Physical treatment combined with treatment with chemical compounds or elements
    • D06M10/04Physical treatment combined with treatment with chemical compounds or elements
    • D06M10/08Organic compounds
    • D06M10/10Macromolecular compounds
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M15/00Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
    • D06M15/19Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
    • D06M15/37Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M15/61Polyamines polyimines
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M16/00Biochemical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. enzymatic
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2101/00Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
    • D06M2101/02Natural fibres, other than mineral fibres
    • D06M2101/10Animal fibres
    • D06M2101/12Keratin fibres or silk
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2200/00Functionality of the treatment composition and/or properties imparted to the textile material
    • D06M2200/35Abrasion, pilling or fibrillation resistance
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2200/00Functionality of the treatment composition and/or properties imparted to the textile material
    • D06M2200/50Modified hand or grip properties; Softening compositions

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  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Biochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Microbiology (AREA)
  • Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
  • Chemical Or Physical Treatment Of Fibers (AREA)

Abstract

The application provides a method for preparing machine washable silk fabrics, which comprises the steps of cleaning silk cocoons, boiling for degumming, washing with water, drying to obtain silk fibers, dissolving the silk fibers in neutral salt solution, dialyzing to obtain silk fibroin solution, preparing dopamine solution, uniformly mixing the dopamine solution with the silk fibroin solution to obtain mixed solution, and finally performing rolling and baking treatment on the silk fabrics by using the mixed solution for 2-5 times by adopting the technological processes of padding, baking, washing and re-baking to obtain the machine washable silk fabrics. The application adopts the polydopamine protein coating with good biocompatibility, utilizes the hydrogen bond and electrostatic various acting forces among polydopamine, silk fibroin and silk fabrics, improves the mechanical strength, friction resistance and washing/machine washing resistance of the silk fabrics without changing the softness and comfort of the silk fabrics, and prolongs the nursing convenience and service life of the silk fabrics.

Description

Machine washable silk fabric and preparation method thereof
Technical Field
The application relates to the technical field of silk fiber surface modification, in particular to a machine washable silk fabric and a preparation method thereof.
Background
The silk fiber has good biocompatibility, and the silk fabric prepared by adopting the silk fiber as a raw material has smooth and glutinous hand feeling, softness and skin friendliness, good air and moisture permeability and good drapability, and is a high-grade fabric which is very representative in the field of textile and clothing. However, silk fibers are fragile in wet state, and are inferior in mechanical properties and chemical resistance (e.g., detergent) and are easily damaged and deformed. In modern life, along with the pursuit of people for high-quality and high-efficiency life, housekeeping has become a popular trend, household textiles are mostly cleaned by machine washing, but real silk fabrics are easily worn in machine washing, and the problems of fibrillation, wrinkling, shrinkage and the like are caused to influence subsequent use, so that hands are required to be completely liberated, and the machine washing resistance of the real silk fabrics is also required to be improved.
In the prior art, some researchers adopt a mode of coating polyurethane and polyester coatings on the surfaces of silk fabrics to improve, however, the mode not only leads silk fibers to lose natural soft texture and skin-friendly property, but also seriously increases the environmental burden of textiles due to the fact that the coating materials are difficult to recover and biodegrade, some researchers adopt resins to finish the silk fabrics, the crease resistance and ash injury resistance of the silk fabrics are improved, but the hydrophilia performance is obviously deteriorated, the hand feeling is obviously hardened, some researchers adopt acrylamide and chitosan citric acid to finish the silk fabrics, the crease resistance of the silk fabrics is improved, but the finishing mode needs high-temperature baking, the loss of fibers is easily caused, and the color of the fabrics is also influenced.
In combination, most current finishing methods can impart excellent functional properties to silk fibers, but less research is conducted on the machine washability of silk fabrics. Although few reports indicate that some methods can improve the machine washing resistance of real silk fabrics, the hand feeling, luster, color, moisture absorption, moisture preservation and other properties of the fabrics are often sacrificed. In view of the above, there is a need to design a machine washable silk fabric and a method for making the same to solve the above problems.
Disclosure of Invention
The application provides a machine washable real silk fabric and a preparation method thereof, and aims to solve the problems that the existing machine washable finishing mode is not environment-friendly and causes the loss of the wearability of the real silk fabric such as hand feeling, luster, moisture absorption and retention. The preparation method provided by the application adopts silk fibroin and polydopamine as coating materials, and the silk fibroin and polydopamine are finished on the surface of the silk fabric in a padding and low-temperature baking mode, so that the machine washable silk fabric is obtained. The finished silk fabric retains the original softness and skin-friendly property of silk fiber, and has the advantages of greatly improved mechanical strength and wear resistance, prolonged service life, and no obvious damage and burrs on the surface of the coating after 30 times of machine washing.
In a first aspect, an embodiment of the present application provides a method for preparing a machine washable silk fabric, including the steps of:
s1, boiling and degumming pretreated cocoons, washing with deionized water, drying to obtain silk fibers, dissolving the silk fibers in neutral salt solution, and then dialyzing to remove salt to obtain silk fibroin solution;
S2, dissolving dopamine hydrochloride in Tris-HCl buffer solution to prepare dopamine solution, mixing the dopamine solution with the silk fibroin solution prepared in the step S1, and gently stirring until the mixture is uniform to obtain mixed solution;
and S3, finishing the real silk fabric by adopting the mixed solution obtained in the step S2 to obtain the machine washable real silk fabric, wherein the finishing comprises 2-5 times of padding and baking treatment, namely, padding the real silk fabric, drying at 35-45 ℃, washing with water, and baking at 35-45 ℃ for 5-10 minutes.
In step S2 of some embodiments, the Tris-HCl buffer has a concentration of 5-15mmol/L, the Tris-HCl buffer has a pH of 7.5-8.5, and the dopamine solution has a concentration of 1.8-2.2mg/mL.
In step S2 of some embodiments, the mass ratio of silk fibroin to dopamine in the mixed solution is (8-12): 1, and the pH of the mixed solution is 7-8.5.
In step S1 of some embodiments, the boiling degumming is to put pretreated cocoons into deionized water, heat and boil for 30-50min, then keep the temperature at 70-85 ℃, add alkaline agent for four times and stir fully every time for 10min, wherein the total time of the boiling degumming is 1.5-2h, the alkaline agent is NaHCO 3 and Na 2CO3, and the mass ratio of the pretreated cocoons to NaHCO 3 and Na 2CO3 is (18-22): 2:1.
In step S1 of some embodiments, the neutral salt solution is an aqueous lithium bromide solution having a concentration of 10-12mol/L.
In step S1 of some embodiments, the pretreatment is to cut off the cocoons, remove the pupa and the dirty silk inside the cocoons, cut the rest into small pieces, and wash with deionized water and dry.
In step S1 of some embodiments, the silk fibers have a dissolution temperature of 60-70 ℃ and a dissolution time of 6-8 hours.
In step S1 of some embodiments, the dialysis time is 3-5 days.
In step S3 of some embodiments, the pressure of the padder is 2-3kg/cm 2.
In a second aspect, an embodiment of the present application provides a machine washable silk fabric, which is manufactured according to the manufacturing method of any one of the foregoing technical solutions.
The beneficial effects of the application are as follows:
the application provides a machine washable real silk fabric and a preparation method thereof, which solve the problems that the existing machine washable finishing mode in the background art is not environment-friendly and can cause the loss of the wearability of the real silk fabric such as hand feeling, luster, moisture absorption and retention. The preparation method provided by the application adopts silk fibroin and polydopamine as coating materials, and the silk fibroin and polydopamine are finished on the surface of the silk fabric in a padding treatment and low-temperature baking mode, so that the machine washable silk fabric is obtained. The finished silk fabric retains the original softness and skin-friendly property of silk fiber, mechanical strength and wear resistance are greatly improved, service life is prolonged, no obvious damage or burrs are generated on the surface of the coating after 30 times of machine washing, the requirements of high-end markets and multifunctional application can be met, and the market competitiveness of products is improved.
(1) The silk fiber coating material has the advantages that silk fibroin and polydopamine with good biocompatibility are used as the coating material, the original softness and skin affinity of the silk fiber are reserved, no pollution and toxicity reagent or medicine is adopted in the preparation process, the environment-friendly concept is met, in addition, the low-temperature baking is adopted in the rolling baking treatment, the fixation strength and fixation amount of the coating are increased through repeated rolling baking treatment, and the silk fiber is protected from being damaged in the treatment process.
(2) The silk fibroin adopted by the application has the same biological source as silk fibers, on one hand, the silk fibroin does not cause skin irritation or anaphylactic reaction, and can retain original softness, skin-friendly property and natural luster of the silk fibers, and on the other hand, the silk fibroin and the silk fibers have better affinity due to almost the same components, so that the interface fastness can be greatly improved.
(3) The polydopamine and the silk fibroin adopted by the application are mutually fused to form the polydopamine protein coating, so that the washing resistance of silk fibers is greatly improved. This is because, in the alkaline mixed solution of silk fibroin and dopamine, the dopamine is continuously oxidized and self-polymerized to form polydopamine, and the polydopamine has a structure similar to mussel adhesive protein and has self-adhesive property, so that the polydopamine can be firmly adhered to the silk surface. Meanwhile, a plurality of hydroxyl groups and amine groups in the polydopamine molecular structure form hydrogen bonds and other non-covalent bonds with hydroxyl groups and amine groups on the surface of silk fibroin, so that acting force between polydopamine and silk fibroin is enhanced, and hydrogen bonds and other non-covalent bonds are also formed between polydopamine and silk fabrics in the same way, so that the polydopamine, the silk fibroin and the silk fabrics have the mutual cooperation of hydrogen bonds and electrostatic various acting forces, interface binding force between a polydopamine protein coating and the silk fabrics is greatly enhanced, mechanical strength and wear resistance of the silk fabrics are improved, and service life of the silk fabrics is prolonged.
(4) The washing-resistant finishing process provided by the application can be combined with other functional finishing, different functional characteristics of machine-washable silk fabrics can be endowed without additional adding working procedures, and the requirements of consumers on high-performance and multifunctional textiles are met. For example, certain functional auxiliary agents or essential oil aromatic finishing agents such as titanium dioxide nano particles, zinc oxide nano particles, rose essential oil and peppermint essential oil are added into the mixed solution used during padding, so that the machine washable real silk fabric has the effects of resisting ultraviolet, relieving emotion and refreshing. In addition, the polydopamine in the coating is a catechol derivative, has good biocompatibility and low toxicity, can inhibit the attachment and growth of bacteria, and has potential antibacterial performance.
The foregoing description is only an overview of the present application, and is intended to be implemented in accordance with the teachings of the present application in order that the same may be more clearly understood and to make the same and other objects, features and advantages of the present application more readily apparent.
Drawings
In order to more clearly illustrate the technical solution of the present application, the following description will briefly explain the drawings used in the present application. It is apparent that the drawings described below are only some embodiments of the present application, and that other drawings may be obtained from these drawings without inventive effort for a person of ordinary skill in the art.
Fig. 1 is a fiber electron microscope image of the machine washable silk fabric and the normal silk fabric prepared in example 1 after 30 times of machine washing, wherein (a), (b), (c), and (d) are fiber electron microscope images of the normal silk fabric after 30 times of washing, and (e), (f), (g), and (h) are fiber electron microscope images of the machine washable silk fabric prepared in example 1 after 30 times of washing.
Fig. 2 is a graph showing the apparent color of the plain silk fabric and the machine washable silk fabric, wherein (i) is the apparent color of the plain silk fabric, (j) is a partial enlarged view of (i), (k) is the apparent color of the machine washable silk fabric prepared in example 1, and (l) is a partial enlarged view of (k).
Detailed Description
Embodiments of the technical scheme of the present application will be described in detail below with reference to the accompanying drawings. The following examples are only for more clearly illustrating the technical aspects of the present application, and thus are merely examples, and are not intended to limit the scope of the present application.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs, the terms used herein are for the purpose of describing particular embodiments only and are not intended to be limiting of the application, and the terms "comprising" and "having" and any variations thereof in the description of the application and the claims and the above description of the drawings are intended to cover non-exclusive inclusions.
In the description of embodiments of the present application, the technical terms "first," "second," and the like are used merely to distinguish between different objects and are not to be construed as indicating or implying a relative importance or implicitly indicating the number of technical features indicated, a particular order or a primary or secondary relationship. In the description of the embodiments of the present application, the meaning of "plurality" is two or more unless explicitly defined otherwise.
Reference herein to "an embodiment" means that a particular feature, structure, or characteristic described in connection with the embodiment may be included in at least one embodiment of the application. The appearances of such phrases in various places in the specification are not necessarily all referring to the same embodiment, nor are separate or alternative embodiments mutually exclusive of other embodiments. Those of skill in the art will explicitly and implicitly appreciate that the embodiments described herein may be combined with other embodiments.
In the description of the embodiment of the present application, the term "and/or" is merely an association relationship describing the association object, and indicates that three relationships may exist, for example, a and/or B, and may indicate that a exists alone, while a and B exist together, and B exists alone. In addition, the character "/" herein generally indicates that the front and rear associated objects are an "or" relationship. The specific meaning of the above terms in the embodiments of the present application will be understood by those of ordinary skill in the art according to specific circumstances.
In order to solve the problems that the existing machine-washing-resistant finishing mode is not environment-friendly and can cause the loss of the wearability of real silk fabrics such as hand feeling, luster, moisture absorption and retention, the application provides a machine-washable real silk fabric and a preparation method thereof.
The embodiment of the application provides a preparation method of machine washable silk fabric, which comprises the following steps:
S1, boiling and degumming pretreated cocoons, washing with deionized water, drying to obtain silk fibers, dissolving the silk fibers in neutral salt solution, and then dialyzing to remove salt to obtain silk fibroin solution with the concentration of 5% -7%;
in the technical scheme of the embodiment of the application, the pretreatment is that the silkworm cocoons are cut off, the silkworm chrysalis and the dirty silk part inside the silkworm cocoons are removed, and the rest parts are cut into small pieces and washed and dried by deionized water.
The boiling degumming is to put pretreated cocoons into deionized water, heat and boil for 30-50min, then keep the temperature at 70-85 ℃, add alkaline agent for four times and stir fully, each time for 10min, wherein the total time of boiling degumming is 1.5-2h, the alkaline agent is NaHCO 3 and Na 2CO3, and the mass ratio of pretreated cocoons to NaHCO 3 and Na 2CO3 is (18-22): 2:1.
The dialysis time is 3-5 days.
The neutral salt solution is lithium bromide water solution, and the concentration of the lithium bromide water solution is 10-12mol/L.
The dissolution temperature of silk fiber is 60-70 ℃ and the dissolution time is 6-8h.
S2, dissolving dopamine hydrochloride in Tris-HCl buffer solution to prepare dopamine solution, mixing the dopamine solution with the silk fibroin solution prepared in the step S1, and gently stirring until the mixture is uniform to obtain mixed solution;
In the technical scheme of the embodiment of the application, the concentration of the Tris-HCl buffer solution is 5-15mmol/L, the pH of the Tris-HCl buffer solution is 7.5-8.5, and the concentration of the dopamine solution is 1.8-2.2mg/mL.
In the mixed solution, the mass ratio of silk fibroin to dopamine is (8-12): 1, and the pH of the mixed solution is 7-8.5.
In the weakly alkaline mixed solution, the dopamine continuously undergoes self-polymerization reaction to form polydopamine with self-adhesion property, and the mixed solution is finished on the surface of the real silk fabric in the subsequent steps to obtain the polydopamine protein coating.
And S3, finishing the real silk fabric by adopting the mixed solution obtained in the step S2 to obtain the machine washable real silk fabric, wherein the finishing comprises 2-5 times of padding and baking treatment, namely padding the real silk fabric, drying at 35-45 ℃, washing with water, and baking at 35-45 ℃ for 5-10 minutes.
In the technical scheme of the embodiment of the application, the pressure of the padder is 2-3kg/cm 2.
Specific embodiments are set forth below, with the understanding that the embodiments described below are illustrative, and are intended to be illustrative of the application only and are not to be construed as limiting the application. The examples are not to be construed as limiting the specific techniques or conditions described in the literature in this field or as per the specifications of the product. The reagents or apparatus used were conventional products commercially available without the manufacturer's attention.
The silk fabrics used in the examples and comparative examples provided by the application are all plain crepe satin with a weight of 63.3g/m 2, purchased from home textile limited company in Zhejiang and Tung China.
Example 1
The embodiment provides a preparation method of machine washable silk fabric, which comprises the following steps:
S1, cutting cocoons, removing silkworm chrysalis, cleaning the rest part by deionized water to remove surface impurities, drying to obtain pretreated cocoons, weighing 20g of cocoons, putting the cocoons in deionized water, heating and boiling for 30 minutes, cooling to 80 ℃, preserving heat, adding 2g of NaHCO 3 and 1g of Na 2CO3 for four times, fully stirring, keeping stirring for 30 minutes after 10 minutes each time, pouring alkali liquor, washing with deionized water, and drying to obtain silk fibers.
18G of silk fiber is weighed and put into 300mL of lithium bromide aqueous solution (LiBr, 10-12 mol/L), heated to 65 ℃ and stirred for 6 hours at the temperature, so that the silk fiber is fully dissolved in the lithium bromide aqueous solution, then naturally cooled, as the temperature of the solution is reduced, originally dissolved silk protein is crystallized and separated out in saturated solution to obtain silk protein lithium bromide solution, silk protein is saturated in the solution, the solution is put into a dialysis membrane bag, the dialysis membrane bag is put into deionized water, and the solution is left for 4 days at normal temperature to remove lithium bromide, so that the silk protein solution with the concentration of 6% is obtained.
S2, dissolving dopamine hydrochloride in 10mmoL/L Tris-HCl buffer solution (pH=8.5) to prepare a dopamine solution with the concentration of 2mg/mL, then mixing the silk fibroin solution prepared in the step S1 with the dopamine solution according to the solute mass ratio of 10:1, and slightly stirring until the mixture is uniform, so that bubbles are avoided, and the pH of the obtained mixed solution is 8.
S3, shearing the silk fabric with the length of 15cm and the width of 5cm, and finishing the silk fabric by adopting the mixed solution prepared in the step S2 as a finishing agent. Firstly, the fabric is soaked for two times, the pressure of a padder is 2-3kg/cm 2, then the padded fabric is put into a blast oven for drying at 40 ℃, excessive finishing agent on the fabric is washed out by clean water, and the fabric is put into the oven for baking for 10 minutes at 40 ℃ again, thus finishing one-time padding and baking treatment, and the padding and baking treatment is repeated for 2 times, thus obtaining the machine washable real silk fabric.
Examples 2 to 4 and comparative example 1
Examples 2 to 4 and comparative example 2 are different from example 1 in that the number of times of the roll baking treatment in step S3 is 3,4, 5, respectively, and the other contents are substantially the same as those in example 1, and are not repeated here.
Project Comparative example 1 Example 2 Example 3 Example 4
Number of times of baking treatment 1 3 4 5
Examples 5 to 7 and comparative examples 2 to 3
Examples 5 to 7 and comparative examples 2 to 3 are different from example 1 in that the baking temperature in step S3 and the time of the second baking are changed, and the following table is specific, and the other contents are substantially the same as those of example 1, and are not repeated here.
Project Comparative example 2 Example 5 Example 6 Example 7 Comparative example 3
First baking temperature (°c) 25 35 45 45 55
Second baking temperature (°c) 25 35 45 45 55
Second baking time (min) 10 10 10 5 10
Examples 8 to 9 and comparative examples 4 to 5
Examples 8-9 and comparative examples 4-5 differ from example 1 in that the mass ratio of silk fibroin to dopamine in step S2 was changed, and the following table shows that the other matters are substantially the same as example 1, and will not be repeated here.
Project Example 8 Example 9 Comparative example 4 Comparative example 5
Mass ratio of silk fibroin to dopamine 8∶1 12∶1 5∶1 15∶1
Comparative example 6
Comparative example 6 differs from example 1 in that the pH of the mixed solution in step S2 was changed to 9.5 by adjusting the pH to 9.5 by dropwise addition of 0.5M NaOH solution to Tris buffer in step S2. The other matters are substantially the same as those of embodiment 1, and will not be described here again.
In the preparation process, the dopamine hydrochloride is not stable enough in an environment with an excessively high pH value, and after being dissolved in Tris-HCl buffer solution, the solution turns black, so that the machine washable silk fabric coating prepared in comparative example 6 turns black, and the machine washable silk fabric coating has no test significance.
The bending length and bending rigidity of the ordinary silk fabrics, the machine washable silk fabrics prepared in examples 1 to 9 and comparative examples 1 to 5 were tested with reference to GB/T18318.1-2009 section 1, inclined plane method for determination of textile bending properties. Each set of samples was tested 10 times and the average of these 10 data was taken as the test result for that set of samples, as detailed in tables 1-3.
TABLE 1 influence of the number of pad-baking treatments on the bending properties of Silk fabrics
Fabric type Number of times/times of baking treatment Bending length/cm Flexural rigidity/(mN cm)
Ordinary silk 0 2.9 0.15
Example 1 2 3.2 0.20
Example 2 3 3.5 0.27
Example 3 4 3.7 0.31
Example 4 5 3.9 0.37
Comparative example 1 1 3.0 0.17
TABLE 2 influence of baking temperature and baking time on bending property of real silk fabrics
TABLE 3 influence of the mass ratio of silk fibroin to dopamine on the bending properties of Silk fabrics
Referring to tables 1 to 3, it can be seen that the bending length of the machine washable silk fabrics prepared in examples 1 to 9 is between 3.2 and 3.9cm, the bending stiffness is between 0.2 and 0.37, and the bending length and the bending stiffness are similar to those of the common silk fabrics, which indicates that the machine washable silk fabrics prepared by the method provided by the application better retain the softness of the silk fabrics and have less influence on the wearability.
Referring to table 1, it can be seen that, with the increase of the number of times of the pad baking treatment, the bending length and bending stiffness of the machine washable silk fabric tend to increase, which indicates that the thickness of the coating layer has a certain effect on the silk hand feeling. The hand feeling of the machine washable silk fabric prepared during the rolling baking treatment for 1 time is closest to that of the original silk fabric, but the coating fastness is far less than that of the machine washable silk fabric prepared during the rolling baking treatment for 2 times or more, so that the times of the rolling baking treatment are controlled between 2 and 5 times and the times of the rolling baking treatment are optimal for balancing the softness and the coating fastness of the fabric.
Referring to Table 2, it can be seen that the softness of the fabric is less affected by the coating, and the thickness of the coating is uniform and the fastness is good when the baking temperature in the step S3 is controlled to be about 35-45 ℃ and the second baking time is controlled to be 5-10 min. The temperature is too low, the solvent in the coating volatilizes slowly, the coating is possibly unevenly distributed on the surface of the fabric, the overall test result is higher, the silk fibroin in the coating and silk fibers in the fabric are damaged due to the too high temperature, and the stiffness of the fabric is increased.
Referring to Table 3, it can be seen that the machine washable silk fabric prepared in step S2 has a mass ratio of silk fibroin to dopamine of (8-12): 1, which is optimal for a mass ratio of 10:1, while maintaining good softness.
This is because the mass ratio of silk fibroin to dopamine affects the thickness and uniformity of the coating. The silk fibroin is a natural high polymer material and has stronger adhesiveness and film forming capability, when the mass ratio of the silk fibroin is too high, the concentration of the silk fibroin in the finishing liquid is increased, so that the thickness of a coating formed in the treatment process is increased, the film structure of the coating is compact, the stiffness of the fabric is increased, the air permeability of the fabric is affected, and similarly, when the mass ratio of the dopamine is too high, the concentration of the dopamine in the finishing liquid is increased, the dopamine can self-polymerize and form a polymer network under specific conditions, when the concentration of the dopamine is too high, the coating is easy to form uneven polymer structures in the curing process, the uneven polymer structures possibly show different adhesiveness and thickness at different parts of the fabric, the thickness of the coating on the surface of the fabric is uneven, the overall test result is higher, and the interaction between the dopamine and the silk fibroin is affected by the concentration. At high concentrations, the interaction of dopamine with silk fibroin is reduced, possibly resulting in reduced adhesion of the coating in certain areas, forming defects or weak areas, affecting the durability of the machine washable fabric.
Application example 1
The ordinary silk fabrics and the machine washable silk fabrics prepared in example 1 were respectively washed by a washing fastness tester for 45 ℃ for 30 times and 45min at a temperature of 150mL commercial detergent (concentration of 0.15 wt%) and 50 steel balls, so as to investigate the washing resistance of the silk fabrics.
Referring to fig. 1, (a), (b), (c) and (d) are fiber electron microscope images of the normal silk fabrics washed 30 times, and (e), (f), (g) and (h) are fiber electron microscope images of the machine washable silk fabrics prepared in example 1 washed 30 times. It can be seen that the surface of the silk fabric without the coating becomes rough after 30 times of machine washing, more tiny damages and burrs appear on the surface of the silk fiber, which are caused by mechanical friction and water flow impact in the machine washing process, while the surface of the silk fabric with the polydopamine protein coating does not have obvious change after 30 times of machine washing, and the surface of the silk fiber does not have obvious damages and burrs, so that the machine-washable silk fabric provided by the application has excellent washing resistance.
The apparent colors of the common silk fabric and the machine washable silk fabric prepared in the embodiment 1 are shown in the figure 2, and the colors of the common silk fabric and the machine washable silk fabric are similar, so that the preparation method of the machine washable silk fabric provided by the application relatively effectively maintains the color and the natural luster of the fabric.
In conclusion, the machine washable silk fabric provided by the application utilizes the hydrogen bond and electrostatic various acting forces among polydopamine, silk fibroin and silk fabric, so that the mechanical strength, friction resistance and washing resistance of the silk fabric are improved and the service life of the silk fabric is prolonged while the softness and comfort of the silk fabric are not changed.
The present application is not limited to the above embodiment. The above embodiments are merely examples, and embodiments having substantially the same configuration and the same effects as those of the technical idea within the scope of the present application are included in the technical scope of the present application. Further, various modifications that can be made to the embodiments and other modes of combining some of the constituent elements in the embodiments, which are conceivable to those skilled in the art, are also included in the scope of the present application within the scope not departing from the gist of the present application.

Claims (10)

1. The preparation method of the machine washable silk fabric is characterized by comprising the following steps of:
s1, boiling and degumming pretreated cocoons, washing with deionized water, drying to obtain silk fibers, dissolving the silk fibers in neutral salt solution, and then dialyzing to remove salt to obtain silk fibroin solution;
S2, dissolving dopamine hydrochloride in Tris-HCl buffer solution to prepare dopamine solution, mixing the dopamine solution with the silk fibroin solution prepared in the step S1, and gently stirring until the mixture is uniform to obtain mixed solution;
and S3, finishing the real silk fabric by adopting the mixed solution obtained in the step S2 to obtain the machine washable real silk fabric, wherein the finishing comprises 2-5 times of padding and baking treatment, namely, padding the real silk fabric, drying at 35-45 ℃, washing with water, and baking at 35-45 ℃ for 5-10 minutes.
2. The method for preparing machine washable silk fabric according to claim 1, wherein in step S2, the concentration of Tris-HCl buffer is 5-15mmol/L, the pH of Tris-HCl buffer is 7.5-8.5, and the concentration of dopamine solution is 1.8-2.2mg/mL.
3. The method for preparing machine washable silk fabric according to claim 2, wherein in step S2, the mass ratio of silk fibroin to dopamine in the mixed solution is (8-12): 1, and the pH of the mixed solution is 7-8.5.
4. The method for preparing the machine washable silk fabric according to claim 1, wherein in the step S1, the boiling degumming is carried out by putting pretreated cocoons into deionized water, heating and boiling for 30-50min, keeping the temperature at 70-85 ℃, adding alkaline agent four times and fully stirring for 10min each time, wherein the total time of boiling degumming is 1.5-2h, the alkaline agent is NaHCO 3 and Na 2CO3, and the mass ratio of pretreated cocoons to NaHCO 3 and Na 2CO3 is (18-22): 2:1.
5. The method for preparing machine washable silk fabric according to claim 4, wherein in step S1, the neutral salt solution is lithium bromide aqueous solution, and the concentration of the lithium bromide aqueous solution is 10-12mol/L.
6. The method for preparing machine washable silk fabric according to claim 5, wherein in step S1, the pretreatment is to cut off the cocoons, remove the pupa and the dirty silk part inside the cocoons, cut the rest into small pieces, and wash with deionized water and dry.
7. The method for preparing machine washable silk fabric according to claim 6, wherein in step S1, the dissolution temperature of silk fiber is 60-70 ℃ and the dissolution time is 6-8h.
8. The method for preparing machine washable silk fabric according to claim 7, wherein in step S1, the dialysis time is 3-5 days.
9. The method for producing machine washable silk fabric according to claim 1, wherein in step S3, the pressure of the padder is 2-3kg/cm 2.
10. A machine washable silk fabric, characterized in that it is produced according to the production method of any one of claims 1 to 9.
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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102400376A (en) * 2010-09-09 2012-04-04 上海海帝园艺有限公司 Crease-resistant finishing liquid for silk and wool blended fabric and crease-resistant finishing method thereof
CN105544209A (en) * 2016-01-21 2016-05-04 苏州印丝特纺织数码科技有限公司 Textile after-finishing process taking silk fibroin as medium

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109403046B (en) * 2018-10-16 2021-03-16 西南交通大学 Preparation method of dopamine-regulated natural fibroin microfiber
CN115679696A (en) * 2022-11-11 2023-02-03 山东科技职业学院 Preparation method of dopamine-assisted silk fibroin coating modified ultra-high molecular weight polyethylene fiber

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102400376A (en) * 2010-09-09 2012-04-04 上海海帝园艺有限公司 Crease-resistant finishing liquid for silk and wool blended fabric and crease-resistant finishing method thereof
CN105544209A (en) * 2016-01-21 2016-05-04 苏州印丝特纺织数码科技有限公司 Textile after-finishing process taking silk fibroin as medium

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