CN107938315B - Protein modification method of polyester fabric - Google Patents
Protein modification method of polyester fabric Download PDFInfo
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- CN107938315B CN107938315B CN201711223862.0A CN201711223862A CN107938315B CN 107938315 B CN107938315 B CN 107938315B CN 201711223862 A CN201711223862 A CN 201711223862A CN 107938315 B CN107938315 B CN 107938315B
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/32—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
- D06M11/36—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond with oxides, hydroxides or mixed oxides; with salts derived from anions with an amphoteric element-oxygen bond
- D06M11/38—Oxides or hydroxides of elements of Groups 1 or 11 of the Periodic System
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07K—PEPTIDES
- C07K14/00—Peptides having more than 20 amino acids; Gastrins; Somatostatins; Melanotropins; Derivatives thereof
- C07K14/435—Peptides having more than 20 amino acids; Gastrins; Somatostatins; Melanotropins; Derivatives thereof from animals; from humans
- C07K14/43504—Peptides having more than 20 amino acids; Gastrins; Somatostatins; Melanotropins; Derivatives thereof from animals; from humans from invertebrates
- C07K14/43563—Peptides having more than 20 amino acids; Gastrins; Somatostatins; Melanotropins; Derivatives thereof from animals; from humans from invertebrates from insects
- C07K14/43586—Peptides having more than 20 amino acids; Gastrins; Somatostatins; Melanotropins; Derivatives thereof from animals; from humans from invertebrates from insects from silkworms
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06L—DRY-CLEANING, WASHING OR BLEACHING FIBRES, FILAMENTS, THREADS, YARNS, FABRICS, FEATHERS OR MADE-UP FIBROUS GOODS; BLEACHING LEATHER OR FURS
- D06L1/00—Dry-cleaning or washing fibres, filaments, threads, yarns, fabrics, feathers or made-up fibrous goods
- D06L1/02—Dry-cleaning or washing fibres, filaments, threads, yarns, fabrics, feathers or made-up fibrous goods using organic solvents
- D06L1/06—De-sizing
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06L—DRY-CLEANING, WASHING OR BLEACHING FIBRES, FILAMENTS, THREADS, YARNS, FABRICS, FEATHERS OR MADE-UP FIBROUS GOODS; BLEACHING LEATHER OR FURS
- D06L1/00—Dry-cleaning or washing fibres, filaments, threads, yarns, fabrics, feathers or made-up fibrous goods
- D06L1/12—Dry-cleaning or washing fibres, filaments, threads, yarns, fabrics, feathers or made-up fibrous goods using aqueous solvents
- D06L1/14—De-sizing
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/01—Treating 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
- D06M15/15—Proteins or derivatives thereof
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/55—Epoxy resins
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/16—Synthetic fibres, other than mineral fibres
- D06M2101/30—Synthetic polymers consisting of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M2101/32—Polyesters
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
- D06M2200/50—Modified hand or grip properties; Softening compositions
Abstract
The invention provides a protein modification method of a polyester fabric, which comprises the following steps: desizing the polyester fabric to obtain a desized fabric; treating the desized fabric with sodium hydroxide, and washing to obtain the fabric subjected to alkali treatment; soaking the fabric subjected to alkali treatment in a cross-linking agent solution, and mixing and reacting with silk fibroin with the molecular weight of 1000-5000 Da; the crosslinking agent comprises polyethylene glycol diglycidyl ether. According to the modification method provided by the invention, the desized fabric is treated by sodium hydroxide, and the alkali treatment is arranged to release reaction sites on a polyester fiber molecular chain; meanwhile, the silk fibroin modified alkali-treated fabric with the limited molecular weight of 1000-5000 Da is adopted, the silk fibroin with the specific small molecular weight is firmly introduced to the fiber surface of the polyester fabric by utilizing the principle of covalent bonding, the cooling property, the flexibility and the antistatic property of the polyester fabric are improved, and meanwhile, the mechanical property and the silk fibroin stability are good.
Description
Technical Field
The invention relates to the technical field of spinning, in particular to a method for modifying protein of a polyester fabric.
Background
The terylene is the fiber with the highest textile fiber yield, is the most main raw material of textile products, accounts for more than 70 percent of the processing amount of the textile fibers, is a chemical synthetic fiber, is widely applied to clothes and household textiles mainly comprising coats, curtains, sofa fabrics, interior ornaments and the like because of the advantages of high breaking strength, good light resistance, stiff and smooth products and the like, but belongs to super-hydrophobic fibers, has extremely poor moisture absorption and rigidity, and limits the application of the terylene in the fields of home textiles and certain clothes, such as summer clothing, underwear, bedding and the like.
The research of silk fibroin coating terylene is reported in the prior art, and the terylene fiber or fabric coated by the terylene fiber or the fabric has brittleness, is easy to crack and fall off, and can influence the surface structure and even the air permeability of the original fabric. There are also literature reports of low weight gain for silk fibroin coating, unsatisfactory water wash resistance, or low moisture regain. So no market applications are available.
Disclosure of Invention
In view of the above, the technical problem to be solved by the invention is to provide a method for modifying protein of a polyester fabric, and the polyester fabric modified by the modification method provided by the invention has good mechanical properties and good stability.
The invention provides a protein modification method of a polyester fabric, which comprises the following steps:
A) desizing the polyester fabric to obtain a desized fabric;
B) treating the desized fabric with sodium hydroxide, and washing to obtain the fabric subjected to alkali treatment;
C) soaking the fabric subjected to alkali treatment in a cross-linking agent solution, and mixing and reacting with silk fibroin with the molecular weight of 1000-5000 Da; the crosslinking agent comprises polyethylene glycol diglycidyl ether.
Preferably, the polyethylene glycol diglycidyl ether accounts for 30-100% of the silk fibroin by mass.
Preferably, the desizing in the step A) is specifically desizing treatment by adopting sodium carbonate; the concentration of the sodium carbonate solution is 6 g/L; the desizing treatment temperature is 90-100 ℃; the desizing treatment time is 1 h.
Preferably, the mass concentration of the sodium hydroxide in the step B) is 5-30%; the treatment temperature of the sodium hydroxide is 30-40 ℃; the treatment time of the sodium hydroxide is 1-3 h.
Preferably, the reaction temperature in the step D) is 25-35 ℃; the reaction time is 1-3 h.
Preferably, the silk fibroin with the molecular weight of 1000-5000 Da is prepared by the following method:
a) degumming silkworm silk by using sodium carbonate, and then adding a neutral salt solution to dissolve to prepare a silk fibroin dissolving solution;
the dextran Sephadex G50 and G25 columns are balanced for standby;
b) adding the silk fibroin dissolving solution into a glucan Sephadex G50 column, eluting the silk fibroin with sterile water, and collecting desalted silk fibroin aqueous solution in a branch pipe;
c) and (b) screening the silk fibroin with the molecular weight of less than 10kD in the collection tube in the step b) by SDS-PAGE electrophoresis or mass spectrometry, adding the silk fibroin into a dextran Sephadex G25 column again, eluting the silk fibroin by using sterilized water, collecting the silk fibroin in different tubes, and screening to obtain the silk fibroin with the small molecular weight of 1000-5000 Da.
Preferably, the neutral salt solution of step a) is selected from lithium bromide or calcium chloride-ethanol; the dissolving time is 5-7 hours; the concentration of the silk fibroin dissolving solution is 10-50 mg/mL.
Preferably, the silk fibroin in the collection tube in the step b) of screening in the step c) is further lyophilized, and then prepared into 30-80 mg/mL aqueous solution.
Preferably, the elution flow rate in the step b) is 200-400 mL/h.
Preferably, the elution flow rate in the step c) is 30-70 mL/h.
Compared with the prior art, the invention provides a method for modifying protein of polyester fabric, which comprises the following steps: A) desizing the polyester fabric to obtain a desized fabric; B) treating the desized fabric with sodium hydroxide to obtain an alkali-treated fabric; C) and (3) soaking the fabric subjected to alkali treatment in a cross-linking agent solution, and mixing and reacting with silk fibroin with the molecular weight of 1000-5000 Da. According to the modification method provided by the invention, the desized fabric is treated by sodium hydroxide, and the alkali treatment is arranged to release reaction sites on a polyester fiber molecular chain; meanwhile, the fabric is subjected to alkali treatment by adopting the silk fibroin graft modification with small relative molecular weight of 1000-5000 Da and concentrated distribution, and the silk fibroin with specific small molecular weight is firmly introduced to the fiber surface of the polyester fabric by utilizing the principle of covalent bonding, so that the cooling property, the flexibility and the antistatic property of the polyester fabric are improved, and meanwhile, the mechanical property is good and the silk fibroin stability is good.
Detailed Description
The invention provides a protein modification method of a polyester fabric, which comprises the following steps:
A) desizing the polyester fabric to obtain a desized fabric;
B) treating the desized fabric with sodium hydroxide, and washing to obtain the fabric subjected to alkali treatment;
C) soaking the fabric subjected to alkali treatment in a cross-linking agent solution, and mixing and reacting with silk fibroin with the molecular weight of 1000-5000 Da; the crosslinking agent comprises polyethylene glycol diglycidyl ether.
The polyester fabric is not limited in the invention, and can be defined as the polyester fabric which is well known to those skilled in the art. The source of the present invention is not limited, and may be commercially available.
The method comprises the following steps of firstly, desizing the polyester fabric to obtain the desized fabric.
In the present invention, the desizing treatment is preferably a sodium carbonate desizing treatment; preferably, the terylene face fabric is heated in the aqueous solution of sodium carbonate. The heating is preferably boiling heating.
The concentration of the sodium carbonate solution is preferably 6 g/L; the preferable desizing treatment temperature is 90-100 ℃; the desizing treatment time is preferably 1 h.
After heating, washing, dehydration, and drying are preferable.
The washing in the invention is preferably tap water, and the washing mode in the invention is not limited, and the washing mode is well known to those skilled in the art; the dehydration mode is not limited in the invention, and the dehydration mode is well known to those skilled in the art; the drying mode is not limited, and the drying method is well known to those skilled in the art; can be air-dried or oven-dried.
And drying to obtain the desized fabric, and treating the desized fabric by adopting sodium hydroxide.
In the invention, the mass concentration of the sodium hydroxide is preferably 5-30%; more preferably 10%; the treatment temperature of the sodium hydroxide is preferably 30-40 ℃; the treatment time of the sodium hydroxide is preferably 1-3 h; more preferably 1-2 h.
In the present invention, the source of the sodium hydroxide is not limited and may be commercially available.
After the sodium hydroxide treatment, washing and drying are preferable.
The washing in the invention is preferably tap water, and the washing mode in the invention is not limited, and the washing mode is well known to those skilled in the art; the drying mode is not limited, and the drying method is well known to those skilled in the art; can be air-dried or oven-dried.
And washing and drying the fabric to obtain the fabric subjected to alkali treatment.
And after the alkali treatment is finished, soaking the treated fabric in a cross-linking agent solution, and mixing and reacting the fabric with silk fibroin with the molecular weight of 1000-5000 Da to obtain the silk fibroin modified polyester fabric.
According to the invention, the crosslinking agent comprises polyethylene glycol diglycidyl ether.
The mass percentage of the polyethylene glycol diglycidyl ether in the silk fibroin is preferably 30-100%; more preferably 80%.
In accordance with the present invention, there is provided,
after dipping, adding the prepared silk fibroin with the molecular weight of 1000-5000 Da for grafting reaction, wherein the final concentration of the silk fibroin solution is preferably 0.5-5%;
the reaction temperature is preferably 25-35 ℃; the reaction time is preferably 1-3 h.
After the grafting reaction, it is preferable to dry, wash, and dry again.
The drying is preferably air drying; the washing is preferably a water rinse; the re-drying is preferably air drying. The present invention is not limited to the specific operations of drying and rinsing, and those skilled in the art will be familiar with the present invention.
In the present invention, the silk fibroin is silk fibroin that has a relatively small molecular weight and is distributed intensively.
The invention creatively adopts the silk fibroin graft modification alkali treated fabric with the limited small molecular weight, utilizes the principle of covalent bonding to lead the silk fibroin with the specific small molecular weight to be firmly introduced to the fiber surface of the polyester fabric, improves the coolness, softness, antistatic property and glossiness of the polyester fabric, improves the skin affinity, and has good mechanical property and silk fibroin stability.
The silk fibroin source with the molecular weight of 1000-5000 Da is not limited, can be commercially available, and is preferably prepared by the following method:
a) degumming silkworm silk by using sodium carbonate, and then adding a neutral salt solution to dissolve to prepare a silk fibroin dissolving solution;
the dextran Sephadex G50 and G25 columns are balanced for standby;
b) adding the silk fibroin dissolving solution into a glucan Sephadex G50 column, eluting the silk fibroin with sterile water, and collecting desalted silk fibroin aqueous solution in a branch pipe;
c) and (b) screening the silk fibroin with the molecular weight of less than 10kD in the collection tube in the step b) by SDS-PAGE electrophoresis or mass spectrometry, adding the silk fibroin into a dextran Sephadex G25 column again, eluting the silk fibroin by using sterilized water, collecting the silk fibroin in different tubes, and screening to obtain the silk fibroin with the small molecular weight of 1000-5000 Da.
Firstly, degumming silkworm silk by using sodium carbonate; preferably, the silkworm silk is put into a sodium carbonate aqueous solution according to a specific bath ratio, treated, cleaned and dried to obtain the degummed silk.
The silkworm silk is not limited in the present invention, and may be a raw silkworm silk known to those skilled in the art, and may be commercially available.
The bath ratio of the present invention is preferably 1:50 (g/mL); the mass concentration of the sodium carbonate aqueous solution is preferably 0.2%; the treatment temperature is preferably 98-100 ℃; the treatment frequency is preferably 1-5 times; more preferably 2-3 times; the treatment time is preferably 30min per treatment.
And cleaning after the treatment is finished, and drying to obtain the degummed silk.
The cleaning is preferably deionized water washing, and the cleaning mode is not limited in the invention and is well known to those skilled in the art; after washing, preferably larch, which is well known to those skilled in the art; the drying method is not limited in the invention, and the drying method is well known to those skilled in the art; drying in an oven may be used. The drying temperature is preferably 65 ℃.
And (3) adding the degummed silk into a neutral salt solution to dissolve, and preparing the silk fibroin dissolving solution.
In the present invention, the neutral salt solution is preferably selected from lithium bromide or calcium chloride-ethanol; the bath ratio of the silk to the neutral salt solution is preferably 1: 15-1: 20 (g/mL);
the concentration of the lithium bromide solution is preferably 9-10M; in the calcium chloride-ethanol, the mol ratio of calcium chloride to ethanol is preferably 1: 2;
the dissolving time is 5-7 hours; the preferred dissolving temperature is 60-70 ℃; more preferably 65 ℃ to 70 ℃; the concentration of the obtained silk fibroin dissolving solution is preferably 10-50 mg/mL.
The dextran Sephadex G50 and G25 columns were equilibrated for use. The sources of the dextran Sephadex G50 and G25 columns are not limited, and the columns can be commercially available or self-made.
The preferable concrete is as follows: boiling dextran Sephadex G50 and G25 with sterilized deionized water until the dextran Sephadex G50 and G25 is fully expanded, continuously filling the dextran Sephadex G50 and G25 into a hollow column made of glass, standing and settling the column, and balancing the column material with the sterilized deionized water; more preferably specifically: respectively putting glucan G-50 and G-25 into deionized water, carrying out boiling water bath for 1.5-2 h, carrying out cooling at normal temperature, then carrying out drainage by using a glass rod, filling into a hollow column made of glass, naturally settling for 2-3 h, then pressurizing by using a peristaltic pump, and balancing the column by using deionized water with 5 times of column volume for three times.
The volume of the preparative bed according to the invention is preferably 2cm × 60 cm.
After balancing, adding the silk fibroin dissolving solution into a glucan Sephadex G50 column, eluting the silk fibroin by using sterilized water, and collecting the desalted silk fibroin aqueous solution by virtue of a branch pipe.
The preferable concrete is as follows: and when the balance water is lowered to the surface of the column material for the last time, adding 5-15 mL of the dissolved silk fibroin mixed solution with the concentration of 10-50 mg/mL into the glucan G-50, continuously eluting with the sterilized deionized water when the silk fibroin mixed solution completely enters the surface of the column material, controlling the flow rate of the eluent by using a peristaltic pump, and collecting the effluent liquid in different tubes until the silk fibroin is completely drained.
The elution flow rate is preferably 200-400 mL/h; more preferably 250 to 350 mL/h.
Screening the silk fibroin with the concentration of less than 10kD in the collection tube in the step b) by SDS-PAGE electrophoresis or mass spectrometry.
The present invention does not limit the specific mode of the SDS-PAGE electrophoresis or mass spectrometry screening step b) to collect the silk fibroin with the kD below in the tube, and the silk fibroin is well known to those skilled in the art.
In the invention, after the silk fibroin with the concentration of less than 10kD in the collection tube in the screening step b), freeze-drying is further carried out, and then 30-80 mg/mL aqueous solution is prepared. Then filtering, wherein the filtration is preferably performed by using a membrane with the diameter of 0.45 mu m.
The present invention is not limited to the specific manner of lyophilization, as will be apparent to those skilled in the art.
Further separation of the molecular weight of silk fibroin below 10kD was performed by means of lyophilization followed by dissolution.
And (3) after filtering, adding the filtered solution into a glucan Sephadex G25 column, eluting silk fibroin by using sterilized water, collecting by tubes, and screening to obtain the silk fibroin with the small molecular weight of 1000-5000 Da.
The flow rate of elution is preferably 30-70 mL/h; more preferably 35 to 50 mL/h.
After elution, screening and collecting 1000-5000 Da low-molecular-weight silk fibroin in the tube by SDS-PAGE electrophoresis or mass spectrum, and freeze-drying and storing.
By adopting the method, the silk fibroin with the small molecular weight of 1000-5000 Da can be obtained more simply, conveniently and accurately.
The present invention is not limited to the specific manner of screening and lyophilization, as will be apparent to those skilled in the art.
The invention provides a protein modification method of a polyester fabric, which comprises the following steps: A) desizing the polyester fabric to obtain a desized fabric; B) treating the desized fabric with sodium hydroxide, washing and drying to obtain the fabric subjected to alkali treatment; C) soaking the fabric subjected to alkali treatment in a cross-linking agent solution, and mixing and reacting with silk fibroin with the molecular weight of 1000-5000 Da; the crosslinking agent comprises polyethylene glycol diglycidyl ether. According to the modification method provided by the invention, the desized fabric is treated by sodium hydroxide, and the alkali treatment is arranged to release reaction sites on a polyester fiber molecular chain; meanwhile, the silk fibroin graft modified alkali-treated fabric with relatively small molecular weight of 1000-5000 Da and concentrated distribution is adopted, the silk fibroin with specific molecular weight is firmly introduced to the fiber surface of the polyester fabric by utilizing the principle of covalent bonding, the coolness, softness, antistatic property and glossiness of the polyester fabric are improved, the skin affinity is improved, and meanwhile, the mechanical property and the silk fibroin stability are good.
The modified terylene fabric has soft, smooth and cool surface and general skin affinity, and is mainly applied to the development of high-grade underwear, summer clothes and bedding.
The invention preferably adopts the following method to measure the mechanical property of the fabric:
the silk fibroin modified polyester fabric is cut into a sample of 15cm multiplied by 30cm, and the sample is measured by a material mechanical property tester.
In order to further explain the invention, the following describes in detail the fibroin modification method of the polyester fabric provided by the invention with reference to the examples.
Example 1
(1) The method comprises the steps of putting silkworm raw silk into a sodium carbonate aqueous solution with the concentration of 0.2% according to the bath ratio of 1:50(g/mL), treating for three times at the temperature of 98-100 ℃ for 30 minutes each time, then fully cleaning the silk with deionized water, loosening, and drying in an oven to obtain the degummed silkworm fibroin fiber.
(2) Weighing degummed bombyx mori silk fibroin, dissolving in a calcium chloride-ethanol aqueous solution with a molar ratio of 1:2 according to a bath ratio of 1:20(g/mL), and dissolving at 70 ℃ for 5-7 hours to obtain a bombyx mori silk fibroin dissolved mixed solution.
(3) Weighing glucan G-50 and G-25, respectively putting into sufficient deionized water, boiling water bath for 1.5 hours, cooling at normal temperature, then draining with a glass rod, filling into a hollow column made of glass, preparing a column bed with a volume of 2cm multiplied by 60cm, naturally settling for 2 hours, pressurizing with a peristaltic pump, and balancing the column with 5 times of column volume of deionized water for three times.
(4) When the balance water is lowered to the surface of the column material for the last time, adding 5-15 mL (10-50 mg/mL) of dissolved silk fibroin mixed solution into the glucan G-50, when the silk fibroin mixed solution completely enters the surface of the column material, continuously eluting with sterilized deionized water, and controlling the flow rate of eluent by using a peristaltic pump to be 300 mL/h; collecting effluent liquid in different tubes until silk fibroin is completely drained.
(5) And (3) identifying the molecular weight distribution of each tube by SDS-PAGE electrophoresis or mass spectrometry, mixing and freeze-drying the silk fibroin solution with the molecular weight of less than 10kDa, preparing into 30-80 mg/ml aqueous solution, and filtering by using a 0.45 mu m membrane to remove microparticles.
(6) Similar to the step (4), adding a proper amount of the silk fibroin aqueous solution obtained in the step (5) into the column material of G-25, controlling the flow rate of the eluent by a peristaltic pump to be 50mL/h, collecting the eluent in different tubes until the silk fibroin is completely drained to obtain the silk fibroin aqueous solution with the molecular weight of 1000-5000 Da, and finally freeze-drying and storing.
(7) And (4) preparing 0.5 mass percent silk fibroin solution from the freeze-dried silk fibroin obtained in the step (6), adding polyethylene glycol diglycidyl ether accounting for 80 mass percent of the silk fibroin, and uniformly stirring.
(8) The weaving terylene face fabric is boiled for about 1 hour at 100 ℃ by 6g/1L of sodium carbonate aqueous solution, taken out and washed clean by tap water repeatedly, dehydrated and dried. And then treating the polyester fabric with 10% sodium hydroxide solution at 30 ℃ for 1-2 hours, rinsing the polyester fabric with tap water, soaking the polyester fabric in silk fibroin solution containing polyethylene glycol diglycidyl ether for reaction for 3 hours, taking out the polyester fabric, and airing, rinsing and drying the polyester fabric again.
(9) The silk fibroin modified polyester fabric is cut into a sample of 15cm multiplied by 30cm, the breaking strength is about 94% of the original fabric, and the breaking elongation is about 103% of the original fabric, which are measured by a material mechanical property tester.
(10) The silk fibroin weight gain rate of the terylene fabric measured by a weighing method is 2.3 percent and is obviously higher than the weight gain rate of 0.9 percent of that of the comparative example 1. After soaking the silk fibroin modified fabric in warm water at 37 ℃ and oscillating for 24 hours, the dissolution rate of the silk fibroin is measured to be less than 7%.
Example 2
(1) The method comprises the steps of putting silkworm raw silk into a sodium carbonate aqueous solution with the concentration of 0.2% according to the bath ratio of 1:50(g/mL), treating for three times at the temperature of 98-100 ℃ for 30 minutes each time, then fully cleaning the silk with deionized water, loosening, and drying in an oven to obtain the degummed silkworm fibroin fiber.
(2) Weighing degummed bombyx mori silk fibroin, dissolving in 9.3 molar concentration lithium bromide aqueous solution according to a bath ratio of 1:15(g/mL), and dissolving at 65 ℃ for 5-7 hours to obtain a bombyx mori silk fibroin dissolving mixed solution.
(3) Weighing glucan G-50 and G-25, respectively putting into sufficient deionized water, boiling water bath for 1.5 hours, cooling at normal temperature, then draining with a glass rod, filling into a hollow column made of glass, preparing a column bed with a volume of 2cm multiplied by 60cm, naturally settling for 2 hours, pressurizing with a peristaltic pump, and balancing the column with 5 times of column volume of deionized water for three times.
(4) When the balance water is lowered to the surface of the column material for the last time, adding 5-15 mL (10-50 mg/mL) of dissolved silk fibroin mixed solution into the glucan G-50, when the silk fibroin mixed solution completely enters the surface of the column material, continuously eluting with sterilized deionized water, and controlling the flow rate of eluent by using a peristaltic pump to be 300 mL/h; collecting effluent liquid in different tubes until silk fibroin is completely drained.
(5) And (3) identifying the molecular weight distribution of each tube by SDS-PAGE electrophoresis or mass spectrometry, mixing and freeze-drying the silk fibroin solution with the molecular weight of less than 10kDa, preparing into 30-80 mg/ml aqueous solution, and filtering by using a 0.45 mu m membrane to remove microparticles.
(6) Similar to the step (4), adding a proper amount of the silk fibroin aqueous solution obtained in the step (5) into the column material of G-25, controlling the flow rate of the eluent by a peristaltic pump to be 50mL/h, collecting the eluent in different tubes until the silk fibroin is completely drained to obtain the silk fibroin aqueous solution with the molecular weight of 1000-5000 Da, and finally freeze-drying and storing.
(7) And (4) preparing a silk fibroin solution with the mass ratio of 1% from the freeze-dried silk fibroin obtained in the step (6), adding polyethylene glycol diglycidyl ether which accounts for 80% of the mass ratio of the silk fibroin, and uniformly stirring.
(8) The weaving terylene face fabric is boiled for about 1 hour at 100 ℃ by 6g/1L of sodium carbonate aqueous solution, taken out and washed clean by tap water repeatedly, dehydrated and dried. And then treating the polyester fabric with 10% sodium hydroxide solution at 30 ℃ for 2-3 hours, rinsing the polyester fabric with tap water, soaking the polyester fabric in silk fibroin solution containing polyethylene glycol diglycidyl ether for reaction for 3 hours, taking out the polyester fabric, and airing, rinsing and drying the polyester fabric again.
(9) The silk fibroin modified polyester fabric is cut into a sample of 15cm multiplied by 30cm, the breaking strength is about 92% of the original fabric, and the breaking elongation is about 117% of the original fabric, which is measured by a material mechanical property tester.
(10) The silk fibroin weight gain rate on the terylene fabric measured by a weighing method is 4.9 percent and is obviously higher than the weight gain rate of 0.92 percent of the comparative example 2. After soaking the silk fibroin modified fabric in warm water at 37 ℃ and oscillating for 24 hours, the dissolution rate of the silk fibroin is measured to be less than 10%.
Example 3
(1) The method comprises the steps of putting silkworm raw silk into a sodium carbonate aqueous solution with the concentration of 0.2% according to the bath ratio of 1:50(g/mL), treating for three times at the temperature of 98-100 ℃ for 30 minutes each time, then fully cleaning the silk with deionized water, loosening, and drying in an oven to obtain the degummed silkworm fibroin fiber.
(2) Weighing degummed bombyx mori silk fibroin, dissolving in a calcium chloride-ethanol aqueous solution with a molar ratio of 1:2 according to a bath ratio of 1:20(g/mL), and dissolving at 70 ℃ for 5-7 hours to obtain a bombyx mori silk fibroin dissolved mixed solution.
(3) Weighing glucan G-50 and G-25, respectively putting into sufficient deionized water, boiling water bath for 1.5 hours, cooling at normal temperature, then draining with a glass rod, filling into a hollow column made of glass, preparing a column bed with a volume of 2cm multiplied by 60cm, naturally settling for 2 hours, pressurizing with a peristaltic pump, and balancing the column with 5 times of column volume of deionized water for three times.
(4) When the balance water is lowered to the surface of the column material for the last time, adding 5-15 mL (10-50 mg/mL) of dissolved silk fibroin mixed solution into the glucan G-50, when the silk fibroin mixed solution completely enters the surface of the column material, continuously eluting with sterilized deionized water, and controlling the flow rate of eluent by using a peristaltic pump to be 300 mL/h; collecting effluent liquid in different tubes until silk fibroin is completely drained.
(5) And (3) identifying the molecular weight distribution of each tube by SDS-PAGE electrophoresis or mass spectrometry, mixing and freeze-drying the silk fibroin solution with the molecular weight of less than 10kDa, preparing into 30-80 mg/ml aqueous solution, and filtering by using a 0.45 mu m membrane to remove microparticles.
(6) Similar to the step (4), adding a proper amount of the silk fibroin aqueous solution obtained in the step (5) into the column material of G-25, controlling the flow rate of the eluent by a peristaltic pump to be 50mL/h, collecting the eluent in different tubes until the silk fibroin is completely drained to obtain the silk fibroin aqueous solution with the molecular weight of 1000-5000 Da, and finally freeze-drying and storing.
(7) And (4) preparing a silk fibroin solution with the mass ratio of 1% from the freeze-dried silk fibroin obtained in the step (6), adding polyethylene glycol diglycidyl ether which accounts for 80% of the mass ratio of the silk fibroin, and uniformly stirring.
(8) The weaving terylene face fabric is boiled for about 1 hour at 100 ℃ by 6g/1L of sodium carbonate aqueous solution, taken out and washed clean by tap water repeatedly, dehydrated and dried. And then treating the polyester fabric with 10% sodium hydroxide solution at 30 ℃ for 1-2 hours, rinsing the polyester fabric with tap water, soaking the polyester fabric in silk fibroin solution containing polyethylene glycol diglycidyl ether for reaction for 3 hours, taking out the polyester fabric, and airing, rinsing and drying the polyester fabric again.
(9) The silk fibroin modified polyester fabric is cut into a sample of 15cm multiplied by 30cm, the breaking strength is about 97 percent of the original fabric, and the breaking elongation is about 110 percent of the original fabric, which is measured by a material mechanical property tester.
(10) The silk fibroin weight gain rate of the terylene fabric measured by a weighing method is 3.2 percent and is obviously higher than the weight gain rate of 0.92 percent of the comparative example 2. After soaking the silk fibroin modified fabric in warm water at 37 ℃ and oscillating for 24 hours, the dissolution rate of the silk fibroin is measured to be less than 10%.
Comparative example 1
(1) The method comprises the steps of putting silkworm raw silk into a sodium carbonate aqueous solution with the concentration of 0.2% according to the bath ratio of 1:50(g/mL), treating for three times at the temperature of 98-100 ℃ for 30 minutes each time, then fully cleaning the silk with deionized water, loosening, and drying in an oven to obtain the degummed silkworm fibroin fiber.
(2) Weighing degummed bombyx mori silk fibroin, dissolving in a calcium chloride-ethanol aqueous solution with a molar ratio of 1:2 according to a bath ratio of 1:20(g/mL), and dissolving at 70 ℃ for 5-7 hours to obtain a bombyx mori silk fibroin dissolved mixed solution.
(3) Weighing glucan G-50 and G-25, respectively putting into sufficient deionized water, boiling water bath for 1.5 hours, cooling at normal temperature, then draining with a glass rod, filling into a hollow column made of glass, preparing a column bed with a volume of 2cm multiplied by 60cm, naturally settling for 2 hours, pressurizing with a peristaltic pump, and balancing the column with 5 times of column volume of deionized water for three times.
(4) When the balance water is lowered to the surface of the column material for the last time, adding 5-15 mL (10-50 mg/mL) of dissolved silk fibroin mixed solution into the glucan G-50, when the silk fibroin mixed solution completely enters the surface of the column material, continuously eluting with sterilized deionized water, and controlling the flow rate of eluent by using a peristaltic pump to be 300 mL/h; collecting effluent liquid in different tubes until silk fibroin is completely drained.
(5) And (3) identifying the molecular weight distribution of each tube by SDS-PAGE electrophoresis or mass spectrometry, mixing and freeze-drying the silk fibroin solution with the molecular weight of less than 10kDa, preparing into 30-80 mg/ml aqueous solution, and filtering by using a 0.45 mu m membrane to remove microparticles.
(6) Similar to the step (4), adding a proper amount of the silk fibroin aqueous solution obtained in the step (5) into the column material of G-25, controlling the flow rate of the eluent by a peristaltic pump to be 50mL/h, collecting the eluent in different tubes until the silk fibroin is completely drained to obtain the silk fibroin aqueous solution with the molecular weight of 1000-5000 Da, and finally freeze-drying and storing.
(7) And (3) boiling the woven polyester fabric for about 1 hour at 100 ℃ by using 6g/1L of sodium carbonate aqueous solution, taking out the woven polyester fabric, repeatedly washing the woven polyester fabric by using tap water, soaking the woven polyester fabric in 0.5% mass concentration of the silk fibroin aqueous solution obtained in the step (6), continuously acting at room temperature for the same time as that in the examples 1-4, taking out, airing, rinsing and re-airing.
(8) The weight gain of silk fibroin on the terylene fabric is measured by a weighing method to be 0.9 percent, and the hot water dissolution loss rate of the silk fibroin is about 25 percent.
Comparative example 2
(1) The method comprises the steps of putting silkworm raw silk into a sodium carbonate aqueous solution with the concentration of 0.2% according to the bath ratio of 1:50(g/mL), treating for three times at the temperature of 98-100 ℃ for 30 minutes each time, then fully cleaning the silk with deionized water, loosening, and drying in an oven to obtain the degummed silkworm fibroin fiber.
(2) Weighing degummed bombyx mori silk fibroin, dissolving in a calcium chloride-ethanol aqueous solution with a molar ratio of 1:2 according to a bath ratio of 1:20(g/mL), and dissolving at 70 ℃ for 5-7 hours to obtain a bombyx mori silk fibroin dissolved mixed solution.
(3) Weighing glucan G-50 and G-25, respectively putting into sufficient deionized water, boiling water bath for 1.5 hours, cooling at normal temperature, then draining with a glass rod, filling into a hollow column made of glass, preparing a column bed with a volume of 2cm multiplied by 60cm, naturally settling for 2 hours, pressurizing with a peristaltic pump, and balancing the column with 5 times of column volume of deionized water for three times.
(4) When the balance water is lowered to the surface of the column material for the last time, adding 5-15 mL (10-50 mg/mL) of dissolved silk fibroin mixed solution into the glucan G-50, when the silk fibroin mixed solution completely enters the surface of the column material, continuously eluting with sterilized deionized water, and controlling the flow rate of eluent by using a peristaltic pump to be 300 mL/h; collecting effluent liquid in different tubes until silk fibroin is completely drained.
(5) And (3) identifying the molecular weight distribution of each tube by SDS-PAGE electrophoresis or mass spectrometry, mixing and freeze-drying the silk fibroin solution with the molecular weight of less than 10kDa, preparing into 30-80 mg/ml aqueous solution, and filtering by using a 0.45 mu m membrane to remove microparticles.
(6) Similar to the step (4), adding a proper amount of the silk fibroin aqueous solution obtained in the step (5) into the column material of G-25, controlling the flow rate of the eluent by a peristaltic pump to be 50mL/h, collecting the eluent in different tubes until the silk fibroin is completely drained to obtain the silk fibroin aqueous solution with the molecular weight of 1000-5000 Da, and finally freeze-drying and storing.
(7) And (3) boiling the woven polyester fabric for about 1 hour at 100 ℃ by using 6g/1L of sodium carbonate aqueous solution, taking out the woven polyester fabric, repeatedly washing the woven polyester fabric by using tap water, soaking the woven polyester fabric in the silk fibroin aqueous solution obtained in the step (6) with the mass concentration of 1%, continuously acting at room temperature for the same time as that of the embodiment 1-4, taking out, airing, rinsing and re-airing.
(8) The weight gain of silk fibroin on the terylene fabric is measured by a weighing method to be 0.92 percent, and the hot water dissolution loss rate of the silk fibroin is about 25 percent.
Comparative example 3
(1) The method comprises the steps of putting silkworm raw silk into a sodium carbonate aqueous solution with the concentration of 0.2% according to the bath ratio of 1:50(g/mL), treating for three times at the temperature of 98-100 ℃ for 30 minutes each time, then fully cleaning the silk with deionized water, loosening, and drying in an oven to obtain the degummed silkworm fibroin fiber.
(2) Weighing degummed bombyx mori silk fibroin, dissolving in 9.3M lithium bromide aqueous solution according to a bath ratio of 1:15(g/mL), and dissolving at 65 ℃ for 5-7 hours to obtain a bombyx mori silk fibroin dissolving mixed solution.
(3) The silkworm fibroin dissolving solution is filled into a dialysis bag, the wall of the dialysis bag is a semipermeable membrane, the molecular weight cutoff is within the range of 12.0-16.0 kDa, the dialysis bag filled with the silkworm fibroin dissolving solution is placed into a container filled with deionized water, the water in the container is replaced by new deionized water or pure water every 2 hours, dialysis is continued for 3 days, and a purified silkworm fibroin aqueous solution (the preparation of a conventional fibroin aqueous solution) is obtained and then freeze-dried for storage.
(4) Preparing a silk fibroin solution with the mass ratio of 1% by using freeze-dried silk fibroin, adding polyethylene glycol diglycidyl ether accounting for 80% of the mass ratio of the silk fibroin, and uniformly stirring.
(5) Boiling the woven polyester fabric for about 1 hour by using 6g/1L sodium carbonate aqueous solution, taking out, washing, dehydrating, airing or drying by using tap water, then treating the polyester fabric for 1-2 hours at 30 ℃ by using 10% sodium hydroxide solution, rinsing, soaking in silk fibroin solution containing polyethylene glycol diglycidyl ether for reacting for 3 hours, taking out, airing, rinsing and airing again.
(6) The silk fibroin modified polyester fabric is cut into a sample of 15cm multiplied by 30cm, the breaking strength is about 97 percent of the original fabric, and the breaking elongation is about 97 percent of the original fabric.
(7) The weight gain of silk fibroin on the terylene fabric is 1.1% measured by adopting a weighing method, and the dissolution rate of the silk fibroin is less than 10% measured after the silk fibroin modified fabric is soaked in warm water at 37 ℃ and oscillated for 24 hours.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (9)
1. A method for modifying protein of polyester fabric is characterized by comprising the following steps:
A) desizing the polyester fabric to obtain a desized fabric;
B) treating the desized fabric with sodium hydroxide, and washing to obtain the fabric subjected to alkali treatment;
C) soaking the fabric subjected to alkali treatment in a cross-linking agent solution, and mixing and reacting with silk fibroin with the molecular weight of 1000-5000 Da; the crosslinking agent comprises polyethylene glycol diglycidyl ether;
the silk fibroin with the molecular weight of 1000-5000 Da is prepared by the following method:
a) degumming silkworm silk by using sodium carbonate, and then adding a neutral salt solution to dissolve to prepare a silk fibroin dissolving solution;
the dextran Sephadex G50 and G25 columns are balanced for standby;
b) adding the silk fibroin dissolving solution into a glucan Sephadex G50 column, eluting the silk fibroin with sterile water, and collecting desalted silk fibroin aqueous solution in a branch pipe;
c) and (b) screening the silk fibroin with the molecular weight of less than 10kD in the collection tube in the step b) by SDS-PAGE electrophoresis or mass spectrometry, adding the silk fibroin into a dextran Sephadex G25 column again, eluting the silk fibroin by using sterilized water, collecting the silk fibroin in different tubes, and screening to obtain the silk fibroin with the small molecular weight of 1000-5000 Da.
2. The method as claimed in claim 1, wherein the polyethylene glycol diglycidyl ether accounts for 30-100% of the silk fibroin by mass.
3. The method according to claim 1, characterized in that the desizing in step a) is in particular a desizing treatment with sodium carbonate; the concentration of the sodium carbonate solution is 6 g/L; the desizing treatment temperature is 90-100 ℃; the desizing treatment time is 1 h.
4. The method according to claim 1, wherein the mass concentration of the sodium hydroxide in the step B) is 5-30%; the treatment temperature of the sodium hydroxide is 30-40 ℃; the treatment time of the sodium hydroxide is 1-3 h.
5. The method according to claim 1, wherein the reaction temperature in step C) is 25-35 ℃; the reaction time is 1-3 h.
6. The process according to claim 1, wherein the neutral salt solution of step a) is selected from lithium bromide or calcium chloride-ethanol; the dissolving time is 5-7 hours; the concentration of the silk fibroin dissolving solution is 10-50 mg/mL.
7. The method of claim 1, wherein the step c) of screening the silk fibroin with a molecular weight of less than 10kD in the collection tube of step b) further comprises freeze-drying, and then preparing into an aqueous solution of 30-80 mg/mL.
8. The method according to claim 1, wherein the elution flow rate in step b) is 200-400 mL/h.
9. The method according to claim 1, wherein the elution flow rate in step c) is 30-70 mL/h.
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| CN113330057A (en) * | 2019-01-28 | 2021-08-31 | 现代牧场股份有限公司 | Protein coated materials |
| CN113106756A (en) * | 2021-03-10 | 2021-07-13 | 浙江凯喜雅国际股份有限公司 | Fibroin coating liquid and application thereof in fiber or fabric surface modification |
| CN113940461A (en) * | 2021-10-18 | 2022-01-18 | 厦门鹏嘉得服装织造有限公司 | Moisture-absorbing and breathable shirt fabric and shirt made of same |
| CN114737293A (en) * | 2022-05-11 | 2022-07-12 | 吴江市兰天织造有限公司 | Production process of polyester weft-elastic double-layer down-filled cloth |
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