CN112900083A - Preparation method of antibacterial and antistatic real silk fabric - Google Patents

Preparation method of antibacterial and antistatic real silk fabric Download PDF

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Publication number
CN112900083A
CN112900083A CN201911220789.0A CN201911220789A CN112900083A CN 112900083 A CN112900083 A CN 112900083A CN 201911220789 A CN201911220789 A CN 201911220789A CN 112900083 A CN112900083 A CN 112900083A
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silk fibroin
soaking
drying
fiber
preparation
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胡士良
胡志明
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Shengzhou Haoyunlai Printing And Dyeing Co ltd
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Shengzhou Haoyunlai Printing And Dyeing Co ltd
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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
    • D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/10—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing oxygen
    • D06M13/224—Esters of carboxylic acids; Esters of carbonic acid
    • D06M13/238—Tannins, e.g. gallotannic acids
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01B—MECHANICAL TREATMENT OF NATURAL FIBROUS OR FILAMENTARY MATERIAL TO OBTAIN FIBRES OF FILAMENTS, e.g. FOR SPINNING
    • D01B7/00—Obtaining silk fibres or filaments
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01C—CHEMICAL OR BIOLOGICAL TREATMENT OF NATURAL FILAMENTARY OR FIBROUS MATERIAL TO OBTAIN FILAMENTS OR FIBRES FOR SPINNING; CARBONISING RAGS TO RECOVER ANIMAL FIBRES
    • D01C3/00—Treatment of animal material, e.g. chemical scouring of wool
    • 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
    • D06M11/44—Oxides or hydroxides of elements of Groups 2 or 12 of the Periodic Table; Zincates; Cadmates
    • 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
    • D06M11/51—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 sulfur, selenium, tellurium, polonium or compounds thereof
    • D06M11/53—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 sulfur, selenium, tellurium, polonium or compounds thereof with hydrogen sulfide or its salts; with polysulfides
    • 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
    • D06M11/58—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 nitrogen or compounds thereof, e.g. with nitrides
    • D06M11/64—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 nitrogen or compounds thereof, e.g. with nitrides with nitrogen oxides; with oxyacids of nitrogen or their salts
    • D06M11/65—Salts of oxyacids of nitrogen
    • 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
    • D06M16/00—Biochemical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. enzymatic
    • 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
    • D06M2101/02—Natural fibres, other than mineral fibres
    • D06M2101/10—Animal fibres

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

Abstract

The invention discloses a preparation method of an antibacterial and antistatic real silk fabric, which is obtained by the following steps: preparing silk fibroin fibers, pretreating, immersing the silk fibroin fibers in finishing liquid, dehydrating, soaking, dehydrating, drying and ironing to obtain a finished product. The surface of the real silk fiber prepared by the method is covered with the antibacterial conductive layer which is continuously and uniformly distributed, so that the real silk fiber has excellent antibacterial property and good conductivity.

Description

Preparation method of antibacterial and antistatic real silk fabric
Technical Field
The invention belongs to the technical field of printing and dyeing, and particularly relates to a preparation method of an antibacterial and antistatic real silk fabric.
Background
Silk broadcloth is one of the most comfortable and highest-grade fabrics as underwear and shirts, and is a hygienic textile fabric, but since the silk broadcloth is protein fiber, the silk broadcloth is a good foodstuff of mould and bacteria. When the relative humidity is more than 85%, the temperature is 5-50 ℃, and the pH value is less than 5, the mold is easy to propagate on silk fibers, bacteria grow on silk fibers when the pH value is more than 6, the pure silk contains much water, or residual sericin, soap, oil or residual starch slurry of printed silk is more, the mold and the bacteria are easy to propagate under the damp and hot conditions, so that the protein fibers are degraded, chain broken and damaged strongly.
Disclosure of Invention
The invention aims to provide a preparation method of an antibacterial and antistatic real silk fabric, which has the advantages of antibacterium and antistatic property.
The technical scheme adopted by the invention is as follows: a preparation method of an antibacterial antistatic real silk fabric comprises the following steps:
preparing silk fibroin fibers: removing pupa from fresh cocoon of silkworm, drying cocoon layer in dryer, refining with 0.5-0.8% mercerized soap solution, and adding 0.05-0.1% Na2CO3Soaking in the solution for 10-20min, taking out, cleaning with distilled water, drying, and extracting wax in diethyl ether for 40-48 hr to obtain pure silk fibroin fiber;
pretreatment: soaking pure silk fibroin fiber and 4.76-4.8% tannin solution at bath ratio of 98-100:1 at 60-70 deg.C for 2-2.5h, taking out silk fibroin fiber, and drying;
immersing in finishing liquid: immersing the dried silk fibroin fibers into a metal complex solution for oscillation;
and (3) dehydrating: washing with distilled water and methanol, and vacuum drying;
soaking: soaking the dehydrated silk fibroin fibers in an adhesive;
dehydrating;
drying;
ironing;
and obtaining a finished product.
Preferably, the metal complex solution consists of, in weight percent: 6-8% of copper nitrate monohydrate, 1-2% of silver nitrate, 2-3% of zinc nitrate, 2-4% of nickel nitrate, 6-10% of sulfur-containing reducing agent, 2-5% of nano zinc oxide and the balance of water.
Preferably, the bath ratio in step 3 is 98-100:1, the temperature is 20-35 ℃, and the oscillation time is 24-26 h.
Preferably, the soaking time in the step 5 is 30-40min, and the bath ratio is 1: 9-12; the temperature is 35-55 ℃.
Compared with the prior art, the invention has the beneficial effects that: the silk fibroin fibers treated by the tannic acid and the metal complex fibers prepared in the aqueous solution of copper, zinc and nickel ammonia complexes generate a planar metal tannic acid complex which is firmly combined with the silk fibroin fibers, so that the silk fibroin fibers have strong bactericidal performance on staphylococcus aureus and klebsiella, and the silk fabrics have higher absorption capacity on Ag + through the tannic acid treatment, so that the silk-tannic acid-Ag complex which is stable abnormally is formed, and the silk-tannic acid-Ag complex has excellent antibacterial property; meanwhile, the copper nitrate monohydrate reacts with the sulfur-containing reducing agent, so that the surface of the real silk is covered with the CuS antibacterial conductive layer which is continuously and uniformly distributed, and the prepared real silk fiber has excellent antibacterial property and good conductivity.
Detailed Description
The technical solutions in the embodiments of the present invention are clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments.
Example 1
A preparation method of an antibacterial antistatic real silk fabric comprises the following steps:
preparing silk fibroin fibers: removing pupa from fresh cocoon of Bombyx mori, drying cocoon layer in dryer, refining with 0.8% mercerized soap solution, and adding 0.06% Na2CO3Soaking in the solution for 15min, taking out, cleaning with distilled water, drying, and extracting wax in diethyl ether for 45 hr to obtain pure silk fibroin fiber;
pretreatment: soaking pure silk fibroin fiber and 4.78% tannin solution at bath ratio of 100:1 at 65 deg.C for 2.5 hr, taking out silk fibroin fiber, and drying;
immersing in finishing liquid: immersing the dried silk fibroin fibers into a metal complex solution for oscillation at the bath ratio of 100:1 and the temperature of 28 ℃ for 24 hours;
and (3) dehydrating: washing with distilled water and methanol, and vacuum drying;
soaking: soaking the dehydrated silk fibroin fibers in an adhesive for 35min at a bath ratio of 1:10 and a temperature of 45 ℃;
dehydrating;
drying;
ironing;
and obtaining a finished product.
The metal complex solution comprises the following components in percentage by weight: 6% of copper nitrate monohydrate, 1% of silver nitrate, 2% of zinc nitrate, 2% of nickel nitrate, 6% of sulfur-containing reducing agent, 2% of nano zinc oxide and the balance of water. The addition of the nano zinc oxide means that under the condition of no illumination, the nano ZnO continuously and slowly releases Zn2+ in the aqueous medium, and Zn2+ can penetrate through cell membranes to enter the cells. The cell membrane is damaged and simultaneously reacts with certain groups on the protein, the structure and the physiological activity of the thallus are damaged, and the thallus enters the thallus to damage the enzyme of an electron transfer system and reacts with-SH to achieve the aim of sterilization;
the experimental results prove that: the bacteriostasis rate of the treated real silk fiber to escherichia coli, staphylococcus aureus and candida albicans reaches 98%, and after 20 times of washing, the fabric still has high bacteriostasis rate, and the concentration of copper ions on the fiber is 3.13 multiplied by 10 tested by an atomic spectrophotometer-4mol/g; volume specific resistance ρνFrom 9.2X 109Omega cm is reduced to 57.6 omega cm, and the washing fastness is good, and rho is obtained after 20 times of washingνThe increase is not large, and the real silk fiber is still in the same order of magnitude, and the real silk fiber prepared by the method not only has excellent antibacterial property, but also has good conductivity.
Example 2
A preparation method of an antibacterial antistatic real silk fabric comprises the following steps:
preparing silk fibroin fibers: removing pupa from fresh cocoon of Bombyx mori, drying cocoon layer in dryer, refining with 0.8% mercerized soap solution, and adding 0.1% Na2CO3Soaking in the solution for 15min, taking out, cleaning with distilled water, drying, and extracting wax in diethyl ether for 46h to obtain pure silk fibroin fiber;
pretreatment: soaking pure silk fibroin fiber and 4.76% tannin solution at bath ratio of 98:1 at 70 deg.C for 2.5 hr, taking out silk fibroin fiber, and drying;
immersing in finishing liquid: immersing the dried silk fibroin fibers into a metal complex solution for oscillation at the bath ratio of 99:1 and the temperature of 32 ℃ for 25 h;
and (3) dehydrating: washing with distilled water and methanol, and vacuum drying;
soaking: soaking the dehydrated silk fibroin fibers in an adhesive for 37min at a bath ratio of 1:11 and a temperature of 38 ℃;
dehydrating;
drying;
ironing;
and obtaining a finished product.
The metal complex solution comprises the following components in percentage by weight: 8% of copper nitrate monohydrate, 2% of silver nitrate, 3% of zinc nitrate, 4% of nickel nitrate, 10% of sulfur-containing reducing agent, 5% of nano zinc oxide and the balance of water. When light irradiates on the surface of the nano ZnO, electrons in a valence band obtain the energy of photons and jump to a conduction band, the formed photogenerated electrons are negatively charged (e-), corresponding positively charged holes (H +) are formed in the valence band, the photogenerated electrons (e-) on the surface are easily captured by oxygen dissolved in water to form negative oxygen ions (O2-), and the holes H + can oxidize H2O molecules adsorbed on the surface of the ZnO to form hydroxyl radicals (-OH). O2-and-OH have strong oxidizing power and can rapidly oxidize cell components and destroy macromolecules in cell walls and cytoplasm, thereby killing bacteria.
The experimental results prove that: the bacteriostasis rate of the treated real silk fiber to escherichia coli, staphylococcus aureus and candida albicans reaches 98.5%, and the fabric still has high bacteriostasis rate after being washed for 20 times, and the concentration of copper ions on the fiber is 3.03 multiplied by 10 through the test of an atomic spectrophotometer-4mol/g; volume specific resistance ρνFrom 9.2X 109Omega cm is reduced to 56.6 omega cm, and the washing fastness is good, and rho is obtained after 20 times of washingνThe increase is not large, and the real silk fiber is still in the same order of magnitude, and the real silk fiber prepared by the method not only has excellent antibacterial property, but also has good conductivity.
Example 3
A preparation method of an antibacterial antistatic real silk fabric comprises the following steps:
preparing silk fibroin fibers: removing pupa from fresh silkworm cocoon, drying cocoon layer in drier, and refining with 0.56% mercerized soap solutionRefining, adding 0.07% Na2CO3Soaking in the solution for 12min, taking out, cleaning with distilled water, drying, and taking out wax in diethyl ether for 40-48 hr to obtain pure silk fibroin fiber;
pretreatment: soaking pure silk fibroin fiber and 4.76-4.8% tannic acid solution at bath ratio of 98-100:1 at 61 deg.C for 2.5h, taking out and drying silk fibroin fiber;
immersing in finishing liquid: immersing the dried silk fibroin fibers into a metal complex solution for oscillation at the bath ratio of 98:1 and the temperature of 25 ℃ for 24 hours;
and (3) dehydrating: washing with distilled water and methanol, and vacuum drying;
soaking: soaking the dehydrated silk fibroin fibers in an adhesive for 32min at a bath ratio of 1: 12; the temperature is 38 ℃;
dehydrating;
drying;
ironing;
and obtaining a finished product.
The metal complex solution comprises the following components in percentage by weight: 7% of copper nitrate monohydrate, 1.5% of silver nitrate, 2.2% of zinc nitrate, 2.2% of nickel nitrate, 7% of sulfur-containing reducing agent, 3.5% of nano zinc oxide and the balance of water.
The experimental results prove that: the bacteriostasis rate of the treated real silk fiber to escherichia coli, staphylococcus aureus and candida albicans reaches 98.3%, the fabric still has high bacteriostasis rate after 20 times of washing, and the concentration of copper ions on the fiber is 3.14 multiplied by 10 through the test of an atomic spectrophotometer-4mol/g; volume specific resistance ρνFrom 9.2X 109Omega cm is reduced to 56.2 omega cm, and the washing fastness is good, and rho is obtained after 20 times of washingνThe increase is not large, and the real silk fiber is still in the same order of magnitude, and the real silk fiber prepared by the method not only has excellent antibacterial property, but also has good conductivity.
Example 4
A preparation method of an antibacterial antistatic real silk fabric comprises the following steps:
preparing silk fibroin fibers: removing pupa from fresh silkworm cocoon, and laying cocoon layerDrying in a dryer, refining with 0.59% mercerized soap solution, adding 0.09% Na2CO3Soaking in the solution for 13min, taking out, cleaning with distilled water, drying, and extracting wax in diethyl ether for 45 hr to obtain pure silk fibroin fiber;
pretreatment: soaking pure silk fibroin fiber and 4.78% tannin solution at bath ratio of 100:1 at 68 deg.C for 2.3 hr, taking out silk fibroin fiber, and drying;
immersing in finishing liquid: immersing the dried silk fibroin fibers into a metal complex solution for oscillation at the bath ratio of 100:1 and the temperature of 23 ℃ for 25 h;
and (3) dehydrating: washing with distilled water and methanol, and vacuum drying;
soaking: soaking the dehydrated silk fibroin fibers in an adhesive for 37min at a bath ratio of 1: 10; the temperature is 42 ℃;
dehydrating;
drying;
ironing;
and obtaining a finished product.
The metal complex solution comprises the following components in percentage by weight: 6.8% of copper nitrate monohydrate, 1.2% of silver nitrate, 2.3% of zinc nitrate, 2.4% of nickel nitrate, 6.1% of sulfur-containing reducing agent, 2.5% of nano zinc oxide and the balance of water.
The experimental results prove that: the bacteriostasis rate of the treated real silk fiber to escherichia coli, staphylococcus aureus and candida albicans reaches 98%, and after 20 times of washing, the fabric still has high bacteriostasis rate, and the concentration of copper ions on the fiber is 3.12 multiplied by 10 tested by an atomic spectrophotometer-4mol/g; volume specific resistance ρνFrom 9.2X 109Omega cm is reduced to 57.5 omega cm, and the washing fastness is good, and rho is obtained after 20 times of washingνThe increase is not large, and the real silk fiber is still in the same order of magnitude, and the real silk fiber prepared by the method not only has excellent antibacterial property, but also has good conductivity.
Example 5
A preparation method of an antibacterial antistatic real silk fabric comprises the following steps:
preparing silk fibroin eggWhite fibers: removing pupa from fresh cocoon of Bombyx mori, drying cocoon layer in dryer, refining with 0.58% mercerized soap solution, and adding 0.06% Na2CO3Soaking in the solution for 18min, taking out, cleaning with distilled water, drying, and extracting wax in diethyl ether for 46h to obtain pure silk fibroin fiber;
pretreatment: soaking pure silk fibroin fiber and 4.8% tannin solution at bath ratio of 100:1 at 69 deg.C for 2.4 hr, taking out silk fibroin fiber, and drying;
immersing in finishing liquid: immersing the dried silk fibroin fibers into a metal complex solution for oscillation at the bath ratio of 100:1 and the temperature of 33 ℃ for 25 h;
and (3) dehydrating: washing with distilled water and methanol, and vacuum drying;
soaking: soaking the dehydrated silk fibroin fibers in an adhesive for 35min at a bath ratio of 1: 10; the temperature is 52 ℃;
dehydrating;
drying;
ironing;
and obtaining a finished product.
The metal complex solution comprises the following components in percentage by weight: 8% of copper nitrate monohydrate, 2% of silver nitrate, 3% of zinc nitrate, 4% of nickel nitrate, 10% of sulfur-containing reducing agent, 5% of nano zinc oxide and the balance of water.
The experimental results prove that: the bacteriostasis rate of the treated real silk fiber to escherichia coli, staphylococcus aureus and candida albicans reaches 99.5%, and the fabric still has high bacteriostasis rate after being washed for 20 times, and the concentration of copper ions on the fiber is 3.15 multiplied by 10 through the test of an atomic spectrophotometer-4mol/g; volume specific resistance ρνFrom 9.2X 109Omega cm is reduced to 58.1 omega cm, and the washing fastness is good, and rho is obtained after 20 times of washingνThe increase is not large, and the real silk fiber is still in the same order of magnitude, and the real silk fiber prepared by the method not only has excellent antibacterial property, but also has good conductivity.
Example 6
A preparation method of an antibacterial antistatic real silk fabric comprises the following steps:
preparing silk fibroin fibers: removing pupa from fresh cocoon of Bombyx mori, drying cocoon layer in dryer, refining with 0.8% mercerized soap solution, and adding 0.06% Na2CO3Soaking in the solution for 15min, taking out, cleaning with distilled water, drying, and extracting wax in diethyl ether for 48 hr to obtain pure silk fibroin fiber;
pretreatment: soaking pure silk fibroin fiber and 4.76% tannin solution at bath ratio of 98:1 at 66 deg.C for 2 hr, taking out silk fibroin fiber, and drying;
immersing in finishing liquid: immersing the dried silk fibroin fibers into a metal complex solution for oscillation at the bath ratio of 100:1 and the temperature of 28 ℃ for 24 hours;
and (3) dehydrating: washing with distilled water and methanol, and vacuum drying;
soaking: soaking the dehydrated silk fibroin fibers in an adhesive for 38min at a bath ratio of 1: 11; the temperature is 45 ℃;
dehydrating;
drying;
ironing;
and obtaining a finished product.
The metal complex solution comprises the following components in percentage by weight: 7.2% of copper nitrate monohydrate, 1.5% of silver nitrate, 2.5% of zinc nitrate, 3.2% of nickel nitrate, 8% of sulfur-containing reducing agent, 4.5% of nano zinc oxide and the balance of water.
The experimental results prove that: the bacteriostasis rate of the treated real silk fiber to escherichia coli, staphylococcus aureus and candida albicans reaches 98.6%, and the fabric still has high bacteriostasis rate after being washed for 20 times, and the concentration of copper ions on the fiber is 3.12 multiplied by 10 through the test of an atomic spectrophotometer-4mol/g; volume specific resistance ρνFrom 9.2X 109Omega cm is reduced to 57.4 omega cm, and the washing fastness is good, and rho is obtained after 20 times of washingνThe increase is not large, and the real silk fiber is still in the same order of magnitude, and the real silk fiber prepared by the method not only has excellent antibacterial property, but also has good conductivity.
Example 7
A preparation method of an antibacterial antistatic real silk fabric comprises the following steps:
preparing silk fibroin fibers: removing pupa from fresh cocoon of Bombyx mori, drying cocoon layer in dryer, refining with 0.6% mercerized soap solution, and adding 0.08% Na2CO3Soaking in the solution for 18min, taking out, cleaning with distilled water, drying, and extracting wax in diethyl ether for 43 hr to obtain pure silk fibroin fiber;
pretreatment: soaking pure silk fibroin fiber and 4.8% tannin solution at bath ratio of 98:1 at 60 deg.C for 2 hr, taking out silk fibroin fiber, and drying;
immersing in finishing liquid: immersing the dried silk fibroin fibers into a metal complex solution for oscillation at the bath ratio of 99:1 and the temperature of 25 ℃ for 26 h;
and (3) dehydrating: washing with distilled water and methanol, and vacuum drying;
soaking: soaking the dehydrated silk fibroin fibers in an adhesive for 37min at a bath ratio of 1: 11; the temperature is 40 ℃;
dehydrating;
drying;
ironing;
and obtaining a finished product.
The metal complex solution comprises the following components in percentage by weight: 6-8% of copper nitrate monohydrate, 1-2% of silver nitrate, 2-3% of zinc nitrate, 2-4% of nickel nitrate, 6-10% of sulfur-containing reducing agent, 2-5% of nano zinc oxide and the balance of water.
The experimental results prove that: the bacteriostasis rate of the treated real silk fiber to escherichia coli, staphylococcus aureus and candida albicans reaches 98%, and after 20 times of washing, the fabric still has high bacteriostasis rate, and the concentration of copper ions on the fiber is 3.13 multiplied by 10 tested by an atomic spectrophotometer-4mol/g; volume specific resistance ρνFrom 9.2X 109Omega cm is reduced to 57.6 omega cm, and the washing fastness is good, and rho is obtained after 20 times of washingνThe increase is not large, and the real silk fiber is still in the same order of magnitude, and the real silk fiber prepared by the method not only has excellent antibacterial property, but also has good conductivity.
Example 8
A preparation method of an antibacterial antistatic real silk fabric comprises the following steps:
preparing silk fibroin fibers: removing pupa from fresh cocoon of silkworm, drying cocoon layer in dryer, refining with 0.5-0.8% mercerized soap solution, and adding 0.05-0.1% Na2CO3Soaking in the solution for 10-20min, taking out, cleaning with distilled water, drying, and extracting wax in diethyl ether for 40-48 hr to obtain pure silk fibroin fiber;
pretreatment: soaking pure silk fibroin fiber and 4.76-4.8% tannin solution at bath ratio of 98-100:1 at 60-70 deg.C for 2-2.5h, taking out silk fibroin fiber, and drying;
immersing in finishing liquid: immersing the dried silk fibroin fiber into a metal complex solution for oscillation at the bath ratio of 98-100:1 and the temperature of 20-35 ℃ for 24-26 h;
and (3) dehydrating: washing with distilled water and methanol, and vacuum drying;
soaking: soaking the dehydrated silk fibroin fibers in an adhesive for 30-40min at a bath ratio of 1: 9-12; the temperature is 35-55 ℃;
dehydrating;
drying;
ironing;
and obtaining a finished product.
The metal complex solution comprises the following components in percentage by weight: 7.5% of copper nitrate monohydrate, 1.6% of silver nitrate, 2.6% of zinc nitrate, 3.5% of nickel nitrate, 9.5% of sulfur-containing reducing agent, 4.5% of nano zinc oxide and the balance of water.
The experimental results prove that: the bacteriostasis rate of the treated real silk fiber to escherichia coli, staphylococcus aureus and candida albicans reaches 98%, and after 20 times of washing, the fabric still has high bacteriostasis rate, and the concentration of copper ions on the fiber is 3.14 multiplied by 10 tested by an atomic spectrophotometer-4mol/g; volume specific resistance ρνFrom 9.2X 109Omega cm is reduced to 56.3 omega cm, and the washing fastness is good, and rho is obtained after 20 times of washingνThe increase is not large, and is still same order of magnitude, the real silk fiber prepared by the method not only has excellent performanceHas good antibacterial property and conductivity.
Conventional operations in the operation steps of the present invention are well known to those skilled in the art and will not be described herein.
The embodiments described above are intended to illustrate the technical solutions of the present invention in detail, and it should be understood that the above-mentioned embodiments are only specific embodiments of the present invention, and are not intended to limit the present invention, and any modification, supplement or similar substitution made within the scope of the principles of the present invention should be included in the protection scope of the present invention.

Claims (4)

1. The preparation method of the antibacterial antistatic real silk fabric is characterized by comprising the following steps of:
1) preparing silk fibroin fibers: removing pupa from fresh cocoon of silkworm, drying cocoon layer in dryer, refining with 0.5-0.8% mercerized soap solution, and adding 0.05-0.1% Na2CO3Soaking in the solution for 10-20min, taking out, cleaning with distilled water, drying, and extracting wax in diethyl ether for 40-48 hr to obtain pure silk fibroin fiber;
2) pretreatment: soaking pure silk fibroin fiber and 4.76-4.8% tannin solution at bath ratio of 98-100:1 at 60-70 deg.C for 2-2.5h, taking out silk fibroin fiber, and drying;
3) immersing in finishing liquid: immersing the dried silk fibroin fibers into a metal complex solution for oscillation;
4) and (3) dehydrating: washing with distilled water and methanol, and vacuum drying;
5) soaking: soaking the dehydrated silk fibroin fibers in an adhesive;
6) dehydrating;
7) drying;
8) ironing;
9) and obtaining a finished product.
2. The preparation method of the bacteriostatic antistatic real silk fabric according to claim 1, wherein the metal complex solution in the step 3 comprises the following components in percentage by weight: 6-8% of copper nitrate monohydrate, 1-2% of silver nitrate, 2-3% of zinc nitrate, 2-4% of nickel nitrate, 6-10% of sulfur-containing reducing agent, 2-5% of nano zinc oxide and the balance of water.
3. The preparation method of the bacteriostatic antistatic real silk fabric according to claim 1, wherein the bath ratio in the step 3 is 98-100:1, the temperature is 20-35 ℃, and the oscillation time is 24-26 h.
4. The preparation method of the bacteriostatic antistatic real silk fabric according to claim 1, wherein the soaking time in the step 5 is 30-40min, and the bath ratio is 1: 9-12; the temperature is 35-55 ℃.
CN201911220789.0A 2019-12-03 2019-12-03 Preparation method of antibacterial and antistatic real silk fabric Pending CN112900083A (en)

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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102936835A (en) * 2012-12-05 2013-02-20 苏州大学 Preparation method of nano-silver antibacterial real silk
CN105369606A (en) * 2015-10-30 2016-03-02 无锡市长安曙光手套厂 Anti-radiation odor-resistant fabric

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102936835A (en) * 2012-12-05 2013-02-20 苏州大学 Preparation method of nano-silver antibacterial real silk
CN105369606A (en) * 2015-10-30 2016-03-02 无锡市长安曙光手套厂 Anti-radiation odor-resistant fabric

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
赵为陶等: "银离子络合蚕丝纤维的工艺研究", 《丝绸》 *

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