CN111809395A - Antistatic overcoat finishing process - Google Patents

Antistatic overcoat finishing process Download PDF

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Publication number
CN111809395A
CN111809395A CN202010450902.0A CN202010450902A CN111809395A CN 111809395 A CN111809395 A CN 111809395A CN 202010450902 A CN202010450902 A CN 202010450902A CN 111809395 A CN111809395 A CN 111809395A
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parts
antistatic
finishing
wool fabric
washing
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余也
潘跃
林晓华
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Zhejiang Ugly Duck Industry Co ltd
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Zhejiang Ugly Duck Industry Co ltd
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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
    • D06M11/00Treating 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
    • D06M11/32Treating 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
    • D06M11/36Treating 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
    • D06M11/46Oxides or hydroxides of elements of Groups 4 or 14 of the Periodic Table; Titanates; Zirconates; Stannates; Plumbates
    • 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
    • D06M11/00Treating 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
    • D06M11/58Treating 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
    • D06M11/64Treating 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
    • D06M11/65Salts of oxyacids of nitrogen
    • 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
    • D06M13/00Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/322Treating 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 nitrogen
    • D06M13/325Amines
    • D06M13/328Amines the amino group being bound to an acyclic or cycloaliphatic carbon atom
    • 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

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  • Textile Engineering (AREA)
  • Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)

Abstract

The invention discloses an antistatic overcoat finishing process, which has the technical scheme key points that the process comprises the following steps: s1 pretreatment: immersing the wool fabric into pretreatment liquid at the temperature of 50-60 ℃, treating for 30-40min, taking out after completion, and washing and drying for later use; s2 finishing silk fibroin: pretreating a wool fabric by S1, immersing the pretreated wool fabric into the silk fibroin finishing liquid, immersing for two times, rolling for two times, pre-drying for 3-5min at 75-80 ℃, then baking for 60-90S at 140-160 ℃, and finally washing and drying for later use; s3 antistatic finishing: the wool fabric is treated by silk fibroin S2 and then is immersed into antistatic finishing liquid at the temperature of 55-65 ℃, taken out and then is baked for 90-120S at the temperature of 120-130 ℃, and finally is washed and dried for standby; and S4 cleaning. Finishing the wool fabric with silk fibroin S2, and coating a layer of silk fibroin film on the surface of the fiber; after S3 antistatic finishing, a large amount of modified nano titanium dioxide is attached to the surface of the silk fibroin film, so that the wool fabric has excellent antistatic property and washing fastness.

Description

Antistatic overcoat finishing process
Technical Field
The invention relates to clothes, in particular to an antistatic overcoat finishing process.
Background
The overcoat is an overcoat which is worn outside the clothes and has a wind-cold defense function, and the length of the overcoat is up to the waist and below. The overcoat fabric has a plurality of types, and the high-grade overcoat fabric has wool fabric. The natural characteristic of the wool fiber enables the wool overcoat to have incomparable comfort, thick texture and good heat retention. When the textile material is rubbed by the outside to generate a large amount of charges and cannot be quickly dissipated, static electricity is generated. Due to the existence of the scale layer, the wool fabric has hydrophobicity, rough and uneven surface and higher friction coefficient, and is easy to generate static electricity, especially in a dry environment.
If the surface of the fabric is provided with a large amount of static charges, the fabric is easy to adsorb dust in the air and has serious influence on the human health. In order to improve the antistatic performance of the wool overcoat, the wool overcoat needs to be subjected to antistatic finishing.
Chinese patent publication No. CN105696343A discloses an antistatic finishing method for wool fabric, which comprises the following steps: firstly, adding water into a finishing agent to prepare a dipping solution, then putting the fabric into the dipping solution for padding, wherein the padding rate is 70-80%, finally washing for 2-3 times, and dehydrating and drying; the finishing agent comprises the following components in parts by weight: 20-25 parts of polyoxyethylene diamine, 12-15 parts of N- (phosphonomethyl) glycine isopropylamine, 6-9 parts of benzyl trimethyl ammonium chloride, 2-4 parts of sodium carboxymethyl starch, 10-14 parts of linolenic acid, 2-5 parts of acetone, 1-6 parts of acrylamide, 4-9 parts of fibraurea stem powder, 3-6 parts of polyvinyl alcohol, 15-17 parts of styrene, 5-8 parts of sodium fatty acid, 3-6 parts of sodium citrate and 1-8 parts of aluminum sulfate.
By the antistatic finishing method, the antistatic agent is applied to the surface of the fiber, so that the hydrophilicity of the fabric is improved, static is prevented from accumulating on the surface of the fiber, the charge releasing capacity of the fabric is improved, and the wool overcoat has antistatic property. However, with the cleaning and washing of the overcoat, the antistatic property of the overcoat is gradually deteriorated and is not durable enough to be improved.
Disclosure of Invention
In view of the technical defects, the invention aims to provide an antistatic overcoat finishing process, and the overcoat has excellent antistatic property and washing fastness after finishing.
In order to achieve the purpose, the invention provides the following technical scheme:
an antistatic overcoat finishing process relates to an overcoat woven by wool fabric, and comprises the following steps:
s1 pretreatment: immersing the wool fabric into pretreatment liquid at the temperature of 50-60 ℃, treating for 30-40min, taking out after completion, and washing and drying for later use;
s2 finishing silk fibroin: pretreating a wool fabric by S1, immersing the pretreated wool fabric into the silk fibroin finishing liquid, immersing for two times, rolling for two times, pre-drying for 3-5min at 75-80 ℃, then baking for 60-90S at 140-160 ℃, and finally washing and drying for later use;
s3 antistatic finishing: the wool fabric is treated by silk fibroin S2 and then is immersed into antistatic finishing liquid at the temperature of 55-65 ℃, taken out and then is baked for 90-120S at the temperature of 120-130 ℃, and finally is washed and dried for standby;
s4 cleaning: after S3 antistatic finishing, sequentially soaping and washing the wool fabric with water at the temperature of 40-50 ℃, and finally drying;
the preparation process of the antistatic finishing liquid is as follows:
firstly, uniformly mixing 10-15 parts of KH550, 15-20 parts of deionized water and 30-40 parts of absolute ethyl alcohol, adding 15-20 parts of nano titanium dioxide, performing ultrasonic dispersion for 20-30min, heating to 70-80 ℃, refluxing for 2-3h, and finally filtering, washing with ethanol, drying and grinding to obtain a pre-product;
secondly, uniformly mixing 6-8 parts of the pre-product, 10-15 parts of triethylamine and 200 parts of 150-one tetrahydrofuran, introducing nitrogen for protection, dropwise adding a mixed solution of 10-15 parts of 2-bromoisobutyl acyl bromide and 30-40 parts of tetrahydrofuran, continuously stirring for 2-3h in an ice bath at the temperature of 0-2 ℃, standing for 12-24h at the temperature of 20-25 ℃, and finally filtering and drying to obtain a secondary product;
step three, uniformly mixing 10-15 parts of secondary product, 3-5 parts of copper bromide, 20-30 parts of fluorine-containing acrylate monomer and 400 parts of tetrahydrofuran 300, introducing nitrogen for protection, then adding 0.1-0.14 part of HMTETA, heating to 65-75 ℃, reacting for 24-48h, and finally filtering, washing with alcohol, washing with water and drying to obtain modified nano titanium dioxide;
and fourthly, mixing the modified nano titanium dioxide with water to prepare antistatic finishing liquid with the concentration of 24-28 g/L.
By adopting the technical scheme, the wool fabric is pretreated by S1 to remove the scale layer on the surface of the fiber; after S2 silk fibroin finishing, coating a layer of silk fibroin film on the surface of the fiber; after S3 antistatic finishing, a large amount of modified nano titanium dioxide is attached to the surface of the silk fibroin film; and cleaning by S4 to obtain the final product.
The nanometer titanium dioxide has the advantages of small particle size, large specific surface area, excellent conductivity, no limitation of climate and applicable environment, stable chemical structure and good biocompatibility, the silane group is grafted on the surface after the modification of the KH550 in the first step, the dispersity is greatly improved, the fluorine-containing acrylate is grafted on the surface through the second step and the third step, so that the nanometer titanium dioxide is more easily attached to the silk fibroin film, the adhesive force is strong, the nanometer titanium dioxide is not easy to fall off, and the fabric still has excellent antistatic property after being washed for dozens of times.
The invention is further configured to: the fluorine-containing acrylate monomer is fluorine-containing alkyl methacrylate.
The invention is further configured to: the preparation process of the fluorine-containing acrylate monomer comprises the following steps: firstly, uniformly mixing 20-25 parts of 1,1, 5-trihydroperfluoropentanol, 30-35 parts of methacrylic acid, 10-15 parts of sulfuric acid and 0.5-0.8 part of phenothiazine, heating to 55-65 ℃, reacting for 3-5h, then carrying out reduced pressure distillation after the reaction is finished, washing the obtained fraction with a sodium carbonate solution, finally washing with deionized water, separating an organic layer, drying, and carrying out reduced pressure distillation to obtain the fluorine-containing acrylate monomer.
By adopting the technical scheme, the fluorine-containing acrylate monomer has low surface energy and high yield.
The invention is further configured to: the pretreatment solution comprises 2-4g/L sodium cyanate, 3-5g/L sodium pyrophosphate, 20-30ml/L hydrogen peroxide and 0.2-0.4g/L penetrant JFC.
By adopting the technical scheme, the strong oxidizing property of the aminoperoxyformic acid generated after the reaction of the sodium cyanate and the hydrogen peroxide is utilized to oxidize and corrode the scale layer of the wool fiber, so that the scale layer is damaged, and the subsequent silk fibroin film layer is conveniently formed. Sodium pyrophosphate is used as a stabilizer to inhibit the rapid and ineffective decomposition of hydrogen peroxide, properly reduce the speed of the decomposition to release active oxygen, relieve the damage of wool scale layers and prevent severe damage to wool fibers caused by violent reaction.
The invention is further configured to: the pretreatment liquid also comprises 3-5g/L diethylamine.
By adopting the technical scheme, the wool fibers are acted by diethylamine to generate the amino alanine, and have a certain effect of dissolving out the adhesive substance between the keratinocytes, thereby increasing the adhesive force of the silk fibroin film. Meanwhile, the diethylamine is alkaline, which is beneficial to corrosion damage of the scale layer.
The invention is further configured to: the silk fibroin finishing liquid comprises the following components in parts by weight: 13-18 parts of silk peptide powder, 20-25 parts of cross-linking agent, 2-4 parts of triethanolamine, 5-8 parts of magnesium chloride and 250 parts of water 200-.
By adopting the technical scheme, the silk fibroin finishing liquid is ecological and environment-friendly, wastewater, waste gas and the like cannot be generated in the finishing process, the silk fibroin macromolecular chains are continuously split to generate low-molecular polypeptides, the low-molecular polypeptides easily enter the interior of the fibers and form hydrogen bonds, salt bonds, van der waals force and the like with active groups in the wool fibers, so that a silk fibroin film is formed on the surfaces of the wool fibers. The fibroin is natural high molecular fibrin extracted from silk, has unique molecular structure, good antimicrobial property, moisture absorption property and moisture retention property, and is mainly used as an adsorption film for adsorbing nano titanium dioxide.
The invention is further configured to: the cross-linking agent is genipin.
By adopting the technical scheme, genipin is an excellent natural biological cross-linking agent, can replace glutaraldehyde, and is used for tightly combining silk fibroin and wool fibers.
The invention is further configured to: the silk fibroin finishing liquid also comprises 2-3 parts of cerium nitrate.
By adopting the technical scheme, the silk fibroin film and the cerium ions are coordinated, so that the solubility of the silk fibroin film is reduced, and the washability of the wool fabric is improved.
In conclusion, the invention has the following beneficial effects:
1. the silk fibroin film is attached to the surface of the wool fiber and is used for improving the adhesive force and the adhesive amount of the nano titanium dioxide so as to improve the antistatic property of the wool fabric and is not easy to lose due to repeated washing;
2. the diethylamine is added into the pretreatment liquid, so that the silk fibroin film and the wool fiber are combined more tightly, and the washability of the wool fabric is improved;
3. cerium nitrate is added into the silk fibroin finishing liquid, so that the silk fibroin film is not easy to lose, and the washability of the wool fabric is improved.
Drawings
Fig. 1 is a schematic flow chart of the first to third embodiments.
Detailed Description
The present invention will be described in further detail with reference to the accompanying drawings.
The embodiment of the invention adopts the following raw materials:
silk peptide powder was purchased from xintiansi biotechnology limited, lake.
The nano titanium dioxide is TA18, and is purchased from Shanghai titanium pigment industry Co.
HMTETA, 1,4,7,10, 10-hexamethyltriethylenetetramine, was purchased from Sigma-Aldrich.
1,1, 5-trihydroperfluoropentanol, purchased from tricyclohexyl chemical Co., Ltd, Zhejiang.
The first embodiment is as follows:
an antistatic overcoat finishing process relates to an overcoat woven by wool fabric. As shown in fig. 1, the finishing process of the wool fabric comprises the following steps:
s1 pretreatment: immersing the wool fabric into pretreatment liquid, wherein the bath ratio is 1:25, the temperature is 50 ℃, the treatment is 30min, the wool fabric is taken out after the treatment, the wool fabric is washed by water and dried at 80 ℃ for standby application, and the pretreatment liquid comprises 2g/L sodium cyanate, 3g/L diethylamine, 3g/L sodium pyrophosphate, 20ml/L30wt% hydrogen peroxide, 0.2g/L penetrating agent JFC and water serving as a solvent;
s2 finishing silk fibroin: the wool fabric is pretreated by S1 and then is immersed into the silk fibroin finishing liquid, the bath ratio is 1:20, the two immersion and the two rolling are carried out, the rolling residue rate is 70%, then the pre-drying is carried out for 3min at the temperature of 75 ℃, then the baking is carried out for 60S at the temperature of 140 ℃, finally the water washing is carried out, the drying is carried out at the temperature of 70 ℃ for standby application, and the silk fibroin finishing liquid comprises the following components in parts by weight: 13 parts of silk peptide powder, 20 parts of genipin, 2 parts of triethanolamine, 2 parts of cerium nitrate, 5 parts of magnesium chloride and 200 parts of water;
s3 antistatic finishing: after being finished by silk fibroin S2, the wool fabric is immersed into antistatic finishing liquid, the bath ratio is 1:20, the temperature is 55 ℃, the wool fabric is taken out and then is baked for 90S at 120 ℃, and finally the wool fabric is washed by water and is dried at 70 ℃ for standby application;
s4 cleaning: after antistatic finishing, soaping and washing the wool fabric with water at the temperature of 40 ℃ in sequence by S3, and finally drying.
The preparation process of the antistatic finishing liquid is as follows:
step one, uniformly mixing 10 parts of KH550, 15 parts of deionized water and 30 parts of absolute ethyl alcohol, adding 15 parts of nano titanium dioxide, performing ultrasonic dispersion for 20min, heating to 70 ℃, refluxing for 2h, and finally filtering, washing with ethanol, drying and grinding to obtain a pre-product;
step two, uniformly mixing 6 parts of the pre-product, 10 parts of triethylamine and 150 parts of tetrahydrofuran, introducing nitrogen for protection, dropwise adding a mixed solution of 10 parts of 2-bromoisobutyl acyl bromide and 30 parts of tetrahydrofuran, continuously stirring for 2 hours in an ice bath at 0.5 ℃, standing for 12 hours at 20 ℃, and finally filtering and drying to obtain a secondary product;
step three, uniformly mixing 10 parts of secondary product, 3 parts of copper bromide, 20 parts of fluorine-containing acrylate monomer and 300 parts of tetrahydrofuran, introducing nitrogen for protection, adding 0.1 part of HMTETA, heating to 65 ℃, reacting for 24 hours, and finally filtering, washing with alcohol, washing with water and drying to obtain modified nano titanium dioxide;
and fourthly, mixing the modified nano titanium dioxide with water to prepare antistatic finishing liquid with the concentration of 24 g/L.
The preparation process of the fluorine-containing acrylate monomer comprises the following steps: firstly, uniformly mixing 20 parts of 1,1, 5-trihydroperfluoropentanol, 30 parts of methacrylic acid, 10 parts of sulfuric acid and 0.5 part of phenothiazine, heating to 55 ℃, reacting for 3 hours, then carrying out reduced pressure distillation after the reaction is finished, washing the obtained fraction with a sodium carbonate solution, finally washing the fraction to be neutral with deionized water, separating an organic layer, drying the organic layer with anhydrous sodium sulfate, and then carrying out reduced pressure distillation to obtain the fluorine-containing acrylate monomer.
Example two:
an antistatic overcoat finishing process relates to an overcoat woven by wool fabric. As shown in fig. 1, the finishing process of the wool fabric comprises the following steps:
s1 pretreatment: immersing the wool fabric into pretreatment liquid, wherein the bath ratio is 1:25, the temperature is 60 ℃, the treatment is carried out for 40min, the wool fabric is taken out after the treatment, the wool fabric is washed by water and dried at 80 ℃ for standby application, and the pretreatment liquid comprises 4g/L sodium cyanate, 5g/L diethylamine, 5g/L sodium pyrophosphate, 30ml/L30wt% hydrogen peroxide, 0.4g/L penetrating agent JFC and water as solvent;
s2 finishing silk fibroin: the wool fabric is pretreated by S1 and then is immersed into the silk fibroin finishing liquid, the bath ratio is 1:20, the two immersion and the two rolling are carried out, the rolling residue rate is 70%, then the pre-drying is carried out for 5min at the temperature of 80 ℃, then the baking is carried out for 90S at the temperature of 160 ℃, finally the water washing is carried out, the drying is carried out at the temperature of 70 ℃ for standby application, and the silk fibroin finishing liquid comprises the following components in parts by weight: 18 parts of silk peptide powder, 25 parts of genipin, 4 parts of triethanolamine, 3 parts of cerium nitrate, 8 parts of magnesium chloride and 250 parts of water;
s3 antistatic finishing: after being finished by silk fibroin S2, the wool fabric is immersed into antistatic finishing liquid with the bath ratio of 1:20 and the temperature of 65 ℃, taken out and then baked for 120S at 130 ℃, finally washed by water and dried at 70 ℃ for standby;
s4 cleaning: after antistatic finishing, soaping and washing the wool fabric with water at the water temperature of 50 ℃ in sequence by S3, and finally drying.
The preparation process of the antistatic finishing liquid is as follows:
step one, uniformly mixing 15 parts of KH550, 20 parts of deionized water and 40 parts of absolute ethyl alcohol, adding 20 parts of nano titanium dioxide, performing ultrasonic dispersion for 30min, heating to 80 ℃, refluxing for 3h, and finally filtering, washing with ethanol, drying and grinding to obtain a pre-product;
step two, uniformly mixing 8 parts of the pre-product, 15 parts of triethylamine and 200 parts of tetrahydrofuran, introducing nitrogen for protection, dropwise adding a mixed solution of 15 parts of 2-bromoisobutyl acyl bromide and 40 parts of tetrahydrofuran, placing the mixture in an ice bath at the temperature of 2 ℃, continuously stirring for 3 hours, standing the mixture at the temperature of 25 ℃ for 24 hours, and finally filtering and drying the mixture to obtain a secondary product;
step three, uniformly mixing 15 parts of secondary product, 5 parts of copper bromide, 30 parts of fluorine-containing acrylate monomer and 400 parts of tetrahydrofuran, introducing nitrogen for protection, adding 0.14 part of HMTETA, heating to 75 ℃, reacting for 48 hours, and finally filtering, washing with alcohol, washing with water and drying to obtain modified nano titanium dioxide;
and fourthly, mixing the modified nano titanium dioxide with water to prepare the antistatic finishing liquid with the concentration of 28 g/L.
The preparation process of the fluorine-containing acrylate monomer comprises the following steps: firstly, uniformly mixing 25 parts of 1,1, 5-trihydroperfluoropentanol, 35 parts of methacrylic acid, 15 parts of sulfuric acid and 0.8 part of phenothiazine, heating to 65 ℃, reacting for 5 hours, then carrying out reduced pressure distillation after the reaction is finished, washing the obtained fraction with a sodium carbonate solution, finally washing the fraction to be neutral with deionized water, separating an organic layer, drying the organic layer with anhydrous sodium sulfate, and then carrying out reduced pressure distillation to obtain the fluorine-containing acrylate monomer.
Example three:
an antistatic overcoat finishing process relates to an overcoat woven by wool fabric. As shown in fig. 1, the finishing process of the wool fabric comprises the following steps:
s1 pretreatment: immersing the wool fabric into pretreatment liquid, wherein the bath ratio is 1:25, the temperature is 55 ℃, the wool fabric is treated for 35min, the wool fabric is taken out after the treatment, the wool fabric is washed by water and dried at 80 ℃ for standby application, and the pretreatment liquid comprises 3g/L sodium cyanate, 4g/L diethylamine, 4g/L sodium pyrophosphate, 25ml/L30wt% hydrogen peroxide, 0.3g/L penetrating agent JFC and water as a solvent;
s2 finishing silk fibroin: the wool fabric is pretreated by S1 and then is immersed into the silk fibroin finishing liquid, the bath ratio is 1:20, the two immersion and the two rolling are carried out, the rolling residue rate is 70%, then the wool fabric is pre-dried for 4min at 78 ℃, then the wool fabric is baked for 80S at 150 ℃, finally the wool fabric is washed by water and dried at 70 ℃ for standby application, and the silk fibroin finishing liquid comprises the following components in parts by weight: 15 parts of silk peptide powder, 23 parts of genipin, 3 parts of triethanolamine, 2.5 parts of cerium nitrate, 6 parts of magnesium chloride and 230 parts of water;
s3 antistatic finishing: the method comprises the following steps of (1) finishing the wool fabric with silk fibroin S2, immersing the wool fabric into antistatic finishing liquid at a bath ratio of 1:20 and a temperature of 60 ℃, taking out the wool fabric, baking the wool fabric for 100S at 125 ℃, finally washing the wool fabric with water, and drying the wool fabric for later use at 70 ℃;
s4 cleaning: after antistatic finishing, soaping and washing the wool fabric with water at the water temperature of 45 ℃ in sequence by S3, and finally drying.
The preparation process of the antistatic finishing liquid is as follows:
step one, uniformly mixing 12 parts of KH550, 18 parts of deionized water and 35 parts of absolute ethyl alcohol, adding 18 parts of nano titanium dioxide, performing ultrasonic dispersion for 25min, heating to 75 ℃, refluxing for 2.5h, and finally filtering, washing with ethanol, drying and grinding to obtain a pre-product;
step two, uniformly mixing 7 parts of the pre-product, 12 parts of triethylamine and 180 parts of tetrahydrofuran, introducing nitrogen for protection, dropwise adding a mixed solution of 12 parts of 2-bromoisobutyl acyl bromide and 35 parts of tetrahydrofuran, placing the mixture in an ice bath at the temperature of 1 ℃, continuously stirring for 2.5 hours, standing the mixture at the temperature of 22 ℃ for 18 hours, and finally filtering and drying the mixture to obtain a secondary product;
step three, uniformly mixing 12 parts of secondary product, 4 parts of copper bromide, 25 parts of fluorine-containing acrylate monomer and 350 parts of tetrahydrofuran, introducing nitrogen for protection, adding 0.12 part of HMTETA, heating to 70 ℃, reacting for 36 hours, and finally filtering, washing with alcohol, washing with water and drying to obtain modified nano titanium dioxide;
and fourthly, mixing the modified nano titanium dioxide with water to prepare antistatic finishing liquid with the concentration of 26 g/L.
The preparation process of the fluorine-containing acrylate monomer comprises the following steps: firstly, uniformly mixing 22 parts of 1,1, 5-trihydroperfluoropentanol, 32 parts of methacrylic acid, 12 parts of sulfuric acid and 0.6 part of phenothiazine, heating to 60 ℃, reacting for 4 hours, then carrying out reduced pressure distillation after the reaction is finished, washing the obtained fraction with a sodium carbonate solution, finally washing the fraction with deionized water to be neutral, separating an organic layer, drying with anhydrous sodium sulfate, and carrying out reduced pressure distillation to obtain the fluorine-containing acrylate monomer.
Example four:
the difference from example three is that the silk fibroin finish did not include cerium nitrate.
Example five:
the difference from example three is that the pretreatment solution does not include diethylamine.
Comparative example one:
the difference from the third embodiment is that silk fibroin finishing in step S2 is not included.
Comparative example two:
the difference from the third embodiment is that the nano titanium dioxide in the antistatic finishing liquid is not modified.
And (3) performance testing:
the wool fabrics of the first to fifth examples, the first comparative example and the second comparative example are directly tested for the surface charge density;
second, the wool fabrics of examples one to five, comparative example one and comparative example two were washed with water 30 times, and then the surface charge densities thereof were measured, and the results are reported in table 1.
Table 1 wool fabric performance test result recording table
Charge density without washing with water (μ C/m)2) Charge density after washing with water (μ C/m)2)
Example one 1.6 2.0
Example two 1.6 1.9
EXAMPLE III 1.5 1.8
Example four 1.5 2.4
EXAMPLE five 1.6 2.5
Comparative example 1 3.2 7.4
Comparative example No. two 1.8 4.7
From the data in table 1, one can see:
1. the wool fabric has excellent antistatic property after finishing, and reaches the standard of antistatic clothing;
2. the charge density reduction amplitude of the wool fabric in the fourth embodiment after washing is larger than that of the wool fabric in the first to third embodiments, and thus cerium nitrate has an inhibiting effect on the dissolution loss of the silk fibroin film;
3. after washing, the charge density of the wool fabric of the fourth embodiment is reduced by more than that of the first to third embodiments, and thus, the diethylamine has a promoting effect on the attachment of the silk fibroin film;
4. compared with the wool fabric prepared in the first embodiment, the antistatic performance of the wool fabric prepared in the first embodiment is greatly reduced, and the attachment amount and the attachment force of the silk fibroin film on the nano titanium dioxide are improved;
5. the charge density reduction amplitude of the wool fabric of the comparative example II after washing is larger than that of the wool fabric of the examples I to III, and the bonding tightness of the modified nano titanium dioxide and the silk fibroin film is improved.
The embodiments of the present invention are preferred embodiments of the present invention, and the scope of the present invention is not limited by these embodiments, so: all equivalent changes made according to the structure, shape and principle of the invention are covered by the protection scope of the invention.

Claims (8)

1. An antistatic overcoat finishing process relates to an overcoat woven by wool fabric, and is characterized by comprising the following steps:
s1 pretreatment: immersing the wool fabric into pretreatment liquid at the temperature of 50-60 ℃, treating for 30-40min, taking out after completion, and washing and drying for later use;
s2 finishing silk fibroin: pretreating a wool fabric by S1, immersing the pretreated wool fabric into the silk fibroin finishing liquid, immersing for two times, rolling for two times, pre-drying for 3-5min at 75-80 ℃, then baking for 60-90S at 140-160 ℃, and finally washing and drying for later use;
s3 antistatic finishing: the wool fabric is treated by silk fibroin S2 and then is immersed into antistatic finishing liquid at the temperature of 55-65 ℃, taken out and then is baked for 90-120S at the temperature of 120-130 ℃, and finally is washed and dried for standby;
s4 cleaning: after S3 antistatic finishing, sequentially soaping and washing the wool fabric with water at the temperature of 40-50 ℃, and finally drying;
the preparation process of the antistatic finishing liquid is as follows:
firstly, uniformly mixing 10-15 parts of KH550, 15-20 parts of deionized water and 30-40 parts of absolute ethyl alcohol, adding 15-20 parts of nano titanium dioxide, performing ultrasonic dispersion for 20-30min, heating to 70-80 ℃, refluxing for 2-3h, and finally filtering, washing with ethanol, drying and grinding to obtain a pre-product;
secondly, uniformly mixing 6-8 parts of the pre-product, 10-15 parts of triethylamine and 200 parts of 150-one tetrahydrofuran, introducing nitrogen for protection, dropwise adding a mixed solution of 10-15 parts of 2-bromoisobutyl acyl bromide and 30-40 parts of tetrahydrofuran, continuously stirring for 2-3h in an ice bath at the temperature of 0-2 ℃, standing for 12-24h at the temperature of 20-25 ℃, and finally filtering and drying to obtain a secondary product;
step three, uniformly mixing 10-15 parts of secondary product, 3-5 parts of copper bromide, 20-30 parts of fluorine-containing acrylate monomer and 400 parts of tetrahydrofuran 300, introducing nitrogen for protection, then adding 0.1-0.14 part of HMTETA, heating to 65-75 ℃, reacting for 24-48h, and finally filtering, washing with alcohol, washing with water and drying to obtain modified nano titanium dioxide;
and fourthly, mixing the modified nano titanium dioxide with water to prepare antistatic finishing liquid with the concentration of 24-28 g/L.
2. The antistatic overcoat finishing process of claim 1, which is characterized in that: the fluorine-containing acrylate monomer is fluorine-containing alkyl methacrylate.
3. The antistatic overcoat finishing process of claim 2, which is characterized in that: the preparation process of the fluorine-containing acrylate monomer comprises the following steps: firstly, uniformly mixing 20-25 parts of 1,1, 5-trihydroperfluoropentanol, 30-35 parts of methacrylic acid, 10-15 parts of sulfuric acid and 0.5-0.8 part of phenothiazine, heating to 55-65 ℃, reacting for 3-5h, then carrying out reduced pressure distillation after the reaction is finished, washing the obtained fraction with a sodium carbonate solution, finally washing with deionized water, separating an organic layer, drying, and carrying out reduced pressure distillation to obtain the fluorine-containing acrylate monomer.
4. The antistatic overcoat finishing process of claim 1, which is characterized in that: the pretreatment solution comprises 2-4g/L sodium cyanate, 3-5g/L sodium pyrophosphate, 20-30ml/L hydrogen peroxide and 0.2-0.4g/L penetrant JFC.
5. The antistatic overcoat finishing process of claim 4, wherein: the pretreatment liquid also comprises 3-5g/L diethylamine.
6. The antistatic overcoat finishing process of claim 1, which is characterized in that: the silk fibroin finishing liquid comprises the following components in parts by weight: 13-18 parts of silk peptide powder, 20-25 parts of cross-linking agent, 2-4 parts of triethanolamine, 5-8 parts of magnesium chloride and 250 parts of water 200-.
7. The antistatic overcoat finishing process of claim 6, which is characterized in that: the cross-linking agent is genipin.
8. The antistatic overcoat finishing process of claim 6, which is characterized in that: the silk fibroin finishing liquid also comprises 2-3 parts of cerium nitrate.
CN202010450902.0A 2020-05-25 2020-05-25 Antistatic overcoat finishing process Pending CN111809395A (en)

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Application publication date: 20201023