CN109610160A - A kind of preparation method of silk fabric with excellent hydrophobicity - Google Patents

A kind of preparation method of silk fabric with excellent hydrophobicity Download PDF

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Publication number
CN109610160A
CN109610160A CN201811317781.1A CN201811317781A CN109610160A CN 109610160 A CN109610160 A CN 109610160A CN 201811317781 A CN201811317781 A CN 201811317781A CN 109610160 A CN109610160 A CN 109610160A
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Prior art keywords
silk fabric
preparation
silk
excellent hydrophobicity
fabric
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CN201811317781.1A
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Chinese (zh)
Inventor
杨明英
范鑫
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Zhejiang University ZJU
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Zhejiang University ZJU
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Priority to CN201811317781.1A priority Critical patent/CN109610160A/en
Publication of CN109610160A publication Critical patent/CN109610160A/en
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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
    • D06M11/77—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 silicon or compounds thereof
    • D06M11/79—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 silicon or compounds thereof with silicon dioxide, silicic acids or their salts
    • 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
    • D06M15/643—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing silicon in the main chain
    • 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
    • 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
    • D06M2200/10—Repellency against liquids
    • D06M2200/12—Hydrophobic properties

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

Abstract

The invention belongs to disclose a kind of preparation method of silk fabric with excellent hydrophobic performance, it is cleaned and dried including the uniform silk fabric of cut size stand-by, by hydrophobic titanium dioxide nano silicon particles, dimethyl silicone polymer and curing agent are dissolved in hexane or toluene solution, and ultrasonic vibration forms uniform and stable coating solution, the present invention has energy consumption low in entire treatment process, biological safety is high, it is cheap, it is simple to operate, the advantages such as can be mass-produced, the silk fabric obtained by the invention, there is excellent mechanical stability and chemical resistance simultaneously, silk fabric obtained, with excellent oil and water separation capability and can be recycled, there is certain reference to Crude oil from CNOOC pollution is administered, the silk fabric obtained by the invention can resist dirt well, rainwater and broken Bits pollution, improves the thermal stability of silk fabric itself, enhances ability and ultraviolet resistance, inhibits the growth of bacterium.

Description

A kind of preparation method of the silk fabric with excellent hydrophobic performance
Technical field
The invention belongs to the processing methods of silk fiber, specifically, being related to a kind of silk with excellent hydrophobic performance The preparation method of fabric.
Background technique
China is silk big country since ancient times, and in all main garment materials, silk fiber and fabric are optimum Textile material, because of its graceful appearance, pliability, excellent snugness of fit, warm property, biological degradability, skin friend The advantages that kind property, reproducibility, is widely loved by people.However, possessing hydrophilic radical such as hydroxyl on silk fiber and fabric surface Base, carboxyl and amino make fabric easily by dirt, rainwater and clast pollution.In addition, silk fabric itself has the shortcomings that, such as Thermal stability is low, and ability and ultraviolet resistance is weak, and inflammability is good.These defects significantly limit silk fiber and the reality of fabric is answered With.
Currently, many inorganic coating methods and techniques, such as photoengraving have been developed, and layer-by-layer (LBL) assembling, plasma Body processing and sol-gal process, prepare super hydrophobic surface by forming hydrophobic coating.However, in many cases, by institute The high reaction temperature being related to, the chemical bond adhesive strength between particle and fabric is weak, and mechanical endurance and thermal stability are poor, so It is not particularly suited for silk fabrics.In addition, the uniformity of the conventional coating techniques on silk fiber and fabric surface is usually undesirable, lead Cause the undesirable change of material property, the serious application for limiting product.Solution dipping method is dredged as a kind of simple and quick imparting material The method of aqueous energy, has received widespread attention.Industrial synthesis super-hydrophobic coat method is excessively complicated at present, has certain ring Border pollution, so that the application of hydrophobic product is restricted, developing the quick and easy method for assigning silk fabric ultra-hydrophobicity will It is an importance.
When silk fabric as coated substrate, hexane or toluene as solvent, hydrophobic silica nano particle and poly- Dimethylsilane is mixed to form coating solution, and silk fabric passes through dipping curing process, and it is irregular to show as particle under Electronic Speculum Accumulation has more areolate microstructure, shows to the stronger repulsion ability of water droplet, so as to so that silk fabric have it is excellent Different hydrophobic performance.In addition, both hydrophobic titanium dioxide nano silicon particles and dimethyl silicone polymer different quality proportion are shown as Different appearance forms and structure can control the microcosmic character of product in production by the adjusting of quality proportioning.
Summary of the invention
The present invention is exactly directed to the technical issues of status of the silk fabric vulnerable to water stain pollution, provides a kind of technique letter Single, processing is convenient and can assign the preparation method of silk fabric ultra-hydrophobicity.
To achieve the goals above, the specific technical solution of the present invention is as follows:
The invention discloses a kind of preparation methods of silk fabric with excellent hydrophobic performance, and specific preparation step is such as Under:
1), the uniform silk fabric of cut size is cleaned and dried stand-by；
2) hydrophobic titanium dioxide nano silicon particles, dimethyl silicone polymer and curing agent, are dissolved in hexane or toluene solution In, and ultrasonic vibration forms uniform and stable coating solution；
3) it, will be stood in the dry silk fabric immersion coating solution of cleaning, and take out silk fabrics and be placed in drying in baking oven Solidification finally measures the contact angle size of sample.
As a further improvement, the silk fabric in step 1) of the present invention is the complete removing bought in the market The product of silk gum, silk fabric cleaning include the ultrasonic cleaning process of ethyl alcohol and deionized water.
As a further improvement, hydrophobic titanium dioxide nano silicon particles and poly dimethyl in step 2) of the present invention The quality proportioning of siloxanes is 1:5~5:5, and under different quality proportionings, coating solution is microcosmic silk fabric surface construction Structure is different.
As a further improvement, the ultrasonic vibration time in step 2) of the present invention is 1-1.5h, the time is too short, It is not uniform enough to will lead to the dispersion of hydrophobic titanium dioxide nano silicon particles, is settled in system, influences silk fabric surface texture Formation.
As a further improvement, in step 3) of the present invention in the dry silk fabric immersion coating solution of cleaning The dip time 10-20min of standing, the time is too short, and to will lead to coating solution not uniform enough in the structure of silk fabric surface construction Completely, whole hydrophobic performance is influenced.
As a further improvement, the solidification temperature range in step 3) of the present invention is 80 DEG C~100 DEG C, temperature The excessively high performance that will will affect silk fabric itself, solidification effect of the too low coating solution of temperature on silk fabric surface is not It is good, damage the affinity between coating and silk fabric.
As a further improvement, the dry solidification time in step 3) of the present invention is 6~10h, the time is too short, The combination of coating solution and silk fabric is ineffective, influences whole hydrophobicity；Overlong time, it will increase energy consumption.
As a further improvement, silk fabric coating composite static contact angle obtained by the present invention is greater than 150 °, Slide angle is less than 10 °.
Compared with prior art, the present invention has following prominent characteristics:
(1) present invention has low, the biological safety height that consumes energy, cheap, side easy to operate in entire treatment process Just, the advantages such as can be mass-produced.
(2) there is excellent repulsion performance to aqueous solution by the silk fabric that the invention obtains, static contact angle is greater than 150 °, slide angle can keep for a long time hydrophobic less than 10 °, and in pH=1 hydrochloric acid solution and pH=12 sodium hydroxide solution The stability of performance.
(3) silk fabric obtained by the invention, while there is excellent mechanical stability and chemical resistance.
(4) present invention silk fabric obtained has excellent oil and water separation capability and can be recycled, to controlling Managing Crude oil from CNOOC pollution has certain reference.
(5) silk fabric obtained by the invention can resist dirt, rainwater and clast pollution well.Improve silk The thermal stability of fabric itself enhances ability and ultraviolet resistance, inhibits the growth of bacterium.
Specific embodiment
The present invention is mainly implemented by following scheme:
(1), the uniform silk fabric of cut size is cleaned and dried stand-by；
(2), by hydrophobic titanium dioxide nano silicon particles, dimethyl silicone polymer and curing agent with mass ratio 1:5~5:5 dissolution In 50ml hexane or toluene solution, and 1~1.5h of ultrasonic vibration forms uniform and stable coating solution；
(3), it by 10~20min in the dry silk fabrics immersion coating solution of cleaning, takes out silk fabrics and is placed in 80~100 6~10h of dry solidification in DEG C baking oven, last silk fabric coating composite static contact angle obtained are greater than 150 °, slide angle Less than 10 °.
Technical solution of the present invention is described in further detail below by specific embodiment, following embodiment is pair Explanation of the invention and the invention is not limited to following embodiments.
Embodiment 1
(1) silk fabric for cutting 20mm × 20mm is several, is successively cleaned by ultrasonic 5min with dehydrated alcohol and deionized water, It takes out silk fabric and is placed in 50 DEG C of baking ovens dry 4h, for use.
(2) 0.5g dimethyl silicone polymer is added in 50ml hexane or toluene solution, to be added after evenly mixing 0.05g curing agent, adds 0.1g hydrophobic titanium dioxide nano silicon particles, and ultrasonic vibration 1h forms hydrophobic silica nanometer The uniform and stable coating solution that grain is 1:5 with dimethyl silicone polymer mass ratio.
(3) the dry silk fabric of cleaning is immersed in 15min in coating solution, taking-up is placed in 90 DEG C of baking ovens dry Solidify 6h, obtains modified silk fabric, and carry out contact angle size measurement, obtaining static contact angle is 151 °, and slide angle is 8 °, With excellent hydrophobic performance.
Embodiment 2
(1) silk fabric for cutting 20mm × 20mm is several, is successively cleaned by ultrasonic 5min with dehydrated alcohol and deionized water, It takes out silk fabric and is placed in 50 DEG C of baking ovens dry 4h, for use.
(2) 0.5g dimethyl silicone polymer is added in 50ml hexane or toluene solution, to be added after evenly mixing 0.05g curing agent, adds 0.3g hydrophobic titanium dioxide nano silicon particles, and ultrasonic vibration 1h forms hydrophobic silica nanometer The uniform and stable coating solution of grain and dimethyl silicone polymer mass ratio 3:5.
(3) the dry silk fabric of cleaning is immersed in 15min in layer solution, taking-up is placed in 90 DEG C of baking ovens dry solid Change 6h, obtain modified silk fabric, and carry out contact angle size measurement, obtaining static contact angle is 161 °, and slide angle is 2 °, tool There is excellent hydrophobic performance.
Embodiment 3
(1) silk fabric for cutting 20mm × 20mm is several, is successively cleaned by ultrasonic 5min with dehydrated alcohol and deionized water, It takes out silk fabric and is placed in 50 DEG C of baking ovens dry 4h, for use.
(2) 0.5g dimethyl silicone polymer is added in 50ml hexane or toluene solution, to be added after evenly mixing 0.05g curing agent, adds 0.5g hydrophobic titanium dioxide nano silicon particles, and ultrasonic vibration 1h forms hydrophobic silica nanometer The uniform and stable coating solution of grain and dimethyl silicone polymer mass ratio 5:5.
(3) the dry silk fabric of cleaning is immersed in 15min in coating solution, taking-up is placed in 90 DEG C of baking ovens dry Solidify 6h, obtains modified silk fabric, and carry out contact angle size measurement, obtaining static contact angle is 157 °, and slide angle is 4 °, With excellent hydrophobic performance.
Finally, it should also be noted that it is listed above be only several specific embodiments of the invention.Obviously, of the invention Above embodiments are not limited to, acceptable there are many deformations.Those skilled in the art can be straight from present disclosure All deformations for connecing export or associating, are considered as protection scope of the present invention.

Claims (8)

1.一种具有优异疏水性能的蚕丝织物的制备方法，其特征在于，具体制备步骤如下：1. a preparation method of the silk fabric with excellent hydrophobicity is characterized in that, concrete preparation steps are as follows: 1)、裁剪尺寸均一的蚕丝织物清洗干燥待用；1), the silk fabric of uniform cutting size is cleaned and dried for use; 2)、将疏水二氧化硅纳米颗粒、聚二甲基硅氧烷和固化剂溶解在己烷或甲苯溶液中，并超声震荡形成均匀稳定的涂层溶液；2), dissolving hydrophobic silica nanoparticles, polydimethylsiloxane and curing agent in hexane or toluene solution, and ultrasonically vibrating to form a uniform and stable coating solution; 3)、将清洁干燥的蚕丝织物浸入涂层溶液中静置，取出丝织物并置于烘箱中干燥固化，最后测量样品的接触角大小。3), immerse the clean and dry silk fabric in the coating solution and stand, take out the silk fabric and place it in an oven to dry and solidify, and finally measure the contact angle of the sample. 2.根据权利要求1所述的具有优异疏水性能的蚕丝织物的制备方法，其特征在于，所述的步骤1)中的蚕丝织物为市场上购买的完全脱除丝胶的产品，蚕丝织物清洗包括乙醇和去离子水的超声清洗过程。2. the preparation method of the silk fabric with excellent hydrophobicity according to claim 1, is characterized in that, the silk fabric in the described step 1) is the product that completely removes sericin purchased in the market, and the silk fabric is cleaned Ultrasonic cleaning process including ethanol and deionized water. 3.根据权利要求1所述的具有优异疏水性能的蚕丝织物的制备方法，其特征在于，所述的步骤2)中的疏水二氧化硅纳米颗粒与聚二甲基硅氧烷的质量配比为1:5～5:5。3. the preparation method of the silk fabric with excellent hydrophobicity according to claim 1, is characterized in that, the mass ratio of the hydrophobic silica nanoparticles and polydimethylsiloxane in the described step 2) 1:5 to 5:5. 4.根据权利要求1或2或3所述的具有优异疏水性能的蚕丝织物的制备方法，其特征在于，所述的步骤2)中的超声震荡时间为1-1.5h。4. The preparation method of silk fabric with excellent hydrophobicity according to claim 1, 2 or 3, wherein the ultrasonic oscillation time in the step 2) is 1-1.5h. 5.根据权利要求4所述的具有优异疏水性能的蚕丝织物的制备方法，其特征在于，所述的步骤3)中清洁干燥的蚕丝织物浸入涂层溶液中静置的浸渍时间10-20min。5. The method for preparing a silk fabric with excellent hydrophobicity according to claim 4, wherein the clean and dry silk fabric in the step 3) is immersed in the coating solution for a dipping time of 10-20 min. 6.根据权利要求1或2或3或5所述的具有优异疏水性能的蚕丝织物的制备方法，其特征在于，所述的步骤3)中的固化温度范围为80℃～100℃。6 . The method for preparing silk fabrics with excellent hydrophobic properties according to claim 1 , 2 or 3 or 5 , wherein the curing temperature in the step 3) ranges from 80° C. to 100° C. 7 . 7.根据权利要求6所述的具有优异疏水性能的蚕丝织物的制备方法，其特征在于，所述的步骤3)中的干燥固化时间为6～10h。7 . The method for preparing silk fabric with excellent hydrophobicity according to claim 6 , wherein the drying and curing time in the step 3) is 6-10 h. 8 . 8.根据权利要求1或2或3或5或7所述的具有优异疏水性能的蚕丝织物的制备方法，其特征在于，所制得的蚕丝织物涂层复合物静态接触角大于150°，滑动角小于10°。8. the preparation method of the silk fabric with excellent hydrophobicity according to claim 1 or 2 or 3 or 5 or 7, is characterized in that, the static contact angle of the prepared silk fabric coating compound is greater than 150 °, sliding The angle is less than 10°.
CN201811317781.1A 2018-11-07 2018-11-07 A kind of preparation method of silk fabric with excellent hydrophobicity Pending CN109610160A (en)

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Cited By (4)

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CN111472176A (en) * 2020-04-15 2020-07-31 江南大学 A kind of graphene/polydimethylsiloxane modified cotton fabric method
CN117248373A (en) * 2023-07-29 2023-12-19 哈尔滨工业大学 Preparation method of fabric with both sweat-wicking, heat-proof and oil-stain self-cleaning properties
CN117601516A (en) * 2023-12-05 2024-02-27 吴江德伊时装面料有限公司 A super hydrophobic silk/superfine viscose fabric with high softness
CN119777144A (en) * 2024-12-11 2025-04-08 浙江理工大学 Preparation method of fluorine-free super-hydrophobic, self-cooling synergistic silk fabric

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111472176A (en) * 2020-04-15 2020-07-31 江南大学 A kind of graphene/polydimethylsiloxane modified cotton fabric method
CN117248373A (en) * 2023-07-29 2023-12-19 哈尔滨工业大学 Preparation method of fabric with both sweat-wicking, heat-proof and oil-stain self-cleaning properties
CN117601516A (en) * 2023-12-05 2024-02-27 吴江德伊时装面料有限公司 A super hydrophobic silk/superfine viscose fabric with high softness
CN117601516B (en) * 2023-12-05 2026-03-06 吴江德伊时装面料有限公司 A superhydrophobic silk/ultrafine viscose high-softness fabric
CN119777144A (en) * 2024-12-11 2025-04-08 浙江理工大学 Preparation method of fluorine-free super-hydrophobic, self-cooling synergistic silk fabric

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Application publication date: 20190412