WO2019011278A1 - Method for preparing super-hydrophobic textile - Google Patents

Method for preparing super-hydrophobic textile Download PDF

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Publication number
WO2019011278A1
WO2019011278A1 PCT/CN2018/095291 CN2018095291W WO2019011278A1 WO 2019011278 A1 WO2019011278 A1 WO 2019011278A1 CN 2018095291 W CN2018095291 W CN 2018095291W WO 2019011278 A1 WO2019011278 A1 WO 2019011278A1
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Prior art keywords
superhydrophobic
textile
sio
preparing
sample
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PCT/CN2018/095291
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French (fr)
Chinese (zh)
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黄家伟
林婉婷
张志远
唐昶宇
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黄家伟
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Publication of WO2019011278A1 publication Critical patent/WO2019011278A1/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
    • D06B—TREATING TEXTILE MATERIALS USING LIQUIDS, GASES OR VAPOURS
    • D06B15/00—Removing liquids, gases or vapours from textile materials in association with treatment of the materials by liquids, gases or vapours
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06B—TREATING TEXTILE MATERIALS USING LIQUIDS, GASES OR VAPOURS
    • D06B3/00—Passing of textile materials through liquids, gases or vapours to effect treatment, e.g. washing, dyeing, bleaching, sizing, impregnating
    • D06B3/10—Passing of textile materials through liquids, gases or vapours to effect treatment, e.g. washing, dyeing, bleaching, sizing, impregnating of fabrics
    • 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
    • D06M11/01—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 hydrogen, water or heavy water; with hydrides of metals or complexes thereof; with boranes, diboranes, silanes, disilanes, phosphines, diphosphines, stibines, distibines, arsines, or diarsines or complexes thereof
    • 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
    • D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
    • D06M15/693—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with natural or synthetic rubber, or derivatives thereof
    • 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
    • D06M2101/04—Vegetal fibres
    • D06M2101/06—Vegetal fibres cellulosic
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
    • D06M2101/16—Synthetic fibres, other than mineral fibres
    • D06M2101/18—Synthetic fibres consisting of macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M2101/20—Polyalkenes, polymers or copolymers of compounds with alkenyl groups bonded to aromatic groups
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
    • D06M2101/16—Synthetic fibres, other than mineral fibres
    • D06M2101/30—Synthetic polymers consisting of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M2101/32—Polyesters
    • 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
    • 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
    • D06M2200/35—Abrasion, pilling or fibrillation resistance

Definitions

  • the invention belongs to the technical field of textile water repellent finishing processing, and relates to a method for preparing a superhydrophobic textile fabric by using an ultrathermal hydrogen crosslinking technology.
  • the superhydrophobic surface has a water droplet contact angle (WCA) greater than 150° and has a low rolling contact angle, which makes the superhydrophobic surface resistant to contamination, water and self-cleaning. Utilizing these properties of superhydrophobic surfaces, superhydrophobic technology has been applied to oil and water separation, electronic device protection, and reduction of fluid resistance.
  • WCA water droplet contact angle
  • the textile After the textile has a super-hydrophobic surface, it is expected to have unique properties, while maintaining the ability of the fabric to breathe and permeable, so that it is possible to manufacture a garment that has comfortable functions such as anti-fouling and protection, and is applied to industrial production. , medical and military supplies.
  • CN 101397754B discloses a process for the preparation of a fluorine-free superhydrophobic cotton fabric.
  • the method comprises reacting tetraethoxysilane (TEOS) with reactive activity into an organic solvent of ammonia water (such as ethanol, methanol) to obtain a silica sol, impregnating and attaching to the cotton fabric, and then adding silicon oxide with alkyl group.
  • TEOS tetraethoxysilane
  • ammonia water such as ethanol, methanol
  • CN 1277019C discloses a nano self-cleaning silk and article
  • CN 1824884A discloses a self-cleaning suit fabric and a garment product containing nano functional materials.
  • the organic fluorine material is used, so that the surface of the textile is water-repellent and oil-repellent.
  • the "superheated hydrogen introduction cross-linking" technique employed in the present invention is a green environmentally friendly method for crosslinking organic polymers as described in US 7,998,537.
  • the method utilizes hydrogen molecules having an energy of 10 to 30 eV to bombard the surface of the organic polymer, thereby breaking the carbon-hydrogen bond on the surface of the organic polymer without interrupting the carbon-carbon bond. This will form carbon radicals (C ⁇ ) on the surface of the organic polymer, and the carbon radicals will react to form new crosslinks without causing chain scission of the polymer molecules, thereby forming tens of nanometers thick on the surface of the object.
  • Cross-linking layer The entire process of the above method uses only a small amount of hydrogen, which does not cause harm to the environment and is environmentally friendly.
  • the inventive discovery of the present invention uses a superheated hydrogen introduction cross-linking technique to treat a textile coated with a superhydrophobic coating, which not only crosslinks the surface of the textile fiber, but also significantly increases the modulus and friction resistance of the surface of the textile fiber. Sexuality and water resistance.
  • the superhydrophobic textile fabric of the present invention is prepared by first immersing the textile fabric with a finishing liquid, and then putting the finished textile into an ultra-thermal hydrogen crosslinking device, using a super-hydrogen molecule of 10-20 eV. It is bombarded and crosslinked to obtain a textile having superhydrophobic properties.
  • the finishing liquid contains hydrophobically modified nano-SiO 2 and an organic polymer having a -CH bond which is miscible with the hydrophobically modified nano-SiO 2 .
  • the hydrophobically modified nano-SiO 2 refers to any method of modifying the surface of the water contact angle obtained> 90 ° hydrophobic pair of nano-SiO 2 SiO 2. As long as the finally obtained nano-SiO 2 is hydrophobic, the present invention does not impose any limitation or limitation on any method/chemical that can achieve the hydrophobicity.
  • the present invention may use a silane-modified hydrophobic nano-SiO 2 .
  • the silane-modified hydrophobic nano-SiO 2 has a particle diameter of 3 to 100 nm. More preferably, nano SiO 2 which is hydrophobically modified with methyltrichlorosilane or dimethyldichlorosilane can be used.
  • the organic polymer of the present invention may specifically be polydimethylsiloxane or polybutadiene.
  • the polydimethylsiloxane of the present invention has a number average molecular weight in the range of 5,000 to 200,000, and the polybutadiene has a number average molecular weight in the range of 1,000 to 20,000.
  • the finishing liquid is a finishing liquid in which any organic solvent which can dissolve the organic polymer is used as a solvent.
  • any organic solvent which can dissolve the organic polymer may be n-hexane or ethanol, or a mixture of the two in any ratio.
  • finishing liquid of the present invention contains 0.1 to 3 wt% of hydrophobically modified nano-SiO 2 and 0.1 to 3 wt% of an organic polymer.
  • the mass ratio of the organic polymer to the hydrophobically modified nano SiO 2 is 1:0.4 to 2.5.
  • the preferred preparation method of the finishing liquid of the present invention comprises dissolving an organic polymer in the solvent, adding hydrophobically modified nano-SiO 2 under mechanical stirring, stirring and ultrasonically dispersing, thereby preparing the finishing liquid.
  • the immersion finishing according to the present invention is that the woven fabric is immersed in the finishing liquid for 1 to 60 minutes, taken out and drained, and then baked in an oven at 85 to 105 ° C for 1 to 3 hours.
  • the ultrathermal hydrogen crosslinking device of the present invention is the device described in US 7,998,537, which is also referred to as HHIC device (Hyperthermal Hydrogen Induced Crosslinking).
  • HHIC device Hydrothermal Hydrogen Induced Crosslinking
  • Qiaoyi Technology Co., Ltd. is the sole manufacturer and supplier of HHIC equipment.
  • the invention puts the immersed and finished textile into a superheated hydrogen introduction cross-linking device, and generates an ultra-energy with an energy of 10-20 eV under an acceleration voltage of 10 to 500 V and a vacuum of less than 10 -3 Pa.
  • the hot hydrogen molecules bombard the textile, and the bombardment time is controlled to be 5 to 120 seconds, and the surface is cross-linked to obtain the superhydrophobic textile.
  • the textile may be various commercial textiles.
  • it may be a cotton woven fabric, and may be a woven fabric such as polyester fiber or polypropylene fiber, or a nonwoven fabric such as polyester fiber or polypropylene fiber.
  • the invention adopts various common commercial textile materials, and is subjected to immersion treatment with a simple and inexpensive reagent, and then subjected to superheated hydrogen treatment to obtain a superhydrophobic textile fabric, which has the advantages of environmental protection and simple production.
  • the superhydrophobic textile treated by the method of the present invention has a rolling contact angle significantly reduced, the number of rubbing resistances and the frictional angle of the original superhydrophobic textile fabric are maintained, due to the increase of mechanical strength and adhesion after crosslinking.
  • the number of washable washes has also been significantly improved.
  • the superhydrophobic cotton cloth treated by the method of the invention has a water contact angle of more than 150°, a rolling angle of less than 30°, a rubbing resistance of more than 3,000, a water washing resistance of more than 30, and a good superhydrophobicity and abrasion resistance. Washable.
  • the textile treated by the method of the present invention can maintain the original fabric morphology, texture and structure without change.
  • Fig. 1 is a photograph showing the contact angle of water of a superhydrophobic cotton cloth of Example 1.
  • Figure 2 is a photograph showing the hydrophobic effect of the superhydrophobic cotton cloth of Example 1.
  • Figure 3 is a photograph measuring the water contact angle of the superhydrophobic polyester fiber fabric of Example 11.
  • Figure 4 is a photograph showing the hydrophobic effect of the superhydrophobic polyester fiber fabric of Example 11.
  • the dried sample was placed in a superheated hydrogen introduction crosslinking device, and superheated hydrogen was introduced into the crosslinking treatment at a voltage of 150 V for 40 seconds under a vacuum of 5.0 ⁇ 10 -4 Pa.
  • a superhydrophobic cotton cloth sample was obtained after the treatment.
  • Fig. 1 is a photograph showing the state of the water contact angle measurement process of the superhydrophobic cotton cloth of this embodiment.
  • the photo was taken with a high resolution camera and the WCA was calculated using ImageJ software.
  • the measuring medium is deionized water.
  • Fig. 2 shows the hydrophobic effect when water droplets are dropped on the superhydrophobic cotton cloth of this embodiment.
  • a small amount of yellow food dye is added to the water droplets.
  • the dried sample was placed in a superheated hydrogen introduction crosslinking device, and superheated hydrogen was introduced into the crosslinking treatment at a voltage of 150 V for 20 seconds under a vacuum of 5.0 ⁇ 10 -4 Pa.
  • a superhydrophobic cotton cloth sample was obtained after the treatment.
  • the dried sample was placed in a superheated hydrogen introduction crosslinking device, and superheated hydrogen was introduced into the crosslinking treatment at a voltage of 150 V for 40 seconds under a vacuum of 5.0 ⁇ 10 -4 Pa.
  • a superhydrophobic cotton cloth sample was obtained after the treatment.
  • the dried sample was placed in a superheated hydrogen introduction crosslinking device, and superheated hydrogen was introduced into the crosslinking treatment at a voltage of 150 V for 40 seconds under a vacuum of 5.0 ⁇ 10 -4 Pa.
  • a superhydrophobic cotton cloth sample was obtained after the treatment.
  • the dried sample was placed in a superheated hydrogen introduction crosslinking device, and superheated hydrogen was introduced into the crosslinking treatment at a voltage of 150 V for 40 seconds under a vacuum of 5.0 ⁇ 10 -4 Pa.
  • a superhydrophobic cotton cloth sample was obtained after the treatment.
  • the dried sample was placed in a superheated hydrogen introduction crosslinking device, and superheated hydrogen was introduced into the crosslinking treatment at a voltage of 150 V for 40 seconds under a vacuum of 5.0 ⁇ 10 -4 Pa.
  • a superhydrophobic cotton cloth sample was obtained after the treatment.
  • the dried sample was placed in a superheated hydrogen introduction crosslinking device, and superheated hydrogen was introduced into the crosslinking treatment at a voltage of 150 V for 40 seconds under a vacuum of 5.0 ⁇ 10 -4 Pa.
  • a superhydrophobic cotton cloth sample was obtained after the treatment.
  • the dried sample was placed in a superheated hydrogen introduction crosslinking device, and superheated hydrogen was introduced into the crosslinking treatment at a voltage of 150 V for 40 seconds under a vacuum of 5.0 ⁇ 10 -4 Pa.
  • a superhydrophobic cotton cloth sample was obtained after the treatment.
  • the dried sample was placed in a superheated hydrogen introduction crosslinking device, and superheated hydrogen was introduced into the crosslinking treatment at a voltage of 150 V for 40 seconds under a vacuum of 5.0 ⁇ 10 -4 Pa.
  • a superhydrophobic cotton cloth sample was obtained after the treatment.
  • the dried sample was placed in a superheated hydrogen introduction crosslinking device, and superheated hydrogen was introduced into the crosslinking treatment at a voltage of 150 V for 40 seconds under a vacuum of 5.0 ⁇ 10 -4 Pa.
  • a superhydrophobic cotton cloth sample was obtained after the treatment.
  • the dried sample was placed in a superheated hydrogen introduction crosslinking device, and superheated hydrogen was introduced into the crosslinking treatment at a voltage of 150 V for 40 seconds under a vacuum of 5.0 ⁇ 10 -4 Pa.
  • a superhydrophobic polyester fabric sample was obtained after the treatment.
  • Fig. 3 and Fig. 4 respectively show photographs of water contact angle measurement states and hydrophobic effect pictures of the superhydrophobic polyester fabric of this embodiment.
  • the dried sample was placed in a superheated hydrogen introduction crosslinking device, and superheated hydrogen was introduced into the crosslinking treatment at a voltage of 150 V for 40 seconds under a vacuum of 5.0 ⁇ 10 -4 Pa.
  • a superhydrophobic polyester fabric sample was obtained after the treatment.
  • the dried sample was placed in a superheated hydrogen introduction crosslinking device, and superheated hydrogen was introduced into the crosslinking treatment at a voltage of 150 V for 40 seconds under a vacuum of 5.0 ⁇ 10 -4 Pa.
  • a superhydrophobic polypropylene nonwoven sample was obtained after the treatment.
  • the dried sample was placed in a superheated hydrogen introduction crosslinking device, and superheated hydrogen was introduced into the crosslinking treatment at a voltage of 150 V for 40 seconds under a vacuum of 5.0 ⁇ 10 -4 Pa.
  • a superhydrophobic polypropylene nonwoven sample was obtained after the treatment.
  • the dried sample was placed in a superheated hydrogen introduction crosslinking device, and superheated hydrogen was introduced into the crosslinking treatment at a voltage of 150 V for 40 seconds under a vacuum of 5.0 ⁇ 10 -4 Pa.
  • a superhydrophobic polyester nonwoven sample was obtained after the treatment.
  • the dried sample was placed in a superheated hydrogen introduction crosslinking device, and superheated hydrogen was introduced into the crosslinking treatment at a voltage of 150 V for 40 seconds under a vacuum of 5.0 ⁇ 10 -4 Pa.
  • a superhydrophobic polyester nonwoven sample was obtained after the treatment.
  • the number of rubbing resistance refers to the number of rubbing cycles when the superhydrophobic fabric is rubbed with a friction pressure of 2300 Pa, and the water contact angle of the superhydrophobic fabric is decreased to 90% of its initial value.
  • Washfastness refers to the number of washes when the water contact angle of the superhydrophobic fabric drops to 90% of its initial value.
  • Example 1 165.7 18 5000 50
  • Example 2 160.4 25 5000 50 Comparative Example 1 167.4 85 1000 5
  • Example 3 162.3 30 5000 50
  • Example 4 165.3 20
  • Example 5 165.0 twenty three 4500 50
  • Example 6 166.2 28 4500 30
  • Example 7 158.3 29 4000 30
  • Example 8 155.2 15 3200 30
  • Example 9 165.1 18 4000 30
  • Example 10 160.0 28 3500 30
  • Example 11 152.0 2 6000 50 Comparative Example 2 157.0 16 5000 30
  • Example 12 159.0 4 4000 40
  • Example 13 154.0 12 7000 - Comparative Example 3 153.0 39 2000 -
  • Example 14 150.0 14 5500 -
  • Example 158.0 42 7000 - Comparative Example 4 156.0 27 1000 -
  • Example 161.0 26 5000 -
  • the water contact angles of the fabrics of different materials are all greater than 150°.
  • the rolling angle of the different fabrics and the number of rubbing resistances, which is closely related to the material of the fabric.
  • the rolling angle and the number of rubbing resistances and the number of times of washing resistance after the treatment of the method of the present invention are significantly better than those of the conventional method.

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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

A method for preparing a super-hydrophobic textile, comprising: firstly using finishing liquor containing hydrophobicity-modified nano SiO2 and an organic polymer to perform impregnation and finish on a textile, and then using 10 eV to 20 eV superheated hydrogen molecules to perform bombardment and crosslinking on the resultant, so as to obtain a textile having a super-hydrophobic property. The super-hydrophobic textile prepared by said method has a significantly reduced roll angle while maintaining the water contact angle of the original super-hydrophobic textile; moreover, the textile has significantly improved friction-resistance performance and wash-resistance performance while maintaining the shape, the quality, and the structure of the original textile.

Description

一种超疏水纺织物的制备方法Preparation method of superhydrophobic textile fabric 技术领域Technical field
[0001] 本发明属于纺织品拒水整理加工技术领域，涉及使用超热氢交联技术制备超疏水纺织物的方法。[0001] The invention belongs to the technical field of textile water repellent finishing processing, and relates to a method for preparing a superhydrophobic textile fabric by using an ultrathermal hydrogen crosslinking technology.
背景技术Background technique
超疏水表面的水滴接触角(WCA)大于150°且具有低的滚动接触角，这使得超疏水表面具有防污染、拒水和自清洁的能力。利用超疏水表面的这些性能，超疏水技术已经应用到了油水分离、电子装置保护、降低流体阻力等领域。The superhydrophobic surface has a water droplet contact angle (WCA) greater than 150° and has a low rolling contact angle, which makes the superhydrophobic surface resistant to contamination, water and self-cleaning. Utilizing these properties of superhydrophobic surfaces, superhydrophobic technology has been applied to oil and water separation, electronic device protection, and reduction of fluid resistance.
纺织物具有超疏水表面后，期望也能具有独特的性能，同时又保持织物透气透湿的能力，这样就有可能制成穿着舒适的具有如防污、保护等功能的服装，应用于工业生产、医疗及军用品方面。After the textile has a super-hydrophobic surface, it is expected to have unique properties, while maintaining the ability of the fabric to breathe and permeable, so that it is possible to manufacture a garment that has comfortable functions such as anti-fouling and protection, and is applied to industrial production. , medical and military supplies.
具有超疏水性能纺织物的制备已经在文献中有所报道。如高琴文等(棉织物无氟超疏水整理, 纺织学报, 2009, 30(5).)，刘军等(基于溶胶-凝胶技术的毛/涤织物疏水改性研究, 毛纺科技, 2015, 43(3).)都采用了最常用的溶胶-凝胶法制备超疏水纺织物。The preparation of textiles having superhydrophobic properties has been reported in the literature. Such as Gao Qinwen et al. (Fluorine-free superhydrophobic finishing of cotton fabrics, Journal of Textiles, 2009, 30(5).), Liu Jun et al. (Study on hydrophobic modification of wool/polyester fabrics based on sol-gel technology, Woolen Textile Technology, 2015 , 43(3).) The most commonly used sol-gel method is used to prepare superhydrophobic textiles.
CN 101397754B公开了一种无氟超疏水棉织物的制备方法。该方法将具有反应活性的四乙氧基硅烷(TEOS)加入到氨水的有机溶剂(如乙醇、甲醇)中反应得到二氧化硅溶胶，浸渍附着于棉织物上，再加入带烷基的硅氧烷进行疏水处理，得到超疏水棉织物。CN 101397754B discloses a process for the preparation of a fluorine-free superhydrophobic cotton fabric. The method comprises reacting tetraethoxysilane (TEOS) with reactive activity into an organic solvent of ammonia water (such as ethanol, methanol) to obtain a silica sol, impregnating and attaching to the cotton fabric, and then adding silicon oxide with alkyl group. The alkane is subjected to a hydrophobic treatment to obtain a superhydrophobic cotton fabric.
CN 1277019C公开了一种纳米自清洁真丝绸及制品，CN 1824884A公开了一种含有纳米功能性材料的自清洁西服面料及成衣制品的制法。其在进行疏水处理时，均使用了有机氟材料，使得纺织物的表面拒水又拒油。CN 1277019C discloses a nano self-cleaning silk and article, and CN 1824884A discloses a self-cleaning suit fabric and a garment product containing nano functional materials. When the hydrophobic treatment is carried out, the organic fluorine material is used, so that the surface of the textile is water-repellent and oil-repellent.
目前虽然已经有较多的超疏水织物制备技术报道，但是对超疏水织物的耐摩擦、耐水洗性能却提及较少。这是因为在对织物进行疏水处理时，其表面的粗糙结构易被破坏，导致制备的超疏水织物常常难以有较好的耐摩擦、耐水洗能力。Although there have been many reports on the preparation technology of superhydrophobic fabrics, there are few mentions on the friction and water wash resistance of superhydrophobic fabrics. This is because when the fabric is subjected to hydrophobic treatment, the rough structure of the surface is easily broken, and the prepared superhydrophobic fabric is often difficult to have good friction and water washing resistance.
将超疏水表面进行化学交联，是提高超疏水纺织物耐摩擦和耐水性的一种比较可行的办法。但是，传统的使用交联剂的方法并没有取得多少成功。Chemical cross-linking of superhydrophobic surfaces is a more feasible way to improve the friction and water resistance of superhydrophobic textiles. However, the traditional method of using a crosslinking agent has not achieved much success.
中国科学院上海应用物理研究所辐射化学与辐照技术研究室(Advanced Materials, 2010, 22, 5473-5477.)利用 60Co源发射的射线，将全氟丁基乙基丙烯酸酯接枝交联到普通棉布表面，获得了超疏水棉布，其制备的超疏水棉布在洗涤50次后仍然具有超疏水性。但 60Co源价格昂贵，防辐射装置结构复杂，而且使用的全氟丁基乙基丙烯酸酯单体毒性大，对环境不利。 Institute of Radiation Chemistry and Irradiation Technology, Shanghai Institute of Applied Physics, Chinese Academy of Sciences (Advanced Materials, 2010, 22, 5473-5477.) Grafts cross-linking of perfluorobutylethyl acrylate to radiation emitted from a 60 Co source. On the surface of the ordinary cotton cloth, a superhydrophobic cotton cloth was obtained, and the prepared superhydrophobic cotton cloth was still superhydrophobic after washing for 50 times. However, the 60 Co source is expensive, the structure of the radiation protection device is complicated, and the perfluorobutylethyl acrylate monomer used is highly toxic and unfavorable to the environment.
因此，如何采用绿色环保的技术手段提高超疏水纺织物的耐摩擦和耐水洗性能，解决化学接枝交联带来的环境污染问题，是目前超疏水纺织物领域亟待解决的技术问题。Therefore, how to adopt green environmental protection technology to improve the friction and water wash resistance of superhydrophobic textiles and solve the environmental pollution caused by chemical grafting crosslinks is a technical problem to be solved urgently in the field of superhydrophobic textiles.
技术问题technical problem
[0003] 本发明的目的是提供一种超疏水纺织物的制备方法，该方法通过使用绿色环保的“超热氢引入交联”技术，以增加超疏水纺织物的耐摩擦和耐水洗性能。[0003] It is an object of the present invention to provide a process for the preparation of a superhydrophobic textile fabric which increases the friction and water wash resistance of the superhydrophobic textile by using a green "superheated hydrogen introduction crosslink" technique.
本发明采用的“超热氢引入交联”技术是US 7,998,537所描述的一种绿色环保的使有机聚合物间进行交联的方法。该方法利用具有10～30eV能量的氢分子轰击有机聚合物表面，就能将有机聚合物表面的碳氢键打断，而不会将碳碳键打断。这样会在有机聚合物表面形成碳自由基(C·)，碳自由基之间发生反应形成新的交联键，同时不会造成聚合物分子的断链，从而在物体表面形成几十纳米厚的交联层。上述方法的整个处理过程仅用到少量氢气，对环境不造成危害，绿色环保。The "superheated hydrogen introduction cross-linking" technique employed in the present invention is a green environmentally friendly method for crosslinking organic polymers as described in US 7,998,537. The method utilizes hydrogen molecules having an energy of 10 to 30 eV to bombard the surface of the organic polymer, thereby breaking the carbon-hydrogen bond on the surface of the organic polymer without interrupting the carbon-carbon bond. This will form carbon radicals (C·) on the surface of the organic polymer, and the carbon radicals will react to form new crosslinks without causing chain scission of the polymer molecules, thereby forming tens of nanometers thick on the surface of the object. Cross-linking layer. The entire process of the above method uses only a small amount of hydrogen, which does not cause harm to the environment and is environmentally friendly.
本发明创造性的发现，使用超热氢引入交联技术处理涂饰了超疏水涂层的纺织物，不仅可以使纺织物纤维表面得到交联，而且可以显著增加纺织物纤维表面的模量、耐摩擦性以及耐水性。The inventive discovery of the present invention uses a superheated hydrogen introduction cross-linking technique to treat a textile coated with a superhydrophobic coating, which not only crosslinks the surface of the textile fiber, but also significantly increases the modulus and friction resistance of the surface of the textile fiber. Sexuality and water resistance.
技术解决方案Technical solution
本发明所述的超疏水纺织物的制备方法是先使用整理液对纺织物进行浸渍整理，再将整理后的纺织物放入超热氢交联装置中，采用10～20eV的超热氢分子对其进行轰击交联，以得到具有超疏水特性的纺织物。其中，在所述的整理液中含有疏水改性纳米SiO 2，以及能够与所述疏水改性纳米SiO 2混溶的、具有-CH键的有机聚合物。 The superhydrophobic textile fabric of the present invention is prepared by first immersing the textile fabric with a finishing liquid, and then putting the finished textile into an ultra-thermal hydrogen crosslinking device, using a super-hydrogen molecule of 10-20 eV. It is bombarded and crosslinked to obtain a textile having superhydrophobic properties. Wherein, the finishing liquid contains hydrophobically modified nano-SiO 2 and an organic polymer having a -CH bond which is miscible with the hydrophobically modified nano-SiO 2 .
本发明中，所述的疏水改性纳米SiO 2是指以任何方法对SiO 2进行表面改性得到的水接触角>90°的疏水性纳米SiO 2。只要最终得到的纳米SiO 2是疏水性的，本发明对任何可以实现该疏水性的方法/化学品不施加任何限定或限制。 In the present invention, the hydrophobically modified nano-SiO 2 refers to any method of modifying the surface of the water contact angle obtained> 90 ° hydrophobic pair of nano-SiO 2 SiO 2. As long as the finally obtained nano-SiO 2 is hydrophobic, the present invention does not impose any limitation or limitation on any method/chemical that can achieve the hydrophobicity.
优选地，本发明可以使用经硅烷改性的疏水性纳米SiO 2。所述硅烷改性的疏水性纳米SiO 2具有3～100nm的粒径。更优选地，可以使用经甲基三氯硅烷或二甲基二氯硅烷进行疏水改性的纳米SiO 2。 Preferably, the present invention may use a silane-modified hydrophobic nano-SiO 2 . The silane-modified hydrophobic nano-SiO 2 has a particle diameter of 3 to 100 nm. More preferably, nano SiO 2 which is hydrophobically modified with methyltrichlorosilane or dimethyldichlorosilane can be used.
例如，可以使用市售的成都今天化工生产的JT-SQ气相法疏水白炭黑，或者德国产的Aerosil ® R974气相二氧化硅等。 For example, a commercially available chemical produced today Chengdu JT-SQ hydrophobic fumed silica, produced in Germany or Aerosil ® R974 fumed silica.
优选地，本发明所述的有机聚合物具体可以是聚二甲基硅氧烷或聚顺丁二烯。Preferably, the organic polymer of the present invention may specifically be polydimethylsiloxane or polybutadiene.
更具体地，本发明所述聚二甲基硅氧烷的数均分子量范围在5000～200000，聚顺丁二烯的数均分子量范围为1000～20000。More specifically, the polydimethylsiloxane of the present invention has a number average molecular weight in the range of 5,000 to 200,000, and the polybutadiene has a number average molecular weight in the range of 1,000 to 20,000.
本发明中，所述的整理液是以可以溶解所述有机聚合物的任何有机溶剂为溶媒的整理液。其中，可以溶解所述有机聚合物的任何有机溶剂可以是正己烷或乙醇，或者是两者的任意比例混合物。In the present invention, the finishing liquid is a finishing liquid in which any organic solvent which can dissolve the organic polymer is used as a solvent. Among them, any organic solvent which can dissolve the organic polymer may be n-hexane or ethanol, or a mixture of the two in any ratio.
进一步地，本发明所述整理液中含有0.1～3wt%疏水改性的纳米SiO 2，以及0.1～3wt%有机聚合物。 Further, the finishing liquid of the present invention contains 0.1 to 3 wt% of hydrophobically modified nano-SiO 2 and 0.1 to 3 wt% of an organic polymer.
更进一步地，在所述整理液中，有机聚合物与疏水改性纳米SiO 2的质量比为1∶0.4～2.5。 Further, in the finishing liquid, the mass ratio of the organic polymer to the hydrophobically modified nano SiO 2 is 1:0.4 to 2.5.
本发明所述整理液的优选配制方法是将有机聚合物溶解在所述溶媒中，机械搅拌下加入疏水改性纳米SiO 2，搅拌并超声分散，从而制备得到所述的整理液。 The preferred preparation method of the finishing liquid of the present invention comprises dissolving an organic polymer in the solvent, adding hydrophobically modified nano-SiO 2 under mechanical stirring, stirring and ultrasonically dispersing, thereby preparing the finishing liquid.
具体地，本发明所述的浸渍整理是将纺织物浸入所述整理液中浸泡1～60分钟，取出沥干后，于85～105℃烘箱中烘1～3小时。Specifically, the immersion finishing according to the present invention is that the woven fabric is immersed in the finishing liquid for 1 to 60 minutes, taken out and drained, and then baked in an oven at 85 to 105 ° C for 1 to 3 hours.
本发明所述的超热氢交联设备为US 7,998,537中所描述的设备，该设备也被称为HHIC设备(Hyperthermal Hydrogen Induced Crosslinking的英文简写)。目前，巧鸾科技有限公司是HHIC设备的唯一制造商和供应商。关于该超热氢交联设备的更详细说明，可以参阅http://hlst.com.hk/a/H_luxe_100/34.html内容。The ultrathermal hydrogen crosslinking device of the present invention is the device described in US 7,998,537, which is also referred to as HHIC device (Hyperthermal Hydrogen Induced Crosslinking). At present, Qiaoyi Technology Co., Ltd. is the sole manufacturer and supplier of HHIC equipment. For a more detailed description of the superheated hydrogen cross-linking device, please refer to http://hlst.com.hk/a/H_luxe_100/34.html.
本发明将所述浸渍整理后的纺织物放入超热氢引入交联设备中，在加速电压10～500 V、真空度低于10 -3Pa条件下，产生具有能量为10～20eV的超热氢分子对纺织物进行轰击，控制轰击时间为5～120秒，使其表面交联后得到所述的超疏水纺织物。 The invention puts the immersed and finished textile into a superheated hydrogen introduction cross-linking device, and generates an ultra-energy with an energy of 10-20 eV under an acceleration voltage of 10 to 500 V and a vacuum of less than 10 -3 Pa. The hot hydrogen molecules bombard the textile, and the bombardment time is controlled to be 5 to 120 seconds, and the surface is cross-linked to obtain the superhydrophobic textile.
本发明中，所述的纺织物可以是各种商品纺织物。例如，可以是棉织布，可以是聚酯纤维、聚丙烯纤维等的纺织布，也可以是聚酯纤维、聚丙烯纤维等的无纺布。In the present invention, the textile may be various commercial textiles. For example, it may be a cotton woven fabric, and may be a woven fabric such as polyester fiber or polypropylene fiber, or a nonwoven fabric such as polyester fiber or polypropylene fiber.
有益效果Beneficial effect
本发明采用各种普通的商品纺织物，以简单价廉的试剂进行浸渍处理后，再进行超热氢处理，即可得到超疏水纺织物，具有环保、生产简便的优点。The invention adopts various common commercial textile materials, and is subjected to immersion treatment with a simple and inexpensive reagent, and then subjected to superheated hydrogen treatment to obtain a superhydrophobic textile fabric, which has the advantages of environmental protection and simple production.
采用本发明方法处理后的超疏水纺织物由于机械强度以及交联后粘附性的增加，在保持了原有超疏水纺织物水接触角的基础上，滚动角显著减小，耐摩擦次数和耐水洗次数也得到了显著提升。例如，以本发明方法处理得到的超疏水棉布的水接触角大于150°，滚动角小于30°，耐摩擦次数大于3000，耐水洗次数大于30，具备了良好的超疏水性、耐摩擦性和耐水洗性。The superhydrophobic textile treated by the method of the present invention has a rolling contact angle significantly reduced, the number of rubbing resistances and the frictional angle of the original superhydrophobic textile fabric are maintained, due to the increase of mechanical strength and adhesion after crosslinking. The number of washable washes has also been significantly improved. For example, the superhydrophobic cotton cloth treated by the method of the invention has a water contact angle of more than 150°, a rolling angle of less than 30°, a rubbing resistance of more than 3,000, a water washing resistance of more than 30, and a good superhydrophobicity and abrasion resistance. Washable.
同时，经本发明方法处理后的纺织物还可以保持原有的织物形态、质地和结构不发生变化。At the same time, the textile treated by the method of the present invention can maintain the original fabric morphology, texture and structure without change.
附图说明DRAWINGS
图1是测量实施例1超疏水棉布水接触角的照片。BRIEF DESCRIPTION OF THE DRAWINGS Fig. 1 is a photograph showing the contact angle of water of a superhydrophobic cotton cloth of Example 1.
图2是实施例1超疏水棉布的疏水性效果照片。Figure 2 is a photograph showing the hydrophobic effect of the superhydrophobic cotton cloth of Example 1.
图3是测量实施例11超疏水聚酯纤维织物水接触角的照片。Figure 3 is a photograph measuring the water contact angle of the superhydrophobic polyester fiber fabric of Example 11.
图4是实施例11超疏水聚酯纤维织物的疏水性效果照片。Figure 4 is a photograph showing the hydrophobic effect of the superhydrophobic polyester fiber fabric of Example 11.
本发明的实施方式Embodiments of the invention
采用以下实施例，进一步详细描述本发明。这些实施例仅用于说明本发明而不用于限制本发明的发明范围。此外，本领域技术人员可以对本发明作出各种改动，这些等价形式同样属于本发明申请的权利要求书所要求的范围。The invention is further described in detail using the following examples. These examples are for illustrative purposes only and are not intended to limit the scope of the invention. In addition, various modifications of the invention may be made by those skilled in the art, and such equivalents are also within the scope of the appended claims.
实施例1。Example 1.
将普通棉布裁剪成10cm 2大小的试样，室温下浸入含有2% JT-SQ纳米SiO 2(5nm)，1%聚二甲基硅氧烷(Mn=15000)的正己烷溶液中。浸泡5分钟后取出试样，挤干，放入90℃烘箱中烘90分钟。 A plain cotton cloth was cut into a sample of 10 cm 2 size, and immersed in a n-hexane solution containing 2% JT-SQ nano-SiO 2 (5 nm) and 1% polydimethylsiloxane (Mn = 15000) at room temperature. After soaking for 5 minutes, the sample was taken out, squeezed, and baked in a 90 ° C oven for 90 minutes.
再将烘干的试样放入超热氢引入交联设备中，在真空度5.0×10 -4Pa条件下，以电压150V进行超热氢引入交联处理40秒。处理完后得到超疏水棉布样品。 The dried sample was placed in a superheated hydrogen introduction crosslinking device, and superheated hydrogen was introduced into the crosslinking treatment at a voltage of 150 V for 40 seconds under a vacuum of 5.0×10 -4 Pa. A superhydrophobic cotton cloth sample was obtained after the treatment.
图1给出了本实施例超疏水棉布水接触角测量过程的状态照片。该照片采用高分辨率摄像机进行，并使用ImageJ软件计算WCA。测量介质为去离子水。Fig. 1 is a photograph showing the state of the water contact angle measurement process of the superhydrophobic cotton cloth of this embodiment. The photo was taken with a high resolution camera and the WCA was calculated using ImageJ software. The measuring medium is deionized water.
图2则展示了本实施例超疏水棉布上滴有水滴时的疏水效果。为了获得更好的颜色对比度，以清晰地展现出疏水性能，在水滴中加入了少量的黄色食用染料。Fig. 2 shows the hydrophobic effect when water droplets are dropped on the superhydrophobic cotton cloth of this embodiment. In order to obtain a better color contrast to clearly show the hydrophobic properties, a small amount of yellow food dye is added to the water droplets.
实施例2。Example 2.
将10cm 2的普通棉布试样在室温下浸入含有2% JT-SQ纳米SiO 2(5nm)，1%聚二甲基硅氧烷(Mn=50000)的正己烷溶液中。浸泡5分钟后取出试样，挤干，放入90℃烘箱中烘90分钟。 A 10 cm 2 sample of plain cotton cloth was immersed in a solution of 2% JT-SQ nano-SiO 2 (5 nm), 1% polydimethylsiloxane (Mn = 50,000) in n-hexane at room temperature. After soaking for 5 minutes, the sample was taken out, squeezed, and baked in a 90 ° C oven for 90 minutes.
再将烘干的试样放入超热氢引入交联设备中，在真空度5.0×10 -4Pa条件下，以电压150V进行超热氢引入交联处理20秒。处理完后得到超疏水棉布样品。 Then, the dried sample was placed in a superheated hydrogen introduction crosslinking device, and superheated hydrogen was introduced into the crosslinking treatment at a voltage of 150 V for 20 seconds under a vacuum of 5.0×10 -4 Pa. A superhydrophobic cotton cloth sample was obtained after the treatment.
对照例1。Comparative Example 1.
将10cm 2的普通棉布试样在室温下浸入含有2% JT-SQ纳米SiO 2(5nm)，1%聚二甲基硅氧烷(Mn=50000)的正己烷溶液中。浸泡5分钟后取出试样，挤干，放入90℃烘箱中烘90分钟，不进行超热氢轰击处理，得到超疏水棉布样品。 A 10 cm 2 sample of plain cotton cloth was immersed in a solution of 2% JT-SQ nano-SiO 2 (5 nm), 1% polydimethylsiloxane (Mn = 50,000) in n-hexane at room temperature. After soaking for 5 minutes, the sample was taken out, squeezed, and baked in an oven at 90 ° C for 90 minutes without superheated hydrogen bombardment treatment to obtain a superhydrophobic cotton cloth sample.
实施例3。Example 3.
将10cm 2的普通棉布试样在室温下浸入含有1% JT-SQ纳米SiO 2(5nm)，0.5%聚二甲基硅氧烷(Mn=50000)的正己烷溶液中。浸泡5分钟后取出试样，挤干，放入100℃烘箱中烘60分钟。 A 10 cm 2 sample of plain cotton cloth was immersed in a solution of 1% JT-SQ nano-SiO 2 (5 nm), 0.5% polydimethylsiloxane (Mn = 50,000) in n-hexane at room temperature. After soaking for 5 minutes, the sample was taken out, squeezed, and baked in a 100 ° C oven for 60 minutes.
再将烘干的试样放入超热氢引入交联设备中，在真空度5.0×10 -4Pa条件下，以电压150V进行超热氢引入交联处理40秒。处理完后得到超疏水棉布样品。 The dried sample was placed in a superheated hydrogen introduction crosslinking device, and superheated hydrogen was introduced into the crosslinking treatment at a voltage of 150 V for 40 seconds under a vacuum of 5.0×10 -4 Pa. A superhydrophobic cotton cloth sample was obtained after the treatment.
实施例4。Example 4.
将10cm 2的普通棉布试样在室温下浸入含有2% JT-SQ纳米SiO 2(5nm)，1%聚顺丁二烯(Mn=5000)的正己烷溶液中。浸泡5分钟后，取出试样，挤干，放入90℃烘箱中烘100分钟。 A 10 cm 2 plain cotton sample was immersed in a solution of 2% JT-SQ nano-SiO 2 (5 nm), 1% polybutadiene (Mn = 5000) in n-hexane at room temperature. After soaking for 5 minutes, the sample was taken out, squeezed out, and baked in a 90 ° C oven for 100 minutes.
再将烘干的试样放入超热氢引入交联设备中，在真空度5.0×10 -4Pa条件下，以电压150V进行超热氢引入交联处理40秒。处理完后得到超疏水棉布样品。 The dried sample was placed in a superheated hydrogen introduction crosslinking device, and superheated hydrogen was introduced into the crosslinking treatment at a voltage of 150 V for 40 seconds under a vacuum of 5.0×10 -4 Pa. A superhydrophobic cotton cloth sample was obtained after the treatment.
实施例5。Example 5.
将10cm 2的普通棉布试样在室温下浸入含有2% JT-SQ纳米SiO 2(15nm)，1%聚顺丁二烯(Mn=5000)的正己烷溶液中。浸泡5分钟后取出试样，挤干，放入100℃烘箱中烘90分钟。 A 10 cm 2 sample of plain cotton cloth was immersed in a solution of 2% JT-SQ nano-SiO 2 (15 nm), 1% polybutadiene (Mn = 5000) in n-hexane at room temperature. After soaking for 5 minutes, the sample was taken out, squeezed, and baked in a 100 ° C oven for 90 minutes.
再将烘干的试样放入超热氢引入交联设备中，在真空度5.0×10 -4Pa条件下，以电压150V进行超热氢引入交联处理40秒。处理完后得到超疏水棉布样品。 The dried sample was placed in a superheated hydrogen introduction crosslinking device, and superheated hydrogen was introduced into the crosslinking treatment at a voltage of 150 V for 40 seconds under a vacuum of 5.0×10 -4 Pa. A superhydrophobic cotton cloth sample was obtained after the treatment.
实施例6。Example 6.
将10cm 2的普通棉布试样在室温下浸入含有2% JT-SQ纳米SiO 2(15nm)，1%聚顺丁二烯(Mn=5000)的正己烷溶液中。浸泡5分钟后取出试样，挤干，放入100℃烘箱中烘60分钟。 A 10 cm 2 sample of plain cotton cloth was immersed in a solution of 2% JT-SQ nano-SiO 2 (15 nm), 1% polybutadiene (Mn = 5000) in n-hexane at room temperature. After soaking for 5 minutes, the sample was taken out, squeezed, and baked in a 100 ° C oven for 60 minutes.
再将烘干的试样放入超热氢引入交联设备中，在真空度5.0×10 -4Pa条件下，以电压150V进行超热氢引入交联处理40秒。处理完后得到超疏水棉布样品。 The dried sample was placed in a superheated hydrogen introduction crosslinking device, and superheated hydrogen was introduced into the crosslinking treatment at a voltage of 150 V for 40 seconds under a vacuum of 5.0×10 -4 Pa. A superhydrophobic cotton cloth sample was obtained after the treatment.
实施例7。Example 7.
将10cm 2的普通棉布试样在室温下浸入含有2% JT-SQ纳米SiO 2(15nm)，1%聚顺丁二烯(Mn=5000)的正己烷溶液中。浸泡25分钟后取出试样，挤干，放入100℃烘箱中烘60分钟。 A 10 cm 2 sample of plain cotton cloth was immersed in a solution of 2% JT-SQ nano-SiO 2 (15 nm), 1% polybutadiene (Mn = 5000) in n-hexane at room temperature. After soaking for 25 minutes, the sample was taken out, squeezed, and baked in a 100 ° C oven for 60 minutes.
再将烘干的试样放入超热氢引入交联设备中，在真空度5.0×10 -4Pa条件下，以电压150V进行超热氢引入交联处理40秒。处理完后得到超疏水棉布样品。 The dried sample was placed in a superheated hydrogen introduction crosslinking device, and superheated hydrogen was introduced into the crosslinking treatment at a voltage of 150 V for 40 seconds under a vacuum of 5.0×10 -4 Pa. A superhydrophobic cotton cloth sample was obtained after the treatment.
实施例8。Example 8.
将10cm 2的普通棉布试样在室温下浸入含有2% Aerosil ® R974纳米SiO 2(15nm)，1%聚顺丁二烯(Mn=5000)的正己烷溶液中。浸泡25分钟后取出试样，挤干，放入100℃烘箱中烘60分钟。 A 10 cm 2 sample of plain cotton cloth was immersed in a solution of 2% Aerosil ® R974 nm SiO 2 (15 nm) in 1% polybutadiene (Mn = 5000) in n-hexane at room temperature. After soaking for 25 minutes, the sample was taken out, squeezed, and baked in a 100 ° C oven for 60 minutes.
再将烘干的试样放入超热氢引入交联设备中，在真空度5.0×10 -4Pa条件下，以电压150V进行超热氢引入交联处理40秒。处理完后得到超疏水棉布样品。 The dried sample was placed in a superheated hydrogen introduction crosslinking device, and superheated hydrogen was introduced into the crosslinking treatment at a voltage of 150 V for 40 seconds under a vacuum of 5.0×10 -4 Pa. A superhydrophobic cotton cloth sample was obtained after the treatment.
实施例9。Example 9.
将10cm 2的普通棉布试样在室温下浸入含有0.5% JT-SQ纳米SiO 2(15nm)，1%聚顺丁二烯(Mn=5000)的正己烷溶液中。浸泡25分钟后取出试样，挤干，放入100℃烘箱中烘60分钟。 A 10 cm 2 plain cotton cloth sample was immersed in a n-hexane solution containing 0.5% JT-SQ nano-SiO 2 (15 nm), 1% poly-butadiene (Mn = 5000) at room temperature. After soaking for 25 minutes, the sample was taken out, squeezed, and baked in a 100 ° C oven for 60 minutes.
再将烘干的试样放入超热氢引入交联设备中，在真空度5.0×10 -4Pa条件下，以电压150V进行超热氢引入交联处理40秒。处理完后得到超疏水棉布样品。 The dried sample was placed in a superheated hydrogen introduction crosslinking device, and superheated hydrogen was introduced into the crosslinking treatment at a voltage of 150 V for 40 seconds under a vacuum of 5.0×10 -4 Pa. A superhydrophobic cotton cloth sample was obtained after the treatment.
实施例10。Example 10.
将10cm 2的普通棉布试样在室温下浸入含有0.2% JT-SQ纳米SiO 2(15nm)，0.1%聚顺丁二烯(Mn=5000)的正己烷溶液中。浸泡25分钟后取出试样，挤干，放入60℃烘箱中烘60分钟。 A 10 cm 2 sample of plain cotton cloth was immersed in a solution of 0.2% JT-SQ nano-SiO 2 (15 nm), 0.1% polybutadiene (Mn = 5000) in n-hexane at room temperature. After soaking for 25 minutes, the sample was taken out, squeezed, and baked in a 60 ° C oven for 60 minutes.
再将烘干的试样放入超热氢引入交联设备中，在真空度5.0×10 -4Pa条件下，以电压150V进行超热氢引入交联处理40秒。处理完后得到超疏水棉布样品。 The dried sample was placed in a superheated hydrogen introduction crosslinking device, and superheated hydrogen was introduced into the crosslinking treatment at a voltage of 150 V for 40 seconds under a vacuum of 5.0×10 -4 Pa. A superhydrophobic cotton cloth sample was obtained after the treatment.
实施例11。Example 11.
将普通聚酯纤维布(100%)裁剪成10cm 2大小的试样，室温下浸入由正己烷与乙醇按照1∶1的质量比组成的混合溶液中，该混合溶液中含有1% JT-SQ纳米SiO 2(15nm)和2%聚二甲基硅氧烷(Mn=15000)。浸泡25分钟后，取出试样，挤干，放入100℃烘箱中烘60分钟。 The ordinary polyester fiber cloth (100%) was cut into a sample of 10 cm 2 size, and immersed in a mixed solution composed of n-hexane and ethanol in a mass ratio of 1:1 at room temperature, and the mixed solution contained 1% JT-SQ. Nano SiO 2 (15 nm) and 2% polydimethylsiloxane (Mn = 15000). After soaking for 25 minutes, the sample was taken out, squeezed, and baked in a 100 ° C oven for 60 minutes.
再将烘干的试样放入超热氢引入交联设备中，在真空度5.0×10 -4Pa条件下，以电压150V进行超热氢引入交联处理40秒。处理完后得到超疏水聚酯织物样品。 The dried sample was placed in a superheated hydrogen introduction crosslinking device, and superheated hydrogen was introduced into the crosslinking treatment at a voltage of 150 V for 40 seconds under a vacuum of 5.0×10 -4 Pa. A superhydrophobic polyester fabric sample was obtained after the treatment.
图3和图4分别给出了本实施例超疏水聚酯织物的水接触角测量状态照片和疏水效果图片。Fig. 3 and Fig. 4 respectively show photographs of water contact angle measurement states and hydrophobic effect pictures of the superhydrophobic polyester fabric of this embodiment.
对照例2。Comparative Example 2.
将普通聚酯纤维布(100%)裁剪成10cm 2大小的试样，室温下浸入由正己烷与乙醇按照1∶1的质量比组成的混合溶液中，该混合溶液中含有1% JT-SQ纳米SiO 2(15nm)和2%聚二甲基硅氧烷(Mn=15000)。浸泡25分钟后，取出试样，挤干，放入100℃烘箱中烘60分钟。 The ordinary polyester fiber cloth (100%) was cut into a sample of 10 cm 2 size, and immersed in a mixed solution composed of n-hexane and ethanol in a mass ratio of 1:1 at room temperature, and the mixed solution contained 1% JT-SQ. Nano SiO 2 (15 nm) and 2% polydimethylsiloxane (Mn = 15000). After soaking for 25 minutes, the sample was taken out, squeezed, and baked in a 100 ° C oven for 60 minutes.
实施例12。Example 12.
将10cm 2的聚酯纤维布(100%)试样在室温下浸入由正己烷与乙醇按照1∶1的质量比组成的混合溶液中，该混合溶液中含有2% JT-SQ纳米SiO 2(15nm)和2%聚二甲基硅氧烷(Mn=15000)。浸泡25分钟后，取出试样，挤干，放入100℃烘箱中烘60分钟。 A 10 cm 2 sample of polyester fiber cloth (100%) was immersed in a mixed solution of n-hexane and ethanol in a mass ratio of 1:1 at room temperature, and the mixed solution contained 2% of JT-SQ nano-SiO 2 ( 15 nm) and 2% polydimethylsiloxane (Mn = 15,000). After soaking for 25 minutes, the sample was taken out, squeezed, and baked in a 100 ° C oven for 60 minutes.
再将烘干的试样放入超热氢引入交联设备中，在真空度5.0×10 -4Pa条件下，以电压150V进行超热氢引入交联处理40秒。处理完后得到超疏水聚酯织物样品。 The dried sample was placed in a superheated hydrogen introduction crosslinking device, and superheated hydrogen was introduced into the crosslinking treatment at a voltage of 150 V for 40 seconds under a vacuum of 5.0×10 -4 Pa. A superhydrophobic polyester fabric sample was obtained after the treatment.
实施例13。Example 13.
将10cm 2的聚丙烯纤维无纺布(100%)试样在室温下浸入由正己烷与乙醇按照1∶1的质量比组成的混合溶液中，该混合溶液中含有1% JT-SQ纳米SiO 2(15nm)和2%聚二甲基硅氧烷(Mn=15000)。浸泡25分钟后，取出试样，挤干，放入100℃烘箱中烘60分钟。 A 10 cm 2 polypropylene fiber nonwoven fabric (100%) sample was immersed in a mixed solution of n-hexane and ethanol in a mass ratio of 1:1 at room temperature, and the mixed solution contained 1% of JT-SQ nano-SiO. 2 (15 nm) and 2% polydimethylsiloxane (Mn = 15,000). After soaking for 25 minutes, the sample was taken out, squeezed, and baked in a 100 ° C oven for 60 minutes.
再将烘干的试样放入超热氢引入交联设备中，在真空度5.0×10 -4Pa条件下，以电压150V进行超热氢引入交联处理40秒。处理完后得到超疏水聚丙烯无纺布样品。 The dried sample was placed in a superheated hydrogen introduction crosslinking device, and superheated hydrogen was introduced into the crosslinking treatment at a voltage of 150 V for 40 seconds under a vacuum of 5.0×10 -4 Pa. A superhydrophobic polypropylene nonwoven sample was obtained after the treatment.
对照例3。Comparative Example 3.
将10cm 2的聚丙烯纤维无纺布(100%)试样在室温下浸入由正己烷与乙醇按照1∶1的质量比组成的混合溶液中，该混合溶液中含有1% JT-SQ纳米SiO 2(15nm)和2%聚二甲基硅氧烷(Mn=15000)。浸泡25分钟后，取出试样，挤干，放入100℃烘箱中烘60分钟。 A 10 cm 2 polypropylene fiber nonwoven fabric (100%) sample was immersed in a mixed solution of n-hexane and ethanol in a mass ratio of 1:1 at room temperature, and the mixed solution contained 1% of JT-SQ nano-SiO. 2 (15 nm) and 2% polydimethylsiloxane (Mn = 15,000). After soaking for 25 minutes, the sample was taken out, squeezed, and baked in a 100 ° C oven for 60 minutes.
实施例14。Example 14.
将10cm 2的聚丙烯纤维无纺布(100%)试样在室温下浸入由正己烷与乙醇按照1∶1的质量比组成的混合溶液中，该混合溶液中含有2% JT-SQ纳米SiO 2(15nm)和2%聚二甲基硅氧烷(Mn=15000)。浸泡25分钟后，取出试样，挤干，放入100℃烘箱中烘60分钟。 A 10 cm 2 polypropylene fiber nonwoven fabric (100%) sample was immersed in a mixed solution of n-hexane and ethanol in a mass ratio of 1:1 at room temperature, and the mixed solution contained 2% of JT-SQ nano-SiO. 2 (15 nm) and 2% polydimethylsiloxane (Mn = 15,000). After soaking for 25 minutes, the sample was taken out, squeezed, and baked in a 100 ° C oven for 60 minutes.
再将烘干的试样放入超热氢引入交联设备中，在真空度5.0×10 -4Pa条件下，以电压150V进行超热氢引入交联处理40秒。处理完后得到超疏水聚丙烯无纺布样品。 The dried sample was placed in a superheated hydrogen introduction crosslinking device, and superheated hydrogen was introduced into the crosslinking treatment at a voltage of 150 V for 40 seconds under a vacuum of 5.0×10 -4 Pa. A superhydrophobic polypropylene nonwoven sample was obtained after the treatment.
实施例15。Example 15.
将10cm 2的聚酯纤维无纺布(100%)试样在室温下浸入由正己烷与乙醇按照1∶1的质量比组成的混合溶液中，该混合溶液中含有1% JT-SQ纳米SiO 2(15nm)和2%聚二甲基硅氧烷(Mn=15000)。浸泡25分钟后，取出试样，挤干，放入100℃烘箱中烘60分钟。 A 10 cm 2 polyester fiber nonwoven fabric (100%) sample was immersed in a mixed solution of n-hexane and ethanol in a mass ratio of 1:1 at room temperature, and the mixed solution contained 1% of JT-SQ nano-SiO. 2 (15 nm) and 2% polydimethylsiloxane (Mn = 15,000). After soaking for 25 minutes, the sample was taken out, squeezed, and baked in a 100 ° C oven for 60 minutes.
再将烘干的试样放入超热氢引入交联设备中，在真空度5.0×10 -4Pa条件下，以电压150V进行超热氢引入交联处理40秒。处理完后得到超疏水聚酯无纺布样品。 The dried sample was placed in a superheated hydrogen introduction crosslinking device, and superheated hydrogen was introduced into the crosslinking treatment at a voltage of 150 V for 40 seconds under a vacuum of 5.0×10 -4 Pa. A superhydrophobic polyester nonwoven sample was obtained after the treatment.
对照例4。Comparative Example 4.
将10cm 2的聚酯纤维无纺布(100%)试样在室温下浸入由正己烷与乙醇按照1∶1的质量比组成的混合溶液中，该混合溶液中含有1% JT-SQ纳米SiO 2(15nm)和2%聚二甲基硅氧烷(Mn=15000)。浸泡25分钟后，取出试样，挤干，放入100℃烘箱中烘60分钟。 A 10 cm 2 polyester fiber nonwoven fabric (100%) sample was immersed in a mixed solution of n-hexane and ethanol in a mass ratio of 1:1 at room temperature, and the mixed solution contained 1% of JT-SQ nano-SiO. 2 (15 nm) and 2% polydimethylsiloxane (Mn = 15,000). After soaking for 25 minutes, the sample was taken out, squeezed, and baked in a 100 ° C oven for 60 minutes.
实施例16。Example 16.
将10cm 2的聚酯纤维无纺布(100%)试样在室温下浸入由正己烷与乙醇按照1∶1的质量比组成的混合溶液中，该混合溶液中含有2% JT-SQ纳米SiO 2(15nm)和2%聚二甲基硅氧烷(Mn=15000)。浸泡25分钟后，取出试样，挤干，放入100℃烘箱中烘60分钟。 A 10 cm 2 polyester fiber nonwoven fabric (100%) sample was immersed in a mixed solution of n-hexane and ethanol in a mass ratio of 1:1 at room temperature, and the mixed solution contained 2% of JT-SQ nano-SiO. 2 (15 nm) and 2% polydimethylsiloxane (Mn = 15,000). After soaking for 25 minutes, the sample was taken out, squeezed, and baked in a 100 ° C oven for 60 minutes.
再将烘干的试样放入超热氢引入交联设备中，在真空度5.0×10 -4Pa条件下，以电压150V进行超热氢引入交联处理40秒。处理完后得到超疏水聚酯无纺布样品。 The dried sample was placed in a superheated hydrogen introduction crosslinking device, and superheated hydrogen was introduced into the crosslinking treatment at a voltage of 150 V for 40 seconds under a vacuum of 5.0×10 -4 Pa. A superhydrophobic polyester nonwoven sample was obtained after the treatment.
检测上述各实施例和对照例得到超疏水织物的接触角、滚动角、耐摩擦次数和耐洗性指标，具体测试结果列在表1中。The contact angle, rolling angle, number of rubbing resistance and washing durability of the superhydrophobic fabric were examined by the above respective examples and comparative examples, and the specific test results are shown in Table 1.
其中，耐摩擦次数是指以2300Pa的摩擦压力摩擦超疏水织物，超疏水织物的水接触角下降至其初始值的90%时的摩擦循环次数。Among them, the number of rubbing resistance refers to the number of rubbing cycles when the superhydrophobic fabric is rubbed with a friction pressure of 2300 Pa, and the water contact angle of the superhydrophobic fabric is decreased to 90% of its initial value.
耐洗性是指超疏水织物的水接触角下降至其初始值的90%时的洗涤次数。Washfastness refers to the number of washes when the water contact angle of the superhydrophobic fabric drops to 90% of its initial value.
表table 1  1 各实施例超疏水纺织物的性能参数Performance parameters of superhydrophobic textiles of various examples
编号Numbering 接触角°Contact angle 滚动角°Rolling angle ° 耐摩擦次数Friction resistance 耐洗性(次)Washability (times)
实施例1Example 1 165.7165.7 1818 50005000 5050
实施例2Example 2 160.4160.4 2525 50005000 5050
对照例1Comparative Example 1 167.4167.4 8585 10001000 55
实施例3Example 3 162.3162.3 3030 50005000 5050
实施例4Example 4 165.3165.3 2020 48004800 5050
实施例5Example 5 165.0165.0 23twenty three 45004500 5050
实施例6Example 6 166.2166.2 2828 45004500 3030
实施例7Example 7 158.3158.3 2929 40004000 3030
实施例8Example 8 155.2155.2 1515 32003200 3030
实施例9Example 9 165.1165.1 1818 40004000 3030
实施例10Example 10 160.0160.0 2828 35003500 3030
实施例11Example 11 152.0152.0 22 60006000 5050
对照例2Comparative Example 2 157.0157.0 1616 50005000 3030
实施例12Example 12 159.0159.0 44 40004000 4040
实施例13Example 13 154.0154.0 1212 70007000 —-
对照例3Comparative Example 3 153.0153.0 3939 20002000 —-
实施例14Example 14 150.0150.0 1414 55005500 —-
实施例15Example 15 158.0158.0 4242 70007000 —-
对照例4Comparative Example 4 156.0156.0 2727 10001000 —-
实施例16Example 16 161.0161.0 2626 50005000 —-
表1中，由于实施例13～16中使用的是聚丙烯和聚酯的无纺布，其主要是一次性用途，不适合/需要做水洗测试，所以未进行耐洗性测试。In Table 1, since the nonwoven fabrics of polypropylene and polyester were used in Examples 13 to 16, they were mainly used for one-time use, and were not suitable/need to be subjected to a water wash test, so the wash durability test was not performed.
表1中，不同材质织物的水接触角均大于150°。但是，不同材质织物的滚动角与耐摩擦次数之间还是存在较大的差异，这与织物的材质密切相关。然而可以看出，同一种织物之间，本发明方法处理后的滚动角与耐摩擦次数以及耐水洗次数还是明显优于传统方法处理的织物。In Table 1, the water contact angles of the fabrics of different materials are all greater than 150°. However, there is still a large difference between the rolling angle of the different fabrics and the number of rubbing resistances, which is closely related to the material of the fabric. However, it can be seen that between the same fabric, the rolling angle and the number of rubbing resistances and the number of times of washing resistance after the treatment of the method of the present invention are significantly better than those of the conventional method.

Claims (10)

  1. 一种超疏水纺织物的制备方法，是先使用整理液对纺织物进行浸渍整理，再将整理后的纺织物放入超热氢交联装置中，以10～20eV的超热氢分子对其进行轰击交联，得到具有超疏水特性的纺织物；其中，在所述整理液中含有疏水改性纳米SiO 2，以及能够与所述疏水改性纳米SiO 2混溶的、具有-CH键的有机聚合物。 A method for preparing a superhydrophobic textile fabric is to first impregnate a textile fabric with a finishing liquid, and then put the finished textile into an ultra-thermal hydrogen crosslinking device to superheat hydrogen molecules of 10-20 eV. Bombardment cross-linking to obtain a textile having superhydrophobic properties; wherein the finishing liquid contains hydrophobically modified nano-SiO 2 and a -CH bond capable of being miscible with the hydrophobically modified nano-SiO 2 Organic polymer.
  2. 根据权利要求1所述的超疏水纺织物的制备方法，其特征是所述的疏水改性纳米SiO 2是经甲基三氯硅烷或二甲基二氯硅烷改性的、粒径3～100nm的疏水改性纳米SiO 2。 The method for preparing a superhydrophobic textile according to claim 1, wherein the hydrophobically modified nano-SiO 2 is modified by methyltrichlorosilane or dimethyldichlorosilane, and has a particle diameter of 3 to 100 nm. Hydrophobically modified nano-SiO 2 .
  3. 根据权利要求1所述的超疏水纺织物的制备方法，其特征是所述的有机聚合物是数均分子量5000～200000的聚二甲基硅氧烷，或数均分子量1000～20000的聚顺丁二烯。The method for preparing a superhydrophobic textile according to claim 1, wherein the organic polymer is a polydimethylsiloxane having a number average molecular weight of 5,000 to 200,000, or a polysulfide having a number average molecular weight of 1,000 to 20,000. Butadiene.
  4. 根据权利要求1所述的超疏水纺织物的制备方法，其特征是所述整理液的溶媒为正己烷或乙醇，或者两者的任意比例混合物。The method for producing a superhydrophobic textile according to claim 1, wherein the solvent of the finishing liquid is n-hexane or ethanol, or a mixture of the two in any ratio.
  5. 根据权利要求1所述的超疏水纺织物的制备方法，其特征是所述整理液中含有0.1～3wt%疏水改性纳米SiO 2、0.1～3wt%有机聚合物。 The method for preparing a superhydrophobic textile according to claim 1, wherein the finishing liquid contains 0.1 to 3 wt% of hydrophobically modified nano-SiO 2 and 0.1 to 3 wt% of an organic polymer.
  6. 根据权利要求1或5所述的超疏水纺织物的制备方法，其特征是所述整理液中有机聚合物与疏水改性纳米SiO 2的质量比为1∶0.4～2.5。 The method for preparing a superhydrophobic textile according to claim 1 or 5, wherein the mass ratio of the organic polymer to the hydrophobically modified nano-SiO 2 in the finishing liquid is 1:0.4 to 2.5.
  7. 根据权利要求1所述的超疏水纺织物的制备方法，其特征是所述的浸渍整理是将纺织物浸入所述整理液中浸泡1～60分钟，取出沥干后，于85～105℃烘箱中烘1～3小时。The method for preparing a superhydrophobic textile according to claim 1, wherein the immersion finishing comprises immersing the woven fabric in the finishing liquid for 1 to 60 minutes, removing and draining, and drying at 85 to 105 ° C. Bake in 1 to 3 hours.
  8. 根据权利要求1所述的超疏水纺织物的制备方法，其特征是所述的超热氢交联设备为US 7,998,537中描述的设备。The method for preparing a superhydrophobic textile according to claim 1, wherein said superheated hydrogen crosslinking device is US The device described in 7,998,537.
  9. 根据权利要求1所述的超疏水纺织物的制备方法，其特征是将浸渍整理后的纺织物放入超热氢引入交联设备中，在加速电压10～500 V、真空度低于10 -3Pa条件下，产生具有能量为10～20eV的超热氢分子，对纺织物轰击5～120秒，使其表面交联后得到所述超疏水纺织物。 The method for preparing a superhydrophobic textile according to claim 1, wherein the immersed and woven fabric is placed in a superheated hydrogen introduction crosslinking device at an acceleration voltage of 10 to 500 V and a vacuum of less than 10 - Under the condition of 3 Pa, an ultra-hydrogen hydrogen molecule having an energy of 10 to 20 eV is generated, and the textile is bombarded for 5 to 120 seconds to cross-link the surface to obtain the superhydrophobic textile.
  10. 根据权利要求1所述的超疏水纺织物的制备方法，其特征是所述的纺织物是棉织布，或者是聚酯纤维或聚丙烯纤维的纺织布或无纺布。The method of preparing a superhydrophobic textile according to claim 1, wherein the textile is a cotton woven fabric or a woven or non-woven fabric of polyester fiber or polypropylene fiber.
PCT/CN2018/095291 2017-07-13 2018-07-11 Method for preparing super-hydrophobic textile WO2019011278A1 (en)

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