CN109400798A - Environment-friendly type is super-hydrophobic/oleophobic textile finish, preparation method and application - Google Patents

Environment-friendly type is super-hydrophobic/oleophobic textile finish, preparation method and application Download PDF

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Publication number
CN109400798A
CN109400798A CN201710702447.7A CN201710702447A CN109400798A CN 109400798 A CN109400798 A CN 109400798A CN 201710702447 A CN201710702447 A CN 201710702447A CN 109400798 A CN109400798 A CN 109400798A
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hydrophobic
monomer
super
environment
friendly type
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CN109400798B (en
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张丹
郑君红
郑磊
黄婵娟
龙柱
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Jiangnan University
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Jiangnan University
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    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F212/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an aromatic carbocyclic ring
    • C08F212/02—Monomers containing only one unsaturated aliphatic radical
    • C08F212/04—Monomers containing only one unsaturated aliphatic radical containing one ring
    • C08F212/06—Hydrocarbons
    • C08F212/08—Styrene
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F2/00—Processes of polymerisation
    • C08F2/12—Polymerisation in non-solvents
    • C08F2/16—Aqueous medium
    • C08F2/22—Emulsion polymerisation
    • C08F2/24—Emulsion polymerisation with the aid of emulsifying agents
    • C08F2/30—Emulsion polymerisation with the aid of emulsifying agents non-ionic
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F2/00—Processes of polymerisation
    • C08F2/36—Polymerisation in solid state
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
    • C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
    • C08F220/10—Esters
    • C08F220/12—Esters of monohydric alcohols or phenols
    • C08F220/14—Methyl esters, e.g. methyl (meth)acrylate
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
    • C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
    • C08F220/10—Esters
    • C08F220/12—Esters of monohydric alcohols or phenols
    • C08F220/16—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms
    • C08F220/18—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms with acrylic or methacrylic acids
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
    • C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
    • C08F220/10—Esters
    • C08F220/22—Esters containing halogen
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
    • C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
    • C08F220/10—Esters
    • C08F220/22—Esters containing halogen
    • C08F220/24—Esters containing halogen containing perhaloalkyl radicals
    • 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
    • D06M15/21—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M15/263—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of unsaturated carboxylic acids; Salts or esters 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
    • D06M15/21—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M15/263—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of unsaturated carboxylic acids; Salts or esters thereof
    • D06M15/277—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of unsaturated carboxylic acids; Salts or esters thereof containing fluorine
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
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    • 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
    • D06M15/21—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M15/347—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of unsaturated ethers, acetals, hemiacetals, ketones or aldehydes
    • 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
    • D06M15/21—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M15/356—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of other unsaturated compounds containing nitrogen, sulfur, silicon or phosphorus atoms
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
    • C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
    • C08F220/10—Esters
    • C08F220/12—Esters of monohydric alcohols or phenols
    • C08F220/16—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms
    • C08F220/18—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms with acrylic or methacrylic acids
    • C08F220/1804—C4-(meth)acrylate, e.g. butyl (meth)acrylate, isobutyl (meth)acrylate or tert-butyl (meth)acrylate
    • 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
    • D06M2200/11—Oleophobic 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
    • D06M2200/10—Repellency against liquids
    • D06M2200/12—Hydrophobic properties
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
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    • D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
    • D06M2200/25—Resistance to light or sun, i.e. protection of the textile itself as well as UV shielding materials or treatment compositions therefor; Anti-yellowing treatments
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
    • D06M2200/50—Modified hand or grip properties; Softening compositions

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Health & Medical Sciences (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Materials Applied To Surfaces To Minimize Adherence Of Mist Or Water (AREA)
  • Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)

Abstract

The invention discloses a kind of environment-friendly type it is super-hydrophobic/oleophobic textile finish, preparation method and application.The preparation method includes: to disperse compound emulsifying agent in deionized water, after agitating and heating, pre-emulsification is carried out with mixing such as acrylic ester monomer, styrene monomer and anti-ultraviolet polymerisable monomers again to react, then temperature of continuing rising is relayed in nitrogen, and fluorochemical monomer and initiator is added with initiated polymerization, inorganic uvioresistant finishing agent is added in polymerization reaction after the completion.It is of the invention that preparation is simple, convenient for large-scale production, and safety and environmental protection, it is low in cost, simultaneously environment-friendly type of the invention it is super-hydrophobic/oleophobic textile finish is easy to use, the excellent wearability of fabric, washability, hydrophobic oleophobic performance can be assigned, while the anti-ultraviolet property of fabric, Resisting fractre intensity can also be significantly increased, and the feel and good gas permeability of soft fabric are kept, and will not influence the wearability of fabric completely.

Description

Environment-friendly type is super-hydrophobic/oleophobic textile finish, preparation method and application
Technical field
The present invention relates to a kind of fabric finishing agents, and in particular to a kind of environment-friendly type is super-hydrophobic/oleophobic textile finish, its Preparation method and application belongs to textile finishing technical field.
Background technique
In recent years, super-hydrophobic/oleophobic material not only has important use in daily life, defends in national defense industry, medical treatment The various fields such as raw have extremely wide application prospect.Super-hydrophobic/oleophobic fabric is because it has special wettability, simultaneously also There are the performances such as Water-proof and oil-proof, antifouling, anticorrosive, freezing and automatically cleaning gradually to have been favored by people.Studies have shown that micro-nano Compound coarse structure and low-surface-energy are the key factors that super-hydrophobic/oleophobic surface is formed.
Based on this, there has been proposed many methods for preparing super-hydrophobic/oleophobic surface, as LBL self-assembly method, colloidal sol-are solidifying Glue method, plasma technology, electrochemical deposition method, etching method, phase separation method and template etc..However, the side of wherein most Method complex procedures, technical process control is difficult, needs to use special equipment, and a part of method therein is also only applicable to The flat surfaces of some special substances, it is difficult to be widely applied.
On the other hand, in textile finishing field, traditional fluorinated acrylate finishing agent mostly uses solution polymerization process system , wherein most organic solvent is poisonous and harmful and volatile, although work well it is unhealthy not environmentally, and higher cost. Furthermore it is 8 perfluoro capryl sulfonyl derivative (PFOS) and perfluorooctanoic acid that traditional fluorine-contained finishing agent, which mostly uses carbon atom number, Compound (PFOA), they are considered to have excellent hydrophobic oleophobic characteristic and good surface-active.However PFOS is a kind of Chemical stability is high, and the perfluorocarbon compound with durability, bioaccumulation and toxicity, not degradable in the environment, and There is harmfulness and potential carcinogenicity to organism, PFOS has been that European Union member countries are forbidden to use and import.
Summary of the invention
The main purpose of the present invention is to provide a kind of environment-friendly type it is super-hydrophobic/oleophobic textile finish, preparation method And application, to overcome deficiency in the prior art.
To realize aforementioned invention purpose, the technical solution adopted by the present invention is as follows:
The embodiment of the invention provides a kind of environment-friendly type it is super-hydrophobic/preparation method of oleophobic textile finish comprising:
(1) compound emulsifying agent is evenly dispersed in deionized water, it is persistently stirred and is added with the speed of 100~900r/min Heat adds acrylic ester monomer, styrene monomer and anti-ultraviolet polymerisable monomer to 40~60 DEG C, carries out pre-emulsification React 30~120min；
(2) the obtained pre-emulsification reaction mixture of step (1) is continuously heating to 65~85 DEG C under protective atmosphere, and slowly Fluorochemical monomer is added；
(3) initiator is added into the obtained hybrid reaction system of step (2), and carries out polymerization reaction 8~for 24 hours, Zhi Houjia Enter inorganic uvioresistant finishing agent, be made the environment-friendly type it is super-hydrophobic/oleophobic textile finish.
In some preferred embodiments, step (3) includes: the uniform speed slow into step (2) obtained hybrid reaction system The aqueous solution of initiator is added dropwise to cause polymerization in ground, and time for adding is 30~120min, is further continued for carrying out polymerization reaction 8~for 24 hours, Inorganic uvioresistant finishing agent is added after the completion of polymerization reaction, obtain the environment-friendly type it is super-hydrophobic/oleophobic textile finish.
The embodiment of the invention also provides the environment-friendly type prepared by preceding method it is super-hydrophobic/oleophobic textile finish.
The embodiment of the invention also provides the environment-friendly type it is super-hydrophobic/purposes of oleophobic textile finish.
Compared with the existing technology, the invention has the advantages that
(1) environment-friendly type provided by the invention it is super-hydrophobic/preparation process of oleophobic textile finish uses emulsion polymerization It realizes, and using water as dispersed phase, it is not only simple and easy, convenient for being mass produced, and also it is low in cost, environmental-friendly；It can assign Give super-hydrophobic textile, oleophobic and anti-pollution；,；
(2) environment-friendly type provided by the invention it is super-hydrophobic/oleophobic textile finish safety and environmental protection, be free of perfluoro caprylic acid (PFOA) and perfluorooctane sulfonate (PFOS) class compound, easy to use, the modes such as it is applicable to spraying, dipping and brushes Textile is arranged, applicable fabric includes all kinds of textiles such as cotton, fiber crops, silk, hair, suede, fiber, leather.
(3) environment-friendly type provided by the invention it is super-hydrophobic/oleophobic textile finish can assign fabric excellent wearability And washability, excellent hydrophobic oleophobic performance, while the anti-ultraviolet property of fabric can also be significantly increased, and significantly increase The Resisting fractre intensity of strong fabric, and also there is the soft feel being equal with fibril materials and good through its fabric after arranging Gas permeability, will not influence the wearability of fabric completely.
Detailed description of the invention
Fig. 1 a- Fig. 1 b be water and n-dodecane a kind of typical environment-friendly type of the invention it is super-hydrophobic/oleophobic textile finishing The test chart of the contact angle (respectively 160 ° and 130 °) on textile after agent arrangement.
Fig. 2 be 10 μ of μ L~30 L water droplet a kind of typical environment-friendly type of the invention it is super-hydrophobic/oleophobic textile finish Wellability test chart on textile after arrangement.
Fig. 3 be water, olive oil, hexadecane, n-dodecane a kind of typical environment-friendly type of the invention it is super-hydrophobic/oleophobic spins The wellability test chart on textile after the arrangement of fabric finishing agent.
Specific embodiment
In view of deficiency in the prior art, inventor is studied for a long period of time and is largely practiced, and is able to propose of the invention Technical solution.A kind of environment-friendly type that the one aspect of the embodiment of the present invention provides is super-hydrophobic/preparation of oleophobic textile finish Method includes:
(1) compound emulsifying agent is evenly dispersed in deionized water, it is persistently stirred and is added with the speed of 100~900r/min Heat adds acrylic ester monomer, styrene monomer and anti-ultraviolet polymerisable monomer to 40~60 DEG C, carries out pre-emulsification React 30~120min；
(2) the obtained pre-emulsification reaction mixture of step (1) is continuously heating to 65~85 DEG C under protective atmosphere, and slowly Fluorochemical monomer is added；
(3) initiator is added into the obtained hybrid reaction system of step (2), and carries out polymerization reaction 8~for 24 hours, Zhi Houjia Enter inorganic uvioresistant finishing agent, be made the environment-friendly type it is super-hydrophobic/oleophobic textile finish.
In some preferred embodiments, the step (3) includes: even into the obtained hybrid reaction system of step (2) The aqueous solution of initiator is added dropwise slowly to cause polymerization in speed, and time for adding is 30~120min, is further continued for carrying out polymerization reaction 8 ~for 24 hours, inorganic uvioresistant finishing agent is added after the completion of polymerization reaction, obtain the environment-friendly type it is super-hydrophobic/oleophobic textile Finishing agent.In some more specific embodiments, the environment-friendly type is super-hydrophobic/the preparation side of oleophobic textile finish Method includes:
(1) compound emulsifying agent is evenly dispersed in deionized water, 40~60 DEG C are heated with stirring to, mixing speed 100 ~900r/min, then acrylic ester monomer, styrene monomer and anti-ultraviolet polymerisable monomer are added in reaction system, It carries out pre-emulsification and reacts 30~120min；
(2) protective gas such as nitrogen are then passed to, 65~85 DEG C is continuously heating to, is slowly added to fluorochemical monomer；
(3) aqueous solution of initiator is added dropwise then to uniform speed slow in system with cause polymerization, time for adding be 30~ 120min, continuation polymerization reaction 8~for 24 hours, inorganic uvioresistant finishing agent is added after the completion of polymerization, it is super that environment-friendly type can be obtained Hydrophobic/oleophobic textile finish.
Further, the compound emulsifying agent includes anionic surfactant and nonionic surfactant；Described Anionic surfactant include neopelex, dodecyl sodium sulfate, double dodecylphenyl ether sodium disulfonates, Lauryl sodium sulfate, enuatrol, odium stearate, sodium abietate, any one or two or more combinations in sodium laurate, And it is without being limited thereto.
Further, the nonionic surfactant includes ethoxylated dodecyl alcohol, secondary alcohol polyoxyethylene ether, alkyl Phenol polyethenoxy ether, fatty acid methyl ester APEO, any one or two or more combinations in 13 carbon alcohol ether of isomery Object, but not limited to this.
Further, the acrylic ester monomer include methyl acrylate, ethyl acrylate, methyl methacrylate, Any one in ethyl methacrylate, butyl acrylate or two or more compositions, but not limited to this.
Further, the fluorochemical monomer includes perfluoro hexyl ethyl propylene acid esters, in ten trifluoro monooctyl ester of methacrylic acid Any one or two or more compositions, but not limited to this.
Further, the initiator includes ammonium persulfate, potassium peroxydisulfate, t-butylperbenzoate, azo diisobutyl amidine It is any one or more among bis- (2- methyl propanamide) dihydrochlorides of hydrochloride, dibenzoyl peroxide, 2,2'- azo Composition, but not limited to this.
Further, the anti-ultraviolet polymerisable monomer includes 2- ethyl -2 '-cyano -3- diphenyl acrylate, third Acrylamide, γ-(methacryloxy) propyl trimethoxy silicane, esters of acrylic acid benzophenone cpd, 2- hydroxyl -4- Propenyloxy group benzophenone, acrylic acid -2,2,6,6- tetramethyl piperidine ester, methacrylic acid -2,2,6,6- tetramethyl piperidine ester, Acrylic acid -1,2,2,6,6- pentamethvl ester, methacrylic acid -1,2,2,6,6- pentamethvl ester any one of or Two or more compositions, and it is without being limited thereto.
Further, the inorganic uvioresistant finishing agent includes TiO2、ZnO、Al2O3, kaolin, talcum powder, charcoal Black, iron oxide, lead monoxide, clay, CaCO3Among any one or more compositions, but not limited to this.
It is more preferred, the acrylic ester monomer, styrene monomer, anti-ultraviolet polymerisable monomer, fluorine-containing list The volume ratio of body and deionized water is 1:0.1~5:0.01~0.1:0.1~5:20~200.
More preferred, the quality of the compound emulsifying agent is the acrylic ester monomer, styrene monomer, uvioresistant The polymerisable monomer of line and 1wt%~10wt% of fluorochemical monomer gross mass.
It is more preferred, the compound emulsifying agent include anionic surfactant that mass ratio is 1:0.1~10 with it is non- Ionic surface active agent.
More preferred, the quality of the initiator is the acrylic ester monomer, styrene monomer, anti-ultraviolet 0.05wt%~10wt% of polymerisable monomer and fluorochemical monomer gross mass.
More preferred, the quality of the inorganic uvioresistant finishing agent is the acrylic ester monomer, styrene 0.1wt%~10wt% of monomer, anti-ultraviolet polymerisable monomer and fluorochemical monomer gross mass.
More preferred, the concentration of the initiator solution is 0.1wt%~10wt%.
The other side of the embodiment of the present invention additionally provide by preceding method preparation environment-friendly type it is super-hydrophobic/oleophobic weaving Product finishing agent.Further, the environment-friendly type it is super-hydrophobic/oleophobic textile finish is emulsion system, wherein emulsion droplet Partial size is 5~200nm.
The another aspect of the embodiment of the present invention additionally provide the environment-friendly type it is super-hydrophobic/oleophobic textile finish is in knitting The purposes of object finishing field.Preferably, the fabric includes cotton, fiber crops, silk, hair, suede, fiber or leather-like textile；Preferably, Fabric after collated at least has super-hydrophobic, oleophobic and anti-pollution.
The another aspect of the embodiment of the present invention additionally provides a kind of fabric finishing method comprising: at least to spray, soak Stain or brush mode by the environment-friendly type it is super-hydrophobic/oleophobic textile finish apply on the fabric, then to fabric carry out It preliminary drying and bakes, preferably in 70~90 DEG C of 5~30min of preliminary drying, in 120~150 DEG C of 20~60min of trainings baking.
Further, the fabric includes cotton, fiber crops, silk, hair, suede, fiber or leather-like textile.
Environment-friendly type of the invention is super-hydrophobic/and oleophobic textile finish has the characteristics that waterproof oil-proof result is good and environmentally friendly, Super-hydrophobic textile, oleophobic, antifouling and high-efficient and lasting anti-ultraviolet property can be assigned.
Environment-friendly type of the invention is super-hydrophobic/and the preparation method of oleophobic textile finish has that preparation is simple, The advantages that convenient for being mass produced.
The present invention is described in detail combined with specific embodiments below.Following embodiment will be helpful to the technology of this field Personnel further understand the present invention, but the invention is not limited in any way.It should be pointed out that the ordinary skill of this field For personnel, without departing from the inventive concept of the premise, various modifications and improvements can be made.These belong to the present invention Protection scope.
Embodiment 1: by the compound emulsifying agent (lauryl alcohol polyethylene glycol oxide of neopelex and 0.65g containing 0.35g Ether) it is dispersed in the deionized water of 200mL, it is heated with stirring to 60 DEG C, mixing speed 300r/min, then by the first of 5mL The 2- ethyl -2 ' of base methacrylate monomer, the styrene monomer of 5mL and 0.5mL-cyano -3- diphenyl acrylate is added anti- It answers in system, carries out pre-emulsification and react 60min；Then pass to nitrogen, be continuously heating to 70 DEG C, be slowly added to 15mL perfluor oneself Base ethyl propylene acid esters；The ammonium persulfate of 0.2g is dissolved in the deionized water of 25mL, then to uniform speed slow in system The aqueous solution of ammonium persulfate is added dropwise to cause polymerization, time for adding 60min continues polymerization reaction 10h, is added after the completion of polymerization The TiO of 0.25g2, can be obtained environment-friendly type it is super-hydrophobic/oleophobic textile finish.
Embodiment 2: by compound emulsifying agent (the secondary alcohol polyoxyethylene ether of dodecyl sodium sulfate and 0.35g containing 0.65g) It is dispersed in the deionized water of 300mL, is heated with stirring to 40 DEG C, mixing speed 200r/min, then by the acrylic acid of 5mL The acrylamide of butyl ester monomer, the styrene monomer of 5mL and 0.25mL is added in reaction system, carries out pre-emulsification and reacts 30min； Nitrogen is then passed to, is continuously heating to 65 DEG C, is slowly added to the ten trifluoro monooctyl ester of methacrylic acid of 10mL；By the persulfuric acid of 0.1g Potassium is dissolved in the deionized water of 30mL, and it is poly- to cause that the aqueous solution of potassium peroxydisulfate is added dropwise then to uniform speed slow in system It closes, time for adding 90min, continues polymerization reaction 8h, the ZnO of 0.1g is added after the completion of polymerization, it is super thin that environment-friendly type can be obtained Water/oleophobic textile finish.
Embodiment 3: by compound emulsifying agent, (alkyl phenol of double dodecylphenyl ether sodium disulfonates and 0.5g containing 0.5g is poly- Ethylene oxide ether) it is dispersed in the deionized water of 100mL, 50 DEG C, mixing speed 400r/min are heated with stirring to, then will γ-(methacryloxy) propyl trimethoxy silicon of the methacrylate monomer of 5mL, the styrene monomer of 5mL and 0.2mL Alkane is added in reaction system, carries out pre-emulsification and reacts 90min；Nitrogen is then passed to, 75 DEG C is continuously heating to, is slowly added to 5mL Perfluoro hexyl ethyl propylene acid esters；The t-butylperbenzoate of 0.1g is dissolved in the deionized water of 10mL, then to system The aqueous solution of t-butylperbenzoate is added dropwise middle uniform speed slow to cause polymerization, time for adding 30min continues polymerization reaction The Al of 0.15g is added in 12h after the completion of polymerization2O3, can be obtained environment-friendly type it is super-hydrophobic/oleophobic textile finish.
Embodiment 4: by compound emulsifying agent (the fatty acid methyl ester polyoxyethylene of lauryl sodium sulfate and 0.6g containing 0.2g Ether) it is dispersed in the deionized water of 250mL, it is heated with stirring to 55 DEG C, mixing speed 500r/min, then by the third of 10mL 2- hydroxyl -4- propenyloxy group the benzophenone of olefin(e) acid acetate monomer, the styrene monomer of 5mL and 0.1mL is added in reaction system, It carries out pre-emulsification and reacts 120min；Nitrogen is then passed to, is continuously heating to 80 DEG C, is slowly added to the methacrylic acid 13 of 5mL Fluorine monooctyl ester；By the azo diisobutyl amidine hydrochloride salt of 0.2g in the deionized water of 40mL, then at the uniform velocity slow in system The aqueous solution of azo diisobutyl amidine hydrochloride is added dropwise slowly to cause polymerization, time for adding 120min continues polymerization reaction 15h, polymerization after the completion of be added 1g kaolin, can be obtained environment-friendly type it is super-hydrophobic/oleophobic textile finish.
Embodiment 5: compound emulsifying agent (the 13 carbon alcohol ether of isomery of sodium abietate and 0.2g containing 0.6g) is evenly dispersed In the deionized water of 200mL, it is heated with stirring to 60 DEG C, mixing speed 900r/min, then by the ethyl methacrylate of 5mL Acrylic acid -2,2 of monomer, the styrene monomer of 10mL and 0.5mL, 6,6- tetramethyl piperidine esters are added in reaction system, carry out Pre-emulsification reacts 70min；Nitrogen is then passed to, is continuously heating to 85 DEG C, is slowly added to the perfluoro hexyl ethylacrylic acid of 10mL Ester；The dibenzoyl peroxide of 0.5g is dissolved in the deionized water of 50mL, was added dropwise then to uniform speed slow in system The aqueous solution of dibenzoyl is aoxidized to cause polymerization, time for adding 60min continues polymerization reaction 10h, is added after the completion of polymerization The talcum powder of 0.15g, can be obtained environment-friendly type it is super-hydrophobic/oleophobic textile finish.
Environment-friendly type prepared by Example 1-5 is super-hydrophobic/oleophobic textile finish (following abbreviation product of the present invention) It the modes such as sprayed, impregnated or is brushed to textile, preliminary drying then is carried out to textile and bake a period of time.It is examined through test It surveys, product of the present invention is all larger than 150 ° to the water contact angle after textile finishing, and vegetable oil contact angle is all larger than 130 °, has excellent Hydrophobic, oleophobic, self-cleaning performance, and arrange after fabric by 30 conventional washes or by 1000 times friction after, still With good hydrophobic oleophobic performance, while also there is excellent washability and wearability.Further, product of the present invention is being assigned While giving fabric excellent hydrophobic oleophobic performance, can also be significantly increased fabric anti-ultraviolet property and enhancing fabric it is anti- Breaking strength, and there is the soft feel and good gas permeability being equal with fibril materials through its fabric after arranging, it is complete It will not influence the wearability of fabric entirely.The environment-friendly type is super-hydrophobic/oleophobic textile finish product be suitable for cotton, fiber crops, silk, All kinds of textiles such as hair, suede, fiber, leather.
Please refer to Fig. 1 a- Fig. 1 b show water and n-dodecane a kind of typical environment-friendly type of the invention it is super-hydrophobic/oleophobic The contact angle (respectively 160 ° and 130 °) on textile after textile finish arrangement.Fig. 2 shows 10 μ of μ L~30 L's Water droplet a kind of typical environment-friendly type of the invention it is super-hydrophobic/oleophobic textile finish arrange after textile on wellability. Fig. 3 show water, olive oil, hexadecane, n-dodecane a kind of typical environment-friendly type of the invention it is super-hydrophobic/oleophobic textile The wellability on textile after finishing agent arrangement.
Various reaction partners and process conditions used by previous embodiment are more typical examples, but by this Case invents the National People's Congress and measures verification experimental verification, other different types of reaction partners and other process conditions listed by this specification It is applicable Deng also, and also equal attainable cost invents claimed technical effect, for example, by environment-friendly type provided by the invention Treated that fabric fibre surface can form one layer of uniform and fine and close film, the tunic for super-hydrophobic/oleophobic textile finish It not only assigns fabric excellent ultra-hydrophobicity, also adds significantly the Resisting fractre intensity of fabric.
It should be appreciated that the technical concepts and features of above-described embodiment only to illustrate the invention, its object is to allow be familiar with this The personage of item technology cans understand the content of the present invention and implement it accordingly, and it is not intended to limit the scope of the present invention.It is all Equivalent change or modification made by Spirit Essence according to the present invention, should be covered by the protection scope of the present invention.

Claims (10)

1. a kind of environment-friendly type is super-hydrophobic/preparation method of oleophobic textile finish, characterized by comprising:
(1) compound emulsifying agent is evenly dispersed in deionized water, it is continuously stirred and heated to the speed of 100~900r/min 40~60 DEG C, acrylic ester monomer, styrene monomer and anti-ultraviolet polymerisable monomer are added, carries out pre-emulsification reaction 30~120min；
(2) the obtained pre-emulsification reaction mixture of step (1) is continuously heating under protective atmosphere 65~85 DEG C, and be slowly added to Fluorochemical monomer；
(3) initiator is added into the obtained hybrid reaction system of step (2), and carries out polymerization reaction 8~for 24 hours, nothing is added later Machine class uvioresistant finishing agent, be made the environment-friendly type it is super-hydrophobic/oleophobic textile finish.
2. preparation method according to claim 1, which is characterized in that step (3) includes: to obtain mixing instead to step (2) Answer the aqueous solution of initiator is added dropwise to uniform speed slow in system with cause polymerization, time for adding be 30~120min, be further continued for into Inorganic uvioresistant finishing agent is added after the completion of polymerization reaction in row polymerization reaction 8~for 24 hours, obtain the environment-friendly type it is super-hydrophobic/ Oleophobic textile finish.
3. preparation method according to claim 1 or 2, it is characterised in that: the compound emulsifying agent includes anionic surface Activating agent and/or nonionic surfactant；Preferably, the anionic surfactant include neopelex, Dodecyl sodium sulfate, double dodecylphenyl ether sodium disulfonates, lauryl sodium sulfate, enuatrol, odium stearate, rosin acid Any one in sodium, sodium laurate or two or more combinations；Preferably, the nonionic surfactant includes laruyl alcohol Polyoxyethylene ether, secondary alcohol polyoxyethylene ether, alkyl phenol polyoxyethylene ether, fatty acid methyl ester APEO, 13 carbon alcohol of isomery Any one in ether or two or more compositions；And/or the acrylic ester monomer includes methyl acrylate, propylene Acetoacetic ester, methyl methacrylate, ethyl methacrylate, any one or two or more combinations in butyl acrylate Object；And/or the fluorochemical monomer include perfluoro hexyl ethyl propylene acid esters, it is any one in ten trifluoro monooctyl ester of methacrylic acid Kind or two or more compositions；And/or the initiator includes ammonium persulfate, potassium peroxydisulfate, t-butylperbenzoate, azo Any one of bis- (2- methyl propanamide) dihydrochlorides of diisobutyl amidine hydrochloride, dibenzoyl peroxide, 2,2'- azo Or two or more composition；And/or the anti-ultraviolet polymerisable monomer includes 2- ethyl -2 '-cyano -3- biphenyl third Olefin(e) acid ester, acrylamide, γ-(methacryloxy) propyl trimethoxy silicane, esters of acrylic acid benzophenone cpd, 2- hydroxyl -4- propenyloxy group benzophenone, acrylic acid -2,2,6,6- tetramethyl piperidine ester, methacrylic acid -2,2,6,6- tetramethyl Phenylpiperidines ester, acrylic acid -1,2,2,6,6- pentamethvl ester, among methacrylic acid -1,2,2,6,6- pentamethvl ester Any one or more compositions；And/or the inorganic uvioresistant finishing agent includes TiO2、ZnO、Al2O3, it is high Ridge soil, talcum powder, carbon black, iron oxide, lead monoxide, clay, CaCO3Among any one or more compositions.
4. preparation method according to claim 1, it is characterised in that: the acrylic ester monomer, resists styrene monomer The volume ratio of the polymerisable monomer of ultraviolet light, fluorochemical monomer and deionized water be 1:0.1~5:0.01~0.1:0.1~5:20~ 200；
And/or the quality of the compound emulsifying agent is the acrylic ester monomer, styrene monomer, anti-ultraviolet gathers Close 1wt%~10wt% of monomer and fluorochemical monomer gross mass；
And/or the compound emulsifying agent includes that the anionic surfactant that mass ratio is 1:0.1~10 is lived with non-ionic surface Property agent；
And/or the quality of the initiator is the acrylic ester monomer, styrene monomer, anti-ultraviolet polymerizable list 0.05wt%~10wt% of body and fluorochemical monomer gross mass；
And/or the quality of the inorganic uvioresistant finishing agent is the acrylic ester monomer, styrene monomer, anti-purple The polymerisable monomer of outside line and 0.1wt%~10wt% of fluorochemical monomer gross mass.
5. preparation method according to claim 2, it is characterised in that: the concentration of the initiator solution is 0.1wt% ~10wt%.
6. by any one of claim 1-5 the method prepare environment-friendly type it is super-hydrophobic/oleophobic textile finish.
7. environment-friendly type according to claim 6 is super-hydrophobic/oleophobic textile finish, it is characterised in that: the environment-friendly type Super-hydrophobic/oleophobic textile finish is emulsion system, and wherein the partial size of emulsion droplet is 5~200nm.
8. the environment-friendly type as described in any one of claim 6-7 is super-hydrophobic/oleophobic textile finish is in textile finishing field Purposes；Preferably, the fabric includes cotton, fiber crops, silk, hair, suede, fiber or leather-like textile；Preferably, knitting after collated Object at least has super-hydrophobic, oleophobic and anti-pollution.
9. a kind of fabric finishing method, characterized by comprising: at least by claim 6-7 in a manner of spraying, dipping or brushing Any one of described in environment-friendly type it is super-hydrophobic/oleophobic textile finish apply on the fabric, then by fabric at 70~90 DEG C 20~60min is dried in 5~30min of preliminary drying, 120~150 DEG C of trainings.
10. fabric finishing method according to claim 9, it is characterised in that: the fabric include cotton, fiber crops, silk, hair, Suede, fiber or leather-like textile.
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CN115058894A (en) * 2022-08-17 2022-09-16 江苏金呢工程织物股份有限公司 Hydrolysis-resistant textile auxiliary for drying net

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