CN108951112A - A kind of preparation method of multifunctional nano finishing agent - Google Patents

A kind of preparation method of multifunctional nano finishing agent Download PDF

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Publication number
CN108951112A
CN108951112A CN201810768810.XA CN201810768810A CN108951112A CN 108951112 A CN108951112 A CN 108951112A CN 201810768810 A CN201810768810 A CN 201810768810A CN 108951112 A CN108951112 A CN 108951112A
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parts
finishing agent
preparation
added
room temperature
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许磊
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Suzhou Institute of Trade and Commerce
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Suzhou Institute of Trade and Commerce
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    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M11/00Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
    • D06M11/32Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
    • D06M11/36Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond with oxides, hydroxides or mixed oxides; with salts derived from anions with an amphoteric element-oxygen bond
    • D06M11/46Oxides or hydroxides of elements of Groups 4 or 14 of the Periodic Table; Titanates; Zirconates; Stannates; Plumbates
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    • D06M11/00Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
    • D06M11/32Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
    • D06M11/36Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond with oxides, hydroxides or mixed oxides; with salts derived from anions with an amphoteric element-oxygen bond
    • D06M11/44Oxides or hydroxides of elements of Groups 2 or 12 of the Periodic Table; Zincates; Cadmates
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    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M11/00Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
    • D06M11/32Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
    • D06M11/36Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond with oxides, hydroxides or mixed oxides; with salts derived from anions with an amphoteric element-oxygen bond
    • D06M11/45Oxides or hydroxides of elements of Groups 3 or 13 of the Periodic Table; Aluminates
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    • D06M11/00Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
    • D06M11/83Treating 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 metals; with metal-generating compounds, e.g. metal carbonyls; Reduction of metal compounds on textiles
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    • D06M13/00Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/322Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing nitrogen
    • D06M13/46Compounds containing quaternary nitrogen atoms
    • D06M13/463Compounds containing quaternary nitrogen atoms derived from monoamines
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    • D06M15/00Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
    • D06M15/01Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with natural macromolecular compounds or derivatives thereof
    • D06M15/03Polysaccharides or derivatives thereof
    • D06M15/05Cellulose or derivatives thereof
    • D06M15/09Cellulose ethers
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    • D06M15/00Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
    • D06M15/19Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
    • D06M15/21Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M15/263Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of unsaturated carboxylic acids; Salts or esters thereof
    • D06M15/277Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of unsaturated carboxylic acids; Salts or esters thereof containing fluorine
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    • D06M15/00Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
    • D06M15/19Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
    • D06M15/21Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M15/327Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of unsaturated alcohols or esters thereof
    • D06M15/333Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of unsaturated alcohols or esters thereof of vinyl acetate; Polyvinylalcohol
    • DTEXTILES; PAPER
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    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M15/00Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
    • D06M15/19Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
    • D06M15/37Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M15/53Polyethers
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    • D06M15/00Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
    • D06M15/19Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
    • D06M15/37Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M15/643Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing silicon in the main chain
    • D06M15/657Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing silicon in the main chain containing fluorine
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2200/00Functionality of the treatment composition and/or properties imparted to the textile material
    • D06M2200/10Repellency against liquids
    • D06M2200/12Hydrophobic properties
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    • D06M2200/00Functionality of the treatment composition and/or properties imparted to the textile material
    • D06M2200/20Treatment influencing the crease behaviour, the wrinkle resistance, the crease recovery or the ironing ease
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
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    • D06M2200/00Functionality of the treatment composition and/or properties imparted to the textile material
    • D06M2200/25Resistance to light or sun, i.e. protection of the textile itself as well as UV shielding materials or treatment compositions therefor; Anti-yellowing treatments

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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)

Abstract

The present invention provides a kind of preparation methods of multifunctional nano finishing agent, comprising the following steps: (1) is successively handled with cetyl trimethylammonium bromide, polyethylene glycol-800 and pentaerythritol stearate after grinding nanoparticle;(2) using n-butanol as organic solvent, silicon-fluorine polymer object is prepared using ten trifluoro monooctyl ester of methacrylic acid, trifluoro propyl methyl cyclotrisiloxane and benzoyl peroxide;(3) precipitating particle is distributed to containing polysorbas20 is added in lauryl sodium sulfate, carboxymethyl cellulose, polyvinyl alcohol water solution, adds silicon-fluorine polymer object and multiple functions auxiliary agent, finishing agent A is made;(4) γ-methacryloxypropyl trimethoxy silane, bleeding agent are added in isopropanol and prepare finishing agent B.The fabric handled through finishing agent of the present invention has good ultraviolet-resistent property, waterproofness, wrinkle resistance and the performances such as antistatic, therefore finishing agent produced by the present invention is with a wide range of applications during material treatment.

Description

A kind of preparation method of multifunctional nano finishing agent
Technical field
The invention belongs to textile technology fields, and in particular to a kind of preparation method of multifunctional nano finishing agent.
Background technique
Fabric finishing agent is a kind of function additive applied to fabric, it can change the surface property of fabric, to assign The special function of fabric.Such as it is to handle fabric with the finishing agent with low surface tension that hydrophobic and oil repellent, which arranges, changes fiber Surface characteristic is not easy fabric surface by water or glossy wet and sprawl, to achieve the purpose that hydrophobic and oil repellent.Soil resistant finish and easily It is to make fabric be not easy to attach dirt under dress, use condition by the surface property or surface state of change fiber that decontamination, which arranges, Dirt, or the dirt attached is easy to wash the processing technology of not recontamination.
With the development of nanosecond science and technology, nano material has become the hot spot in current new material research field, nano material Refer to size in the material of 1-100nm, there is the general material institutes such as surface area is big, Active sites are more, adsorption capacity is strong not The excellent properties that can be compared, research field have been expanded to electronics, metallurgy, space flight and aviation, chemical industry, environment, biology and medicine etc. Every field.Nano material also has a wide range of applications in field of textiles, is such as added in finishing agent and arranges to fabric, mentions For performances such as antibacterial fabric, uvioresistants.
With the improvement of living standards, people also increasingly increase the safety of textile and functional requirement, especially That there is the textile of persistence, safety, more kinetic energy increasingly to attract people's attention, there are also the comfort level of textile and Aesthetics also has higher requirement, and textile finishing is also increasing to the effect of textile therewith.However current finishing agent Can be relatively simple, be not able to satisfy the growing multi-functional demand of people, it is therefore necessary to existing finishing agent carry out into The exploitation of one step.
Summary of the invention
Above of the existing technology in order to solve the problems, such as, the purpose of the present invention is to provide a kind of arrangements of multifunctional nano The preparation method of agent, the fabric after being arranged using the finishing agent have multiple functions characteristic.
To achieve the goals above, the present invention the following technical schemes are provided:
A kind of preparation method of multifunctional nano finishing agent, comprising the following steps:
(1) by nanoscale TiO2 10-20 parts, 15-25 parts of ZnO, 8-16 parts of Ag, 5-10 parts of MgO, Al2O3 7-14 parts of progress Mixing is placed in grinder and is ground the obtained nano-mixture of 15min, nano-mixture is then added to 30-50 In the aqueous solution of part 10-30% cetyl trimethylammonium bromide, mixing 20-40min is stirred at room temperature, then places it in Then ultrasonic disperse 10-20min in Ultrasound Instrument adds 6-13 parts of polyethylene glycol-800,7-15 parts of pentaerythritol stearate, Continue to be ultrasonically treated 30-60min at a temperature of 40-50 DEG C, reactant is cooled to room temperature, is collected by centrifugation removal solvent Lower sediment particle;
(2) 20-40 parts of n-butanols are added in reaction flask as organic solvent, ten trifluoro monooctyl ester 5- of methacrylic acid is then added 10 parts,
4-8 parts of trifluoro propyl methyl cyclotrisiloxane and 0.1-0.5 parts of benzoyl peroxides, under 80-90 DEG C of water bath condition Stirring is condensed back reaction 2-4h, then cools to room temperature, reactant is placed on Rotary Evaporators and is spin-dried for solvent to get fluorine silicon Polymer;
(3) 4-8 containing lauryl sodium sulfate parts, carboxymethyl fibre are distributed to by 20-40 parts of lower sediment particle made from step (1) In the 15-30 part aqueous solution for tieing up 2-6 parts of element, 6-10 parts of polyvinyl alcohol, 1-4 parts of polysorbas20 of addition, while stirring plus Enter 20-40 parts of silicon-fluorine polymer object made from step (2), 4-9 parts of triethanolamine, 6-12 parts of 2- phosphorus base butane -1,2,4- tricarboxylic acids, 5-10 parts of maleic anhydride, 3-8 parts of ESCALOL 567,2-6 parts of octadecyldimethyl ammonium chloride, acrylic acid 7-13 parts of dimethylaminoethyl, 1-4 parts of emulsifier, persistently stir 1-3h in room temperature, and finishing agent A is made;
(4) γ -15-30 parts of methacryloxypropyl trimethoxy silane, 10-20 parts of bleeding agent are added to 30-50 parts Aqueous isopropanol in, stir 20-40min at room temperature, be made finishing agent B.
Preferably, in the step (1) each raw material parts by weight are as follows: nanoscale TiO2 15 parts, 20 parts of ZnO, 12 parts of Ag, 8 parts of MgO, Al2O3 In the aqueous solution of 10 parts, 40 parts 10-30% cetyl trimethylammonium bromides, 10 parts of polyethylene glycol-800, 11 parts of pentaerythritol stearate.
Preferably, in the step (2) each raw material parts by weight are as follows: 30 parts of n-butanol, ten trifluoro monooctyl ester 7 of methacrylic acid Part, 6 parts of trifluoro propyl methyl cyclotrisiloxane, 0.3 part of benzoyl peroxide.
Preferably, in the step (3) each raw material parts by weight are as follows: precipitating 30 parts of particle, 6 parts of lauryl sodium sulfate, 4 parts of carboxymethyl cellulose, 8 parts of polyvinyl alcohol, 23 parts of aqueous solution, 2.5 parts of polysorbas20,30 parts of silicon-fluorine polymer object, triethanolamine 6.5 parts, 9 parts of 2- phosphorus base butane -1,2,4- tricarboxylic acids, 8 parts of maleic anhydride, 5.5 parts of ESCALOL 567, ten Eight 4 parts of alkyl dimethyl ammonium chlorides, 10 parts of dimethylaminoethyl acrylate, 2.5 parts of emulsifier.
Preferably, in the step (4) each raw material parts by weight are as follows: γ-methacryloxypropyl trimethoxy silicon 23 parts of alkane, 15 parts of bleeding agent, 40 parts of isopropanol.
Preferably, the emulsifier is octyl phenol polyoxyethylene ether, dodecyl benzyl dimethyl ammonium chloride or fat One of alcohol Pluronic F-127 ether.
Preferably, the bleeding agent is one kind of Aerosol OT, mannitol or Di-phosphorus pentonide.
The technique that fabric is arranged using the finishing agent are as follows: fabric is dipped in finishing agent B first, is impregnated at room temperature After 1h, it is washed with distilled water clean, drying;Then it is dipped in finishing agent A, carries out second dipping and rolling processing, pick-up rate is 80%, the single impregnation time is 1h, dries fabric washing after the completion of processing.
The utility model has the advantages that the present invention provides a kind of preparation methods of multifunctional nano finishing agent, first by several nanoscales Functional particulate is handled with cetyl trimethylammonium bromide, so that nano grain surface forms positive charge environment, then again It is modified with polyethylene glycol-800 and pentaerythritol stearate, nano particle is adsorbed by electrostatic adsorption Surface, so that nano grain surface generates a large amount of alcoholic OH groups;Ten trifluoro monooctyl ester of methacrylic acid and trifluoro first Hydroxypropyl methyl cyclotrisiloxane
Silicon-fluorine polymer object is prepared, the surface free energy of silicon-fluorine polymer object is lower, while having excellent hydrophobic, oleophobic and stain resistant Performance, and provide finishing agent good film forming;By the nanometer hybrid particles of modification and silicon-fluorine polymer object, other function auxiliary agent into Multi-function finish A liquid is made in row hybrid reaction.It include γ-methacryloxypropyl trimethoxy in finishing agent B liquid Silane and
Bleeding agent, γ-methacryloxypropyl trimethoxy silane assigns fabric surface more hydroxyl, thus with nanometer The hydroxyl on hybrid particles surface is combined by hydrogen bond action, is improved nanometer hybrid particles in the adhesive force of web surface, is seeped The addition of saturating agent promotes finishing agent A liquid to the osmosis of fabric, to improve finishing agent to the ability to function of fabric, fills The function of finishing agent is waved in distribution.
The fabric UPF value handled through finishing agent of the present invention is up to 128.62, and surface and water contact angle are up to 205.21 °, because This is with good uvioresistant performance and waterproof performance;The creasy recovery angle of processed fabric is up to 324.3 °, breaking strength Retention rate is up to 95.6%, and therefore, fabric, which is made, in the present invention has excellent wrinkle resistance;The surface resistivity of fabric is down to 4.8 ×106Ω, volume resistivity are down to 2.2 × 106Ω, therefore fabric has good antistatic effect.Therefore it is obtained from experimental configuration To know, the fabric handled through finishing agent of the present invention has good ultraviolet-resistent property, waterproofness, wrinkle resistance and the performances such as antistatic, Therefore finishing agent produced by the present invention is with a wide range of applications during material treatment.
Specific embodiment
The invention will now be further described with reference to specific embodiments, but examples are merely exemplary, not to this hair Bright range constitutes any restrictions.It will be understood by those skilled in the art that without departing from the spirit and scope of the invention Can with the details and forms of the technical scheme of the invention are modified or replaced, but these modification and replacement each fall within it is of the invention In protection scope.
In following embodiment and comparative example, fabric is arranged using the finishing agent technique are as follows: first by fabric It is dipped in finishing agent B, after impregnating 1h at room temperature, is washed with distilled water clean, drying;Then it is dipped in finishing agent A, is carried out Second dipping and rolling processing, pick-up rate 80%, single impregnation time are 1h, dry fabric washing after the completion of processing.
Embodiment 1
A kind of preparation method of multifunctional nano finishing agent, comprising the following steps:
(1) by nanoscale TiO2 15 parts, 20 parts of ZnO, 12 parts of Ag, 8 parts of MgO, Al2O3 10 parts are mixed, and grinding is placed in It is ground 15min in machine, nano-mixture is made, nano-mixture is then added to 40 part of 20% cetyl front three In the aqueous solution of base ammonium bromide, mixing 30min is stirred at room temperature, then places it in ultrasonic disperse 15min in Ultrasound Instrument, so After add 10 parts of polyethylene glycol-800,11 parts of pentaerythritol stearate, continue to be ultrasonically treated at a temperature of 45 DEG C Reactant is cooled to room temperature by 45min, collects lower sediment particle by centrifugation removal solvent;
(2) in reaction flask be added 30 parts of n-butanols be used as organic solvent, then addition 7 parts of ten trifluoro monooctyl ester of methacrylic acid,
6 parts and 0.3 part benzoyl peroxide of trifluoro propyl methyl cyclotrisiloxane, stirs under 85 DEG C of water bath condition and is condensed back to Stream reaction 3h, then cools to room temperature, reactant is placed on Rotary Evaporators and is spin-dried for solvent to get silicon-fluorine polymer object;
(3) 30 parts of lower sediment particle made from step (1) are distributed to containing 6 parts of lauryl sodium sulfate, carboxymethyl cellulose 4 In part, 8 parts of polyvinyl alcohol of 23 parts of aqueous solutions, 2.5 parts of polysorbas20 is added, step (2) are added while stirring and are made 30 parts of silicon-fluorine polymer object, 6.5 parts of triethanolamine, 9 parts of 2- phosphorus base butane -1,2,4- tricarboxylic acids, 8 parts of maleic anhydride, 2- hydroxyl - 5.5 parts of 4- methoxy benzophenone, 4 parts of octadecyldimethyl ammonium chloride, 10 parts of dimethylaminoethyl acrylate, emulsifier 2.5 parts, 2h is persistently stirred in room temperature, finishing agent A is made;
(4) 15 parts of 23 parts of γ-methacryloxypropyl trimethoxy silane, bleeding agent isopropanols for being added to 40 parts are molten In liquid, 30min is stirred at room temperature, and finishing agent B is made.
The emulsifier is octyl phenol polyoxyethylene ether.
The bleeding agent is Aerosol OT.
Embodiment 2
A kind of preparation method of multifunctional nano finishing agent, comprising the following steps:
(1) by nanoscale TiO2 10 parts, 15 parts of ZnO, 8 parts of Ag, 5 parts of MgO, Al2O3 7 parts are mixed, and grinder is placed in In be ground 15min be made nano-mixture, nano-mixture is then added to 30 part of 10% cetyl trimethyl In the aqueous solution of ammonium bromide, mixing 20min is stirred at room temperature, then places it in ultrasonic disperse 10min in Ultrasound Instrument, then 6 parts of polyethylene glycol-800,7 parts of pentaerythritol stearate are added, continues to be ultrasonically treated 30min at a temperature of 40 DEG C, it will Reactant is cooled to room temperature, and collects lower sediment particle by centrifugation removal solvent;
(2) in reaction flask be added 20 parts of n-butanols be used as organic solvent, then addition 5 parts of ten trifluoro monooctyl ester of methacrylic acid,
4 parts and 0.1 part benzoyl peroxide of trifluoro propyl methyl cyclotrisiloxane, stirs under 80 DEG C of water bath condition and is condensed back to Stream reaction 2h, then cools to room temperature, reactant is placed on Rotary Evaporators and is spin-dried for solvent to get silicon-fluorine polymer object;
(3) 20 parts of lower sediment particle made from step (1) are distributed to containing 4 parts of lauryl sodium sulfate, carboxymethyl cellulose 2 In part, 6 parts of polyvinyl alcohol of 15 parts of aqueous solutions, 1 part of polysorbas20 is added, it is obtained that step (2) are added while stirring 20 parts of silicon-fluorine polymer object, 4 parts of triethanolamine, 6 parts of 2- phosphorus base butane -1,2,4- tricarboxylic acids, 5 parts of maleic anhydride, 2- hydroxyl -4- first 3 parts of oxygroup benzophenone, 2 parts of octadecyldimethyl ammonium chloride, 7 parts of dimethylaminoethyl acrylate, 1 part of emulsifier, in room Temperature persistently stirs 1h, and finishing agent A is made;
(4) 10 parts of 15 parts of γ-methacryloxypropyl trimethoxy silane, bleeding agent isopropanols for being added to 30 parts are molten In liquid, 20min is stirred at room temperature, and finishing agent B is made.
The emulsifier is dodecyl benzyl dimethyl ammonium chloride.
The bleeding agent is mannitol.
Embodiment 3
A kind of preparation method of multifunctional nano finishing agent, comprising the following steps:
(1) by nanoscale TiO2 12 parts, 18 parts of ZnO, 10 parts of Ag, 6 parts of MgO, Al2O3 8 parts are mixed, and grinder is placed in In be ground 15min be made nano-mixture, nano-mixture is then added to 35 part of 15% cetyl trimethyl In the aqueous solution of ammonium bromide, mixing 20-40min is stirred at room temperature, then places it in ultrasonic disperse 12min in Ultrasound Instrument, Then 8 parts of polyethylene glycol-800,8 parts of pentaerythritol stearate are added, continues to be ultrasonically treated at a temperature of 42 DEG C Reactant is cooled to room temperature by 40min, collects lower sediment particle by centrifugation removal solvent;
(2) in reaction flask be added 25 parts of n-butanols be used as organic solvent, then addition 6 parts of ten trifluoro monooctyl ester of methacrylic acid,
5 parts and 0.2 part benzoyl peroxide of trifluoro propyl methyl cyclotrisiloxane, stirs under 82 DEG C of water bath condition and is condensed back to Stream reaction 2.5h, then cools to room temperature, reactant is placed on Rotary Evaporators and is spin-dried for solvent to get silicon-fluorine polymer object;
(3) 25 parts of lower sediment particle made from step (1) are distributed to containing 5 parts of lauryl sodium sulfate, carboxymethyl cellulose 3 In part, 7 parts of polyvinyl alcohol of 20 parts of aqueous solutions, 2 parts of polysorbas20 is added, it is obtained that step (2) are added while stirring 25 parts of silicon-fluorine polymer object, 5 parts of triethanolamine, 8 parts of 2- phosphorus base butane -1,2,4- tricarboxylic acids, 6 parts of maleic anhydride, 2- hydroxyl -4- first 4 parts of oxygroup benzophenone, 3 parts of octadecyldimethyl ammonium chloride, 8 parts of dimethylaminoethyl acrylate, 2 parts of emulsifier, in room Temperature persistently stirs 1.5h, and finishing agent A is made;
(4) 12 parts of 20 parts of γ-methacryloxypropyl trimethoxy silane, bleeding agent isopropanols for being added to 35 parts are molten In liquid, 25min is stirred at room temperature, and finishing agent B is made.
The emulsifier is poly alkyl alcohol oxireme ether.
The bleeding agent is Di-phosphorus pentonide.
Embodiment 4
A kind of preparation method of multifunctional nano finishing agent, comprising the following steps:
(1) by nanoscale TiO2 20 parts, 25 parts of ZnO, 16 parts of Ag, 10 parts of MgO, Al2O3 14 parts are mixed, and grinding is placed in It is ground 15min in machine, nano-mixture is made, nano-mixture is then added to 50 parts of 10-30% cetyls In the aqueous solution of trimethylammonium bromide, mixing 40min is stirred at room temperature, then places it in ultrasonic disperse in Ultrasound Instrument Then 20min adds 13 parts of polyethylene glycol-800,15 parts of pentaerythritol stearate, continue ultrasound at a temperature of 50 DEG C 60min is handled, reactant is cooled to room temperature, lower sediment particle is collected by centrifugation removal solvent;
(2) 40 parts of n-butanols are added in reaction flask as organic solvent, ten trifluoro monooctyl ester 5-10 of methacrylic acid is then added Part,
8 parts and 0.5 part benzoyl peroxide of trifluoro propyl methyl cyclotrisiloxane, is stirred cold under 80-90 DEG C of water bath condition Solidifying back flow reaction 4h, then cools to room temperature, reactant is placed on Rotary Evaporators and is spin-dried for solvent to get silicon-fluorine polymer object;
(3) 40 parts of lower sediment particle made from step (1) are distributed to containing 8 parts of lauryl sodium sulfate, carboxymethyl cellulose 6 In part, 10 parts of polyvinyl alcohol of 30 parts of aqueous solutions, 4 parts of polysorbas20 is added, it is obtained that step (2) are added while stirring 40 parts of silicon-fluorine polymer object, 9 parts of triethanolamine, 12 parts of 2- phosphorus base butane -1,2,4- tricarboxylic acids, 10 parts of maleic anhydride, 2- hydroxyl -4- 8 parts of methoxy benzophenone, 6 parts of octadecyldimethyl ammonium chloride, 13 parts of dimethylaminoethyl acrylate, 4 parts of emulsifier, in Room temperature persistently stirs 3h, and finishing agent A is made;
(4) 20 parts of 30 parts of γ-methacryloxypropyl trimethoxy silane, bleeding agent isopropanols for being added to 50 parts are molten In liquid, 40min is stirred at room temperature, and finishing agent B is made.
The emulsifier is octyl phenol polyoxyethylene ether.
The bleeding agent is Aerosol OT.
Comparative example 1
Comparative example 1 the difference from embodiment 1 is that, unused polyethylene glycol-800 and pentaerythrite are hard in (1) the step of comparative example 1 Resin acid ester is handled.
Comparative example 2
Comparative example 2 the difference from embodiment 1 is that, silicon-fluorine polymer object is not added in comparative example 2.
Fabric after embodiment 1-4, comparative example 1-2 are arranged carries out the test of following performance, test result such as 1 institute of table Show.
(1) it is penetrated using KHF2BP032 type UV resistance and preventing coating protection test macro (SDLAtlas company) measures it and resists Ultraviolet effect, same sample measure 5 times in different location, take its average value;(2) OCA40 type video contact angle measuring instrument is used Contact angle determination is carried out, same sample measures 5 times in different location, takes its average value;(3) creasy recovery angle presses GB 3819- 1997 measurements, every kind of sample are surveyed 5 through 5 latitudes and are averaged, and the creasy recovery angle measured is fabric through returning to the wrinkle with broadwise The sum of multiple angle;(4) finished tensile strength is measured referring to GB 3923.1-1997, and every kind of sample is through 3 times and being averaged to surveying; (5) it is measured using bending resistance length of the pliability analyzer to sample;(6) by fabric made from embodiment 1-4 referring to GB/T 16801-1997 " measurement of fabric conditioner antistatic property ", with the surface of the high insulation measurement instrument measurement fabric of ZC36 type Resistivity and volume resistivity.Obtained from table 1, the fabric UPF value handled through finishing agent of the present invention is up to 128.62, surface with Water contact angle is up to 205.21 °, therefore has good uvioresistant performance and waterproof performance;The crease recovery of processed fabric Angle is up to 324.3 °, and breaking strength retention is up to 95.6%, and therefore, fabric, which is made, in the present invention has excellent wrinkle resistance;Face The surface resistivity of material is down to 4.8 × 106Ω, volume resistivity are down to 2.2 × 106Ω, therefore fabric is with good antistatic Effect.
Table 1

Claims (7)

1. a kind of preparation method of multifunctional nano finishing agent, which comprises the following steps:
(1) by nanoscale TiO2 10-20 parts, 15-25 parts of ZnO, 8-16 parts of Ag, 5-10 parts of MgO, Al2O3 7-14 parts are mixed It closes, is placed in grinder and is ground the obtained nano-mixture of 15min, nano-mixture is then added to 30-50 parts In the aqueous solution of 10-30% cetyl trimethylammonium bromide, mixing 20-40min is stirred at room temperature, then places it in super Then ultrasonic disperse 10-20min on sound instrument adds 6-13 parts of polyethylene glycol-800,7-15 parts of pentaerythritol stearate, in Continue to be ultrasonically treated 30-60min at a temperature of 40-50 DEG C, reactant is cooled to room temperature, under being collected by centrifugation removal solvent Layer precipitating particle;
(2) 20-40 parts of n-butanols are added in reaction flask as organic solvent, ten trifluoro monooctyl ester 5- of methacrylic acid is then added 10 parts,
4-8 parts of trifluoro propyl methyl cyclotrisiloxane and 0.1-0.5 parts of benzoyl peroxides, under 80-90 DEG C of water bath condition Stirring is condensed back reaction 2-4h, then cools to room temperature, reactant is placed on Rotary Evaporators and is spin-dried for solvent to get fluorine silicon Polymer;
(3) 4-8 containing lauryl sodium sulfate parts, carboxymethyl fibre are distributed to by 20-40 parts of lower sediment particle made from step (1) In the 15-30 part aqueous solution for tieing up 2-6 parts of element, 6-10 parts of polyvinyl alcohol, 1-4 parts of polysorbas20 of addition, while stirring plus Enter 20-40 parts of silicon-fluorine polymer object made from step (2), 4-9 parts of triethanolamine, 6-12 parts of 2- phosphorus base butane -1,2,4- tricarboxylic acids, 5-10 parts of maleic anhydride, 3-8 parts of ESCALOL 567,2-6 parts of octadecyldimethyl ammonium chloride, acrylic acid 7-13 parts of dimethylaminoethyl, 1-4 parts of emulsifier, persistently stir 1-3h in room temperature, and finishing agent A is made;
(4) γ -15-30 parts of methacryloxypropyl trimethoxy silane, 10-20 parts of bleeding agent are added to 30-50 parts Aqueous isopropanol in, stir 20-40min at room temperature, be made finishing agent B.
2. a kind of preparation method of multifunctional nano finishing agent according to claim 1, which is characterized in that the step (1) parts by weight of each raw material in are as follows: nanoscale TiO2 15 parts, 20 parts of ZnO, 12 parts of Ag, 8 parts of MgO, Al2O3 10 parts, 40 parts In the aqueous solution of 10-30% cetyl trimethylammonium bromide, 10 parts of polyethylene glycol-800,11 parts of pentaerythritol stearate.
3. a kind of preparation method of multifunctional nano finishing agent according to claim 1, which is characterized in that the step (2) parts by weight of each raw material in are as follows: 30 parts of n-butanol, 7 parts of ten trifluoro monooctyl ester of methacrylic acid, three silicon oxygen of trifluoro propyl methyl ring 6 parts of alkane, 0.3 part of benzoyl peroxide.
4. a kind of preparation method of multifunctional nano finishing agent according to claim 1, which is characterized in that the step (3) parts by weight of each raw material in are as follows: precipitating 30 parts of particle, 6 parts of lauryl sodium sulfate, 4 parts of carboxymethyl cellulose, polyvinyl alcohol 8 parts, 23 parts of aqueous solution, 2.5 parts of polysorbas20,30 parts of silicon-fluorine polymer object, 6.5 parts of triethanolamine, 2- phosphorus base butane -1,2,4- three 9 parts of carboxylic acid, 8 parts of maleic anhydride, 5.5 parts of ESCALOL 567,4 parts of octadecyldimethyl ammonium chloride, propylene 10 parts of sour dimethylaminoethyl, 2.5 parts of emulsifier.
5. a kind of preparation method of multifunctional nano finishing agent according to claim 1, which is characterized in that the step (4) parts by weight of each raw material in are as follows: 23 parts of γ-methacryloxypropyl trimethoxy silane, 15 parts of bleeding agent, isopropanol 40 parts.
6. a kind of preparation method of multifunctional nano finishing agent according to claim 1, which is characterized in that the emulsification Agent is one of octyl phenol polyoxyethylene ether, dodecyl benzyl dimethyl ammonium chloride or poly alkyl alcohol oxireme ether.
7. a kind of preparation method of multifunctional nano finishing agent according to claim 1, which is characterized in that the infiltration Agent is one kind of Aerosol OT, mannitol or Di-phosphorus pentonide.
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Application publication date: 20181207