CN106700659A - Preparation method for light-curing super-hydrophobic composite structural nano-silicon dioxide - Google Patents

Preparation method for light-curing super-hydrophobic composite structural nano-silicon dioxide Download PDF

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Publication number
CN106700659A
CN106700659A CN201611064000.3A CN201611064000A CN106700659A CN 106700659 A CN106700659 A CN 106700659A CN 201611064000 A CN201611064000 A CN 201611064000A CN 106700659 A CN106700659 A CN 106700659A
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China
Prior art keywords
silicon dioxide
super
preparation
light
nano silicon
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CN201611064000.3A
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姚伯龙
孙常青
李洪萍
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Jiangnan University
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Jiangnan University
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    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/28—Compounds of silicon
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/12—Treatment with organosilicon compounds
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/90—Other properties not specified above

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Silicon Polymers (AREA)

Abstract

The invention relates to a preparation method for light-curing super-hydrophobic composite structural nano-silicon dioxide. The preparation method comprises the following steps: dispersing nano-silicon dioxide with different particle sizes in absolute ethyl alcohol; reacting with different silane coupling agents and fluorine-containing siloxane for four hours to obtain two products under 50 DEG C heating and stirring and acidic conditions; washing the products, drying and re-dispersing; dropping a small-particle size dispersing liquid into a large-particle size dispersing liquid with stirring at normal temperature, and reacting for three hours to obtain the light-curing super-hydrophobic composite structural nano-silicon dioxide. The surfaces of particles prepared by the preparation method are of nano-scale slightly convex structures, and have fluorine-containing chain segments and double-bond groups, so that the particles have excellent super-hydrophobic characteristic and light curing characteristic; the using stability of the particles can be effectively enhanced when the particles are applied to the field of light-curing materials.

Description

A kind of preparation method of photocuring super-hydrophobic composite construction nano silicon
Technical field
The present invention relates to a kind of preparation method of photocuring super-hydrophobic composite construction nano silicon, belong to feature Field of nanometer material technology.
Background introduction
Nano silicon is a kind of widely used inorganic chemical industry material, due to its UV resistant and can improve other materials The performances such as the anti-aging of material, intensity and chemically-resistant, therefore have the application of uniqueness in fields such as coating.To nano-silicon dioxide particle Carry out surface modified, grafting functional group makes its obtain specific function, and as the material modified matrix material such as with resin Material is compound, the excellent modified multifunctional material of availability.Using nanometer grade silica, silane coupler, fluorine-containing silica Modified manometer silicon dioxide obtained in the monomers such as alkane is keeping the same of nano silicon characteristic compared with general silica When, with excellent ultra-hydrophobicity, and a large amount of double bonds being connected in particle surface, can effectively add when being applied to photo-curing material The stability of strong nano-particle, has a good application prospect in photo-curing material field.
The content of the invention
The present invention relates to a kind of preparation method of photocuring super-hydrophobic composite construction nano silicon, its object is to There is provided a kind of utilization nanometer grade silica, silane coupler, flucride siloxane modified synthesis with photocuring and super-hydrophobic The composite construction nano silicon of characteristic.In the nano-particle, composite construction causes that particle surface has nanoscale dimpling Structure, while modified monomer makes particle surface have a large amount of fluorine-containing groupses and double bond group, makes modified manometer silicon dioxide particle Possess excellent superhydrophobic characteristic and photocuring characteristic, the steady of particle can be effectively strengthened when photo-curing material field is applied to It is qualitative.
The technical scheme is that：
The preparation method of photocuring super-hydrophobic composite construction nano silicon, comprises the following steps：
(1) nano silicon of the different-grain diameter of metering is respectively placed in the there-necked flask of dried and clean, adds 150 The absolute ethyl alcohol of times quality, ultrasound makes nano silicon uniformly be scattered in absolute ethyl alcohol；
(2) scattered solution is respectively placed in 50 DEG C of water-baths, respectively add identical metering through acetic acid or other acid The acid water (pH value range is 4~5) of class regulation, stirs 10min；
(3) added in big particle diameter system metering containing amino silicane coupling agent and flucride siloxane, lasting stirring, altogether Reaction 4h；In small particle system add metering containing epoxy silane coupling and group containing double bond silane coupler, continue Stirring, reacts 4h altogether；
(4) after first stage reaction terminates, wash respectively, dry obtained different-grain diameter modified manometer silicon dioxide grain Son, and be scattered in absolute ethyl alcohol again respectively；
(5) big particle diameter modified manometer silicon dioxide alcohol dispersion liquid is placed in the there-necked flask of dried and clean, under normal temperature Stirring, small particle modified manometer silicon dioxide alcohol dispersion liquid is added dropwise with dropping funel with the speed that 2s often drips, and reacts 3h, reaction Washed after end, dried, the photocuring super-hydrophobic composite construction nano silicon for being designed.
Specific embodiment
Embodiment 1
By 1.5g SiO2(300nm), 225g absolute ethyl alcohols and 1g SiO2(30nm), 150g absolute ethyl alcohols are separately added into two In individual clean there-necked flask, ultrasonic 0.5h is uniformly dispersed, and dispersion liquid is placed in 50 DEG C of thermostat water baths respectively, accesses stirring Device, it is each to add 5ml acid waters, stir 10min；
To 0.15g Kh550 are added in 300nm dispersions, 0.5h is reacted, continuously add 0.15g FAS-17, reacted 3.5h；
To 0.1g Kh560 are added in 30nm dispersions, 0.5h is reacted, continuously add 0.1g Kh570, react 3.5h；
The two kinds of samples that will be prepared are washed, dried, and are scattered in absolute ethyl alcohol again, by 300nm SiO2Ethanol disperses Liquid is placed in dry, clean there-necked flask, is stirred under normal temperature, and 30nm SiO are added dropwise with the speed that 2s often drips with dropping funel2 Alcohol dispersion liquid, reacts 3h, and reaction is washed after terminating, dried, and obtains final product the photocuring super-hydrophobic composite construction nanometer two of design Silica.

Claims (2)

1. a kind of preparation method of photocuring super-hydrophobic composite construction nano silicon, its characterization step is：
(1) nano silicon of the different-grain diameter of metering is respectively placed in the there-necked flask of dried and clean, adds 150 times of matter The absolute ethyl alcohol of amount, ultrasound makes nano silicon uniformly be scattered in absolute ethyl alcohol；
(2) scattered solution is respectively placed in 50 DEG C of water-baths, respectively adds being adjusted through acetic acid or other acids for identical metering The acid water (pH value range is 4~5) of section, stirs 10min；
(3) added in big particle diameter system metering containing amino silicane coupling agent and flucride siloxane, lasting stirring is reacted altogether 4h；Added in small particle system metering containing epoxy silane coupling and group containing double bond silane coupler, lasting stirring, 4h is reacted altogether；
(4) after first stage reaction terminates, wash respectively, dry obtained different-grain diameter modified manometer silicon dioxide particle, and It is scattered in absolute ethyl alcohol again respectively；
(5) big particle diameter modified manometer silicon dioxide alcohol dispersion liquid is placed in the there-necked flask of dried and clean, is stirred under normal temperature, Small particle modified manometer silicon dioxide alcohol dispersion liquid is added dropwise with the speed that 2s often drips with dropping funel, 3h is reacted, reaction terminates Wash afterwards, dry, the photocuring super-hydrophobic composite construction nano silicon for being designed.
2. a kind of preparation method of photocuring super-hydrophobic composite construction nano silicon as claimed in claim 1, it is special Levy and be：Nano silicon described in step (1) is aerosil, hydrolysis silica, silica ethanol point At least one in dispersion liquid；
Silane coupler described in step (3) include it is all containing amino, epoxy radicals, double bond group silane coupler, it is fluorine-containing Siloxanes includes silicon fluoride complete series hydrolyzable monomer.
CN201611064000.3A 2016-11-28 2016-11-28 Preparation method for light-curing super-hydrophobic composite structural nano-silicon dioxide Pending CN106700659A (en)

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Application Number Priority Date Filing Date Title
CN201611064000.3A CN106700659A (en) 2016-11-28 2016-11-28 Preparation method for light-curing super-hydrophobic composite structural nano-silicon dioxide

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109505142A (en) * 2018-11-01 2019-03-22 佛山市南海区里水镇经济促进局 The hydrophobic oleophobic method for preparing antibiotic coating on textile material surface
CN112608068A (en) * 2020-12-30 2021-04-06 江南大学 Preparation method of antifouling self-cleaning water-based architectural coating by recycling waste paint residues
CN113088123A (en) * 2021-04-02 2021-07-09 广东工业大学 Micro-nano composite SiO2Particle, micro-nano composite structure super-hydrophobic coating, preparation method and application thereof

Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1887972A (en) * 2006-07-14 2007-01-03 浙江大学 Nanometer SiO2 modifying process of ultraviolet ray cured adhesive
CN101880478A (en) * 2010-06-17 2010-11-10 华南理工大学 Method for preparing hydrophobic nano-silica with controllable grain diameter
CN102675941A (en) * 2012-05-29 2012-09-19 江门亿源生化工程有限公司 Ultraviolet (UV) curable super-hydrophobic anti-fingerprint coating and preparation method thereof
CN102911530A (en) * 2012-11-07 2013-02-06 北京化工大学 Preparation method capable of realizing chemical blending of modified nano silicon dioxide particles in acrylate monomer
CN103224719A (en) * 2013-02-04 2013-07-31 湖北大学 Fluorosilicone material for super-hydrophobic coating and its preparation method and use method
CN103936996A (en) * 2014-04-14 2014-07-23 茂名市信龙科技有限公司 Synthesis of photo-cured fluorosilicone polymer and preparation method of photo-cured fluorosilicone polymer coating
CN104988728A (en) * 2015-07-30 2015-10-21 江南大学 Method for modifying fabric by UV light-cured responsive sol
CN105820287A (en) * 2016-04-14 2016-08-03 西南科技大学 Preparation method of solvent-based brittle self-peeling radioactive detergent

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1887972A (en) * 2006-07-14 2007-01-03 浙江大学 Nanometer SiO2 modifying process of ultraviolet ray cured adhesive
CN101880478A (en) * 2010-06-17 2010-11-10 华南理工大学 Method for preparing hydrophobic nano-silica with controllable grain diameter
CN102675941A (en) * 2012-05-29 2012-09-19 江门亿源生化工程有限公司 Ultraviolet (UV) curable super-hydrophobic anti-fingerprint coating and preparation method thereof
CN102911530A (en) * 2012-11-07 2013-02-06 北京化工大学 Preparation method capable of realizing chemical blending of modified nano silicon dioxide particles in acrylate monomer
CN103224719A (en) * 2013-02-04 2013-07-31 湖北大学 Fluorosilicone material for super-hydrophobic coating and its preparation method and use method
CN103936996A (en) * 2014-04-14 2014-07-23 茂名市信龙科技有限公司 Synthesis of photo-cured fluorosilicone polymer and preparation method of photo-cured fluorosilicone polymer coating
CN104988728A (en) * 2015-07-30 2015-10-21 江南大学 Method for modifying fabric by UV light-cured responsive sol
CN105820287A (en) * 2016-04-14 2016-08-03 西南科技大学 Preparation method of solvent-based brittle self-peeling radioactive detergent

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109505142A (en) * 2018-11-01 2019-03-22 佛山市南海区里水镇经济促进局 The hydrophobic oleophobic method for preparing antibiotic coating on textile material surface
CN112608068A (en) * 2020-12-30 2021-04-06 江南大学 Preparation method of antifouling self-cleaning water-based architectural coating by recycling waste paint residues
CN113088123A (en) * 2021-04-02 2021-07-09 广东工业大学 Micro-nano composite SiO2Particle, micro-nano composite structure super-hydrophobic coating, preparation method and application thereof

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