CN108085996A - A kind of photochromic micro-encapsulation hybrid modification silicon dioxide gel coated fabric and preparation method thereof - Google Patents
A kind of photochromic micro-encapsulation hybrid modification silicon dioxide gel coated fabric and preparation method thereof Download PDFInfo
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- CN108085996A CN108085996A CN201711421306.4A CN201711421306A CN108085996A CN 108085996 A CN108085996 A CN 108085996A CN 201711421306 A CN201711421306 A CN 201711421306A CN 108085996 A CN108085996 A CN 108085996A
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M23/00—Treatment of fibres, threads, yarns, fabrics or fibrous goods made from such materials, characterised by the process
- D06M23/12—Processes in which the treating agent is incorporated in microcapsules
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K9/00—Tenebrescent materials, i.e. materials for which the range of wavelengths for energy absorption is changed as a result of excitation by some form of energy
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/77—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with silicon or compounds thereof
- D06M11/79—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with silicon or compounds thereof with silicon dioxide, silicic acids or their salts
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/01—Treating 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
- D06M15/03—Polysaccharides or derivatives thereof
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/564—Polyureas, polyurethanes or other polymers having ureide or urethane links; Precondensation products forming them
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
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- D06M16/00—Biochemical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. enzymatic
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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
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- C09K2211/00—Chemical nature of organic luminescent or tenebrescent compounds
- C09K2211/14—Macromolecular compounds
- C09K2211/1441—Heterocyclic
- C09K2211/145—Heterocyclic containing oxygen as the only heteroatom
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- D—TEXTILES; PAPER
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- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/02—Natural fibres, other than mineral fibres
- D06M2101/04—Vegetal fibres
- D06M2101/06—Vegetal fibres cellulosic
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- D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
- D06M2200/10—Repellency against liquids
- D06M2200/11—Oleophobic properties
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- D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
- D06M2200/10—Repellency against liquids
- D06M2200/12—Hydrophobic properties
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- 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
- D06M2200/20—Treatment influencing the crease behaviour, the wrinkle resistance, the crease recovery or the ironing ease
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- 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
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
- D06M2200/50—Modified hand or grip properties; Softening compositions
Abstract
A kind of photochromic micro-encapsulation hybrid modification silicon dioxide gel coated fabric and preparation method thereof, it is related to a kind of coated fabric and preparation method thereof.Present invention aim to address existing photochromic micro-encapsulations directly as dyeing or printing the problem of colored textile friction fastness is good, washing fastness is not good enough, Boardy Feeling, photochemistry sun-resistant fatigue strength difference and service life are short on coated fabric.A kind of photochromic micro-encapsulation hybrid modification silicon dioxide gel coated fabric is made of hydrophobic modified silicon dioxide gel and photochromic micro-encapsulation；Preparation method：Photochromic micro-encapsulation is added in container, hydrophobic modified silicon dioxide gel is then added in, is stirred to react to obtain photochromic micro-encapsulation hybrid modification silicon dioxide gel coated fabric.Advantage：There can also be photochromic functional effect while water repellent effect can be reached.Present invention is mainly used for prepare photochromic micro-encapsulation hybrid modification silicon dioxide gel coated fabric.
Description
Technical field
The present invention relates to a kind of coated fabrics and preparation method thereof.
Background technology
In recent years, the photochromic dyes for directly applying to weaving category is few, mainly fastness to light is undesirable, color
Change resume speed is slow, dyestuff higher price, and stability and Reusability are poor, high temperature resistance difference etc..So nowadays compel
It cuts and wants to develop novel durable and aberration is apparent, high temperature resistant, the excellent photochromic compound such as fast light.Therefore compared with
Difficulty is processed by conventional dyeing and printing technique, not high to fiber affinity, disperses to gather by chromotropic dye in melt spinning method
It closes in object, microstructure and performance is influenced by polymer molecule, therefore reply fiber microstructure and type of polymer are controlled by
And selection, it is also limited by spinning condition, photochromic dyes is applied in a manner of microcapsules mostly, but price, fast light
Its commercialization, is still there is certain difficulty by the influence of the factors such as fastness and dye stability.It is prepared by existing photochromic micro-encapsulation
Mill base directly to the textile of fabric coating or stamp due to be between photochromic micro-encapsulation and fabric by thickener and
Adhesive combines on the textile, is combined by adhesive between them, so its crock fastness, washing fastness be not good enough, light-induced variable
Color microcapsules easily peel off.Further, since thickener and adhesive in mill base uses the textile for causing coating or stamp
Feel is not good enough, not soft enough.
The content of the invention
Present invention aim to address existing photochromic micro-encapsulations directly as dyeing or printing colored weaving on coated fabric
The problem of product crock fastness is good, washing fastness is not good enough, Boardy Feeling, short photochemistry sun-resistant fatigue strength difference and service life, and one
Kind photochromic micro-encapsulation hybrid modification silicon dioxide gel coated fabric and preparation method thereof.
A kind of photochromic micro-encapsulation hybrid modification silicon dioxide gel coated fabric, it is by hydrophobic modified silica
Colloidal sol and photochromic micro-encapsulation are made, and the mass ratio of the hydrophobic modified silicon dioxide gel and photochromic micro-encapsulation is
(30~35):1；The photochromic micro-encapsulation is bivalve polyurethane-chitosan photochromic micro-encapsulation.
A kind of preparation method of photochromic micro-encapsulation hybrid modification silicon dioxide gel coated fabric, specifically by following
What step was completed：
Photochromic micro-encapsulation is added in container, then adds in hydrophobic modified silicon dioxide gel, is 24 in temperature
Magnetic agitation reacts 5min~20min under the conditions of~40 DEG C, obtains the painting of photochromic micro-encapsulation hybrid modification silicon dioxide gel
Layer fabric；The mass ratio of the hydrophobic modified silicon dioxide gel and photochromic micro-encapsulation is (30~35):1；Described
Photochromic micro-encapsulation is bivalve polyurethane-chitosan photochromic micro-encapsulation.
Advantage of the present invention：
First, photochromic micro-encapsulation is made using hydrophobic modified silicon dioxide gel and photochromic micro-encapsulation in the present invention
Hybrid modification silicon dioxide gel coated fabric, the photochromic micro-encapsulation hybrid modification silicon dioxide gel coated fabric is in energy
There can also be photochromic functional effect while enough reaching water repellent effect, and the modification sol after hydridization can be stablized and deposit
, paint excellent effect, fabric it is highly practical and can band give good snugness of fit.
2nd, the hydrophobic modified silicon dioxide gel that uses of the present invention by centrifugal stability the result shows that, stability compared with
It is good, substantive influence will not be generated to hybrid modification colloidal sol.And the distribution uniform of hydrophobic modified silicon dioxide gel, knot
Without layered structure in structure.Thermal gravimetric analyzer test result shows that hydrophobic modified stability of silica sol is excellent.
Weight loss is 70% or so at 120 DEG C, and weight loss is 79% when temperature is 698 DEG C, is primarily due to remaining solvent
The result of polymerization dehydration between Si-OH groups in the molecular structure of volatilization and hydrophobic modified silicon dioxide gel.
3rd, absorbance test result shows photochromic micro-encapsulation hybrid modification silicon dioxide gel prepared by the present invention
Coated fabric relatively saves raw material compared with other dyestuffs of same amount, above dyes the fabric that color is relatively deep and stablizes.
4th, contact angle test result shows photochromic micro-encapsulation hybrid modification silicon dioxide gel prepared by the present invention
Contact angle of the coated fabric after textile finishing can reach 133 °.
5th, fabric seepage of water and the test result of wicking properties show photochromic micro-encapsulation hydridization prepared by the present invention
The modified silicon dioxide sol coated fabric water-column that resistance to hydrostatic pressure is tested after textile finishing is 470mm and Plug design
It can be in 30min without wicking.
6th, Air permenbility, vapor transfer rate test result show that coating photochromic micro-encapsulation hybrid modification silicon dioxide gel applies
The vapor transfer rate of the dress ornament class of layer fabric reaches 149L/m2S, Air permenbility reach 168L/m2S, thus the present invention prepare it is photic
Discoloration microcapsules hybrid modification silicon dioxide gel coated fabric also is adapted in terms of applying to dress ornament, simultaneously as good
Gas, penetrability, which can also give people to bring, comfortable wears condition.
7th, the test result of crease recovery and ultimate strength shows photochromic micro-encapsulation hydridization prepared by the present invention
Modified silicon dioxide sol coated fabric is arranged in that can reach daily demand on fabric, disclosure satisfy that people wear dress ornament class
Condition.
8th, the absorbance performance of photochromic micro-encapsulation hybrid modification silicon dioxide gel coated fabric improves, and is organized in
After on fabric, fabric has good photoresponse discoloration and thermal stability, and Washing can reach 2~3 grades, and rub
Fastness can reach 4 grades.
Specific embodiment
Specific embodiment one：Present embodiment is a kind of photochromic micro-encapsulation hybrid modification silicon dioxide gel coating
Fabric, it is made of hydrophobic modified silicon dioxide gel and photochromic micro-encapsulation, and the hydrophobic modified silica is molten
The mass ratio of glue and photochromic micro-encapsulation is (30~35):1；The photochromic micro-encapsulation gathers for bivalve polyurethane-shell
Sugared photochromic micro-encapsulation.
Photochromic micro-encapsulation hybrid modification silicon dioxide gel coated fabric is knitted with other photochromic micro-encapsulation coatings
Object is compared, and in addition to photochromic properties, also with super-hydrophobic performance and antifouling property, is imparted textile and is answered
Close function.Mill base, which is made, in double-shell microcapsule photochromic dyes again, which carries out top finish, can improve its resistance extraneous factor
Ability, photochemistry endurance after the multiple reciprocal irradiation or chronic exposure as caused by influencing pH, solvent, oxidation and temperature
The problem of degree is deteriorated, and discoloration is caused to fail, and reversible color function life-span shortens.The photochromic chemical combination of unencapsulated azo
Object, since UV-Vis light sources direct irradiation is on azo photochromic compound surface, azo photochromic compound can be most
Limits receive light radiation.For bivalve polyurethane-chitosan photochromic micro-encapsulation, because its surface coated two layers it is transparent
And mirror-reflection and diffusing reflection has occurred in the wall shell of surface imperfection, cyst wall surface, the refraction of light, shell also has occurred in double wall shell
Body also absorbs part light in itself, i.e., the physical phenomenon being equally happened on polyurethane monoshell microcapsules has then carried out twice, therefore
The light that the azo photochromic compound of cladding receives inside bivalve polyurethane-chitosan photochromic micro-encapsulation irradiates strong
Degree will be less than the irradiation intensity that azo photochromic compound receives inside polyurethane monoshell microcapsules, more below unencapsulated
Azo photochromic compound.
Mill base prepared by existing photochromic micro-encapsulation directly carries out light-induced variable used in coating or stamp to fabric
Color microcapsules are monoshell microcapsules.Therefore the azo light-induced variable coated inside bivalve polyurethane-chitosan photochromic micro-encapsulation
The intensity for the light irradiation that color compound receives will be less than azo photochromic compound inside polyurethane monoshell microcapsules and receive
The irradiation intensity arrived, more below unencapsulated azo photochromic compound, monoshell microcapsules exist to photochromic compound
It is not so good as bivalve polyurethane-chitosan photochromic micro-encapsulation, therefore this implementation in terms of improving sun-resistant fatigue strength and service life
Mode selects bivalve polyurethane-chitosan photochromic micro-encapsulation.
Colloidal sol, will by hydridization into modified material nano-oxide film that fabric surface is formed is transparent, adhesiveness is strong
Modified material is transferred on textile so as to fulfill the functionality of textile.Directly make to solve existing photochromic micro-encapsulation
To be dyed or printed on coated fabric, colored textile friction fastness is good, washing fastness is not good enough, Boardy Feeling, the sun-resistant fatigue strength of photochemistry
The problem of difference and service life are short, present invention discover that photochromic micro-encapsulation and colloidal sol hybrid modification, whole to improve color-changeable fabric
Color and fastness properties；One stable polymorphic system etc. can be formed by the combination of two kinds of photochromic compounds, this
The kind more superior photochromic material of performance will have very vast potential for future development.Therefore the present invention carries out colloidal sol deep
Research.
It is existing generally to use ethyl orthosilicate (TEOS) as presoma, by Stober methods or using hydrochloric acid as catalyst
Make TEOS polymerization hydrolysis and formed silicon dioxide gel.Due to the surface of hydrophilic and oleophobic silica, it is difficult to organic
Disperse in medium and infiltrate, if being directly filled into institute's sorted material, it is difficult to play its effect, silica applies model
It encloses and is just limited.Therefore, there is very important meaning to the modification of silica particle surface.Silica surface
Modifying agent is connected, it is made to be changed into hydrophobic oleophilic oil by hydrophilic and oleophobic, at the same time can increase the steric hindrance between silicon oxide particle,
Make it preferably to be dispersed in organic media, so as to enhance the intermiscibility of organic dispersion medium and silica, reach improvement
The performance of silica.Due on the surface of silica there are more each other with Hydrogenbond hydroxyl, electronegative atom
Isolated hydrogen atom absorption easily strong with electropositive easily generates dehydration condensation with the compound containing hydroxyl, with epoxide
Esterification is generated, is reacted with phosgene or thionyl chloride.The presence of surface hydroxyl makes sol surface possess chemical adsorptivity, meets
Hydrogen Binding Adsorption is easily formed during hydrone.Therefore it is sol surface hydroxyl and hydroxyl chemical combination to silica modified basic principle
Object easily reacts, the characteristic of easy adsorpting anion.Based on this, the present invention is modified silicon dioxide gel, obtains hydrophobicity
Then modified silicon dioxide sol hydrophobic modified silicon dioxide gel is made with photochromic micro-encapsulation photic photochromic
Microcapsules hybrid modification silicon dioxide gel coated fabric knits photochromic micro-encapsulation hybrid modification silicon dioxide gel coating
Colored textile is dyed or printed on object, compared with mill base coating prepared by photochromic micro-encapsulation, through photic photochromic micro-encapsulation
The fiber surface that hybrid modification silicon dioxide gel coated fabric is handled well is covered with continuous film, the original groove structure of fiber
It disappears, fabric contact angle reaches 133 °, and the fabric contact angle after mill base top finish prepared by photochromic micro-encapsulation is only
42°.The absorbance performance of photochromic micro-encapsulation hybrid modification silicon dioxide gel coated fabric improves, and arranges on the fabric
Afterwards, fabric has good photoresponse discoloration and thermal stability, and Washing can reach 2~3 grades, and crock fastness energy
Enough reach 4 grades.When the object of top finish is all pure cotton fabric, twills need 10.2s when reaching discoloration stable state,
Plain cloth needs 10.6s；The fabric of photochromic micro-encapsulation mill base top finish, when reaching discoloration stable state, twill weave
Object needs 10.5s, and plain cloth needs 10.9s.Twill structure assigns more efficient lasting photoresponse discolouration than plain weave structure
Can, faster, photochromic properties improve for discoloration.What photochromic micro-encapsulation hybrid modification silicon dioxide gel coated fabric arranged
Pure cotton fabric changes colour faster than the pure cotton fabric of photochromic micro-encapsulation mill base top finish, and photochromic properties improve.It will be even
It is fairly good can so that azo-compound microcapsules are shown in the sealed environment of nitrogen photochromic compound progress bivalve cladding
Ability of reverse photochromism performance, the optical switch of photoresponse can be repeated multiple times, azo photochromic compound is coated on double
In the sealed environment of shell cladding its photosensitive colour-changing reversibility is enabled to enhance, and without apparent fatigue strength or " photic
Decline " influences.In the case where the ultraviolet-visible photoperiod irradiates repeatedly, until reach the 37th time it is reversible change colour repeatedly when, it is photochromic micro-
The variation that the pure cotton fabric absorbance that capsule hybrid modification silicon dioxide gel coated fabric arranges just is reduced, it is photochromic micro-
The pure cotton fabric of capsule mill base top finish be the 19th time it is reversible change colour repeatedly when, variation that absorbance is reduced.
Hydridization arrangement is modified under the low viscosity state of 156.73mPas to fabric, characterizes the K/S values of dyed color performance depth
Reach 2.73, red green tone pitch a* is partially red for 9.216, and champac tone pitch b* is partially blue for -19.44, according to three primary colors color theory, at this time
It is deep that the light of cotton fabric becomes purple effect.
Specific embodiment two：The difference of present embodiment and specific embodiment one is：Described hydrophobic modified two
The preparation process of silica sol is as follows：
Silicon dioxide gel is added in container, then adds in modifying agent, then catalyst is added dropwise, sealing container, in water-bath
Temperature is that magnetic agitation reacts 1.5h~2.5h at 40 DEG C, obtains hydrophobic modified silicon dioxide gel；The silica is molten
The volume ratio of glue and modifying agent is (30~50):1；The volume ratio of the silicon dioxide gel and catalyst is (200~300):
1。
Other are same as the specific embodiment one.
Specific embodiment three：The difference of present embodiment and specific embodiment two is：The modifying agent is ethylene
Base trimethoxy silane；The catalyst is dibutyl tin laurate.Other are identical with embodiment two.
Specific embodiment four：Present embodiment is with one of specific embodiment two or three difference：The titanium dioxide
The preparation process of Ludox is as follows：
First, ethyl orthosilicate with absolute ethyl alcohol under air-proof condition is uniformly mixed, obtains mixed liquor；The positive silicic acid second
The volume ratio of ester and absolute ethyl alcohol is 1:(1~1.6)；2nd, the hydrochloric acid that mass fraction is 27% is added in deionized water, obtained
Dilute hydrochloric acid, the hydrochloric acid that the mass fraction is 27% are 1 with entering deionized water volume ratio:(1~44)；3rd, it is 60 DEG C in temperature
It is added dropwise dilute hydrochloric acid under constant temperature water bath condition of heating and stirring into mixed liquor, the volume ratio of the dilute hydrochloric acid and mixed liquor is 1:
(6~8), are then stirred to react 1.5h~2.5h in the case where temperature is 60 DEG C of constant temperature water bath condition of heating and stirring, initial reaction object, so
After add in n,N-Dimethylformamide, the volume ratio of the n,N-Dimethylformamide and initial reaction object is (3~4.5):10,
12h~for 24 hours is stood after stirring and evenly mixing at room temperature, obtains silicon dioxide gel.
Other are identical with specific embodiment two or three.
Specific embodiment five：Present embodiment is a kind of photochromic micro-encapsulation hybrid modification silicon dioxide gel coating
The preparation method of fabric, is specifically realized by the following steps：
Photochromic micro-encapsulation is added in container, then adds in hydrophobic modified silicon dioxide gel, is 24 in temperature
Magnetic agitation reacts 5min~20min under the conditions of~40 DEG C, obtains the painting of photochromic micro-encapsulation hybrid modification silicon dioxide gel
Layer fabric；The mass ratio of the hydrophobic modified silicon dioxide gel and photochromic micro-encapsulation is (30~35):1；Described
Photochromic micro-encapsulation is bivalve polyurethane-chitosan photochromic micro-encapsulation.
Specific embodiment six：The difference of present embodiment and specific embodiment five is：Described hydrophobic modified two
The preparation process of silica sol is as follows：
Silicon dioxide gel is added in container, then adds in modifying agent, then catalyst is added dropwise, sealing container, in water-bath
Temperature is that magnetic agitation reacts 1.5h~2.5h at 40 DEG C, obtains hydrophobic modified silicon dioxide gel；The silica is molten
The volume ratio of glue and modifying agent is (30~50):1；The volume ratio of the silicon dioxide gel and catalyst is (200~300):
1。
Other are identical with specific embodiment five.
Specific embodiment seven：The difference of present embodiment and specific embodiment six is：The modifying agent is ethylene
Base trimethoxy silane；The catalyst is dibutyl tin laurate.Other are identical with specific embodiment six.
Specific embodiment eight：Present embodiment is with one of specific embodiment six or seven difference：The titanium dioxide
The preparation process of Ludox is as follows：
First, ethyl orthosilicate with absolute ethyl alcohol under air-proof condition is uniformly mixed, obtains mixed liquor；The positive silicic acid second
The volume ratio of ester and absolute ethyl alcohol is 1:(1~1.6)；2nd, the hydrochloric acid that mass fraction is 27% is added in deionized water, obtained
Dilute hydrochloric acid, the hydrochloric acid that the mass fraction is 27% are 1 with entering deionized water volume ratio:(1~44)；3rd, it is 60 DEG C in temperature
It is added dropwise dilute hydrochloric acid under constant temperature water bath condition of heating and stirring into mixed liquor, the volume ratio of the dilute hydrochloric acid and mixed liquor is 1:
(6~8), are then stirred to react 1.5h~2.5h in the case where temperature is 60 DEG C of constant temperature water bath condition of heating and stirring, initial reaction object, so
After add in n,N-Dimethylformamide, the volume ratio of the n,N-Dimethylformamide and initial reaction object is (3~4.5):10,
12h~for 24 hours is stood after stirring and evenly mixing at room temperature, obtains silicon dioxide gel.
Other are identical with specific embodiment six or seven.
Using following verification experimental verifications effect of the present invention
Embodiment 1：A kind of preparation method of photochromic micro-encapsulation hybrid modification silicon dioxide gel coated fabric, specifically
It completes according to the following steps：
0.3g photochromic micro-encapsulations are added in container, the hydrophobic modified silicon dioxide gels of 10g are then added in, in temperature
It spends and reacts 5min for magnetic agitation under the conditions of 40 DEG C, obtain photochromic micro-encapsulation hybrid modification silicon dioxide gel coating and knit
Object；The photochromic micro-encapsulation is bivalve polyurethane-chitosan photochromic micro-encapsulation.
The preparation process of hydrophobic modified silicon dioxide gel is as follows described in the present embodiment：
40mL silicon dioxide gels are added in container, then add in 1.12mL modifying agent, then 0.15mL catalyst is added dropwise,
Sealing container, in the case where bath temperature is 40 DEG C, magnetic agitation reacts 2h, obtains hydrophobic modified silicon dioxide gel；The modification
Agent is vinyltrimethoxysilane；The catalyst is dibutyl tin laurate；The preparation of the silicon dioxide gel
Journey is as follows：
First, 22.2575mL ethyl orthosilicates with 22.132mL absolute ethyl alcohols under air-proof condition are uniformly mixed, are mixed
Close liquid；2nd, the hydrochloric acid that 0.2626mL mass fractions are 27% is added in 11.52mL deionized waters, obtains dilute hydrochloric acid,；3rd, exist
Temperature is to be added dropwise what step 2 obtained in the mixed liquor obtained under 60 DEG C of constant temperature water bath condition of heating and stirring into step 1
Then dilute hydrochloric acid is stirred to react 2h in the case where temperature is 60 DEG C of constant temperature water bath condition of heating and stirring, then initial reaction object adds in N,
The volume ratio of dinethylformamide, the n,N-Dimethylformamide and initial reaction object is 3:10, in room after stirring and evenly mixing
Temperature is lower to stand 12h, obtains silicon dioxide gel.
Photochromic micro-encapsulation hybrid modification silicon dioxide gel coated fabric manufactured in the present embodiment weight at 120 DEG C
It loses as 68.1%, weight loss is 79% when temperature is 698 DEG C.
Photochromic micro-encapsulation hybrid modification silicon dioxide gel coated fabric manufactured in the present embodiment is after textile finishing
Contact angle can reach 133 °；The fabric is plain weave pure cotton fabric.
Photochromic micro-encapsulation hybrid modification silicon dioxide gel coated fabric manufactured in the present embodiment is after textile finishing
Resistance to hydrostatic pressure test water-column for 470mm and wicking properties in 30min without wicking；The fabric is flat
Line pure cotton fabric.
Photochromic micro-encapsulation hybrid modification silicon dioxide gel coated fabric manufactured in the present embodiment arranges on the fabric
Afterwards, fabric has good photoresponse discoloration and thermal stability, and Washing can reach 3 grades, and crock fastness can
Reach 4 grades；The fabric is plain weave pure cotton fabric.
Claims (8)
1. a kind of photochromic micro-encapsulation hybrid modification silicon dioxide gel coated fabric, it is characterised in that a kind of photochromic micro-
Capsule hybrid modification silicon dioxide gel coated fabric is made of hydrophobic modified silicon dioxide gel and photochromic micro-encapsulation,
The mass ratio of the hydrophobic modified silicon dioxide gel and photochromic micro-encapsulation is (30~35):1；Described is photochromic
Microcapsules are bivalve polyurethane-chitosan photochromic micro-encapsulation.
2. a kind of photochromic micro-encapsulation hybrid modification silicon dioxide gel coated fabric according to claim 1, special
Sign is that the preparation process of the hydrophobic modified silicon dioxide gel is as follows：
Silicon dioxide gel is added in container, then adds in modifying agent, then catalyst is added dropwise, sealing container, in bath temperature
1.5h~2.5h is reacted for magnetic agitation at 40 DEG C, obtains hydrophobic modified silicon dioxide gel；The silicon dioxide gel with
The volume ratio of modifying agent is (30~50):1；The volume ratio of the silicon dioxide gel and catalyst is (200~300):1.
3. a kind of photochromic micro-encapsulation hybrid modification silicon dioxide gel coated fabric according to claim 2, special
Sign is that the modifying agent is vinyltrimethoxysilane；The catalyst is dibutyl tin laurate.
4. a kind of photochromic micro-encapsulation hybrid modification silicon dioxide gel coated fabric according to claim 2, special
Sign is that the preparation process of the silicon dioxide gel is as follows：
First, ethyl orthosilicate with absolute ethyl alcohol under air-proof condition is uniformly mixed, obtains mixed liquor；The ethyl orthosilicate with
The volume ratio of absolute ethyl alcohol is 1:(1~1.6)；2nd, the hydrochloric acid that mass fraction is 27% is added in deionized water, obtains dilute salt
Acid, the hydrochloric acid that the mass fraction is 27% are 1 with entering deionized water volume ratio:(1~44)；3rd, it is 60 DEG C of water-baths in temperature
It is added dropwise dilute hydrochloric acid under heated at constant temperature stirring condition into mixed liquor, the volume ratio of the dilute hydrochloric acid and mixed liquor is 1:(6~
8) 1.5h~2.5h, initial reaction object, Ran Houjia then, are stirred to react in the case where temperature is 60 DEG C of constant temperature water bath condition of heating and stirring
Enter n,N-Dimethylformamide, the volume ratio of the n,N-Dimethylformamide and initial reaction object is (3~4.5):10, stirring
12h~for 24 hours is stood after mixing at room temperature, obtains silicon dioxide gel.
5. a kind of preparation side of photochromic micro-encapsulation hybrid modification silicon dioxide gel coated fabric as described in claim 1
Method, it is characterised in that a kind of preparation method of photochromic micro-encapsulation hybrid modification silicon dioxide gel coated fabric is by following
What step was completed：
Photochromic micro-encapsulation is added in container, then adds in hydrophobic modified silicon dioxide gel, is 24~40 in temperature
Magnetic agitation reacts 5min~20min under the conditions of DEG C, obtains photochromic micro-encapsulation hybrid modification silicon dioxide gel coating and knits
Object；The mass ratio of the hydrophobic modified silicon dioxide gel and photochromic micro-encapsulation is (30~35):1；Described is photic
Discoloration microcapsules are bivalve polyurethane-chitosan photochromic micro-encapsulation.
6. a kind of preparation of photochromic micro-encapsulation hybrid modification silicon dioxide gel coated fabric according to claim 5
Method, it is characterised in that the preparation process of the hydrophobic modified silicon dioxide gel is as follows：
Silicon dioxide gel is added in container, then adds in modifying agent, then catalyst is added dropwise, sealing container, in bath temperature
1.5h~2.5h is reacted for magnetic agitation at 40 DEG C, obtains hydrophobic modified silicon dioxide gel；The silicon dioxide gel with
The volume ratio of modifying agent is (30~50):1；The volume ratio of the silicon dioxide gel and catalyst is (200~300):1.
7. a kind of preparation of photochromic micro-encapsulation hybrid modification silicon dioxide gel coated fabric according to claim 6
Method, it is characterised in that the modifying agent is vinyltrimethoxysilane；The catalyst is dibutyl tin laurate.
8. a kind of preparation of photochromic micro-encapsulation hybrid modification silicon dioxide gel coated fabric according to claim 6
Method, it is characterised in that the preparation process of the silicon dioxide gel is as follows：
First, ethyl orthosilicate with absolute ethyl alcohol under air-proof condition is uniformly mixed, obtains mixed liquor；The ethyl orthosilicate with
The volume ratio of absolute ethyl alcohol is 1:(1~1.6)；2nd, the hydrochloric acid that mass fraction is 27% is added in deionized water, obtains dilute salt
Acid, the hydrochloric acid that the mass fraction is 27% are 1 with entering deionized water volume ratio:(1~44)；3rd, it is 60 DEG C of water-baths in temperature
It is added dropwise dilute hydrochloric acid under heated at constant temperature stirring condition into mixed liquor, the volume ratio of the dilute hydrochloric acid and mixed liquor is 1:(6~
8) 1.5h~2.5h, initial reaction object, Ran Houjia then, are stirred to react in the case where temperature is 60 DEG C of constant temperature water bath condition of heating and stirring
Enter n,N-Dimethylformamide, the volume ratio of the n,N-Dimethylformamide and initial reaction object is (3~4.5):10, stirring
12h~for 24 hours is stood after mixing at room temperature, obtains silicon dioxide gel.
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| CN111455693A (en) * | 2020-04-13 | 2020-07-28 | 探路者控股集团股份有限公司 | Modified long-acting photochromic microcapsule, preparation method thereof, photochromic dye printing paste containing modified long-acting photochromic microcapsule and application of photochromic dye printing paste |
| CN112176720A (en) * | 2020-09-28 | 2021-01-05 | 安徽瑜合警用装备有限公司 | Photoluminescent finishing agent based on silica microspheres, preparation method and application thereof |
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