CN104711856A - Production method of self-repairing super-hydrophobic flame retardation coat layer - Google Patents

Production method of self-repairing super-hydrophobic flame retardation coat layer Download PDF

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CN104711856A
CN104711856A CN201510053494.4A CN201510053494A CN104711856A CN 104711856 A CN104711856 A CN 104711856A CN 201510053494 A CN201510053494 A CN 201510053494A CN 104711856 A CN104711856 A CN 104711856A
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self
fabric
super hydrophobic
repairing super
flame retardant
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孙俊奇
陈姗姗
李想
李洋
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Jilin University
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Jilin University
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Abstract

The invention relates to a production method of a self-repairing super-hydrophobic flame retardation coat layer, and belongs to the technical filed of production self-repairing super-hydrophobic flame retardation coat layers. The method comprises the following steps: a self-extinguishing flame retardation coat layer is made through a simple technology, and a self-repairing super-hydrophobic film is used to protect the flame retardation function easily destroyed by water. The method comprises the steps of substrate processing, solution preparation and three-layer film assembling. The substrate is not restricted by the size or shape of a fabric, and is suitable for various common fabrics. Terylene is modified with the self-repairing self-hydrophobic flame retardation coat layer, only 10cm of the fabric is blackened after the obtained fabric is ignited and burns for 12s, and the remaining portion of the fabric is completely not influenced by flame. The contact angle of the modified fabric is 160DEG, and the super-hydrophobicity can be rapidly restored after being destroyed. The method used in the invention has simple program, has the advantages of long acting and energy saving, can be used in various fabrics, and is expected to be widely applied in the fields of packaging, home finishing and buildings.

Description

A kind of preparation method of self-repairing super hydrophobic flame retardant coating
Technical field
The invention belongs to self-repairing super hydrophobic and flame retardant coating preparing technical field; a kind of flame retardant coating of self-gravitation is specifically prepared by simple method; and with self-repairing super hydrophobic function and protecting easily by the inflaming retarding membrane of water destruct, provide a kind of preparation method that can extend the flame retardant coating of the self-repairing super hydrophobic in super-hydrophobic coat and flame retardant coating service life.
Background technology
Fabric has a wide range of applications in daily life, and its figure can be seen in a lot of aspect such as clothing, household packaging material, but the inflammable characteristic of fabric height is deep annoyings us, greatly limit its application.Carry out flame treatment to combustible material effectively to delay propagation of flame and even can prevent material from being lighted.A lot of research is all in the preparation paying close attention to fire proofing recently; one of most effective method wherein giving textile material fire resistance is modification; flame retarding agents can be made at the surface enrichment of material by finishing; thus reach the highest fire protection efficiency; and finishing can not change the mechanical performance of protected fabric, modification is utilized also can selectively to deposit other functional moleculars and realize multi-functional integration in addition.As a kind of modification, laminated assembling technology (layer-by-layer, LbL) has played great advantage in the preparation of flame-retardant layer.Nearest Grunlan and his colleague with LbL method at cotton surface alternating deposit polyphosphate sodium and PAH, obtain efficient expansion fire-proof layer (Adv.Mater.2011,23,3926 – 3931).Afterwards, they also explore the fire-retardant application of boiomacromolecule at cotton surface, and when after the alternately modification carrying out 30 shitosans and phytic acid, the flame spread can by effective compacting (Biomacromolecules 2012,13,2843-2848).The flame retardant coating of these intumescents usually all need polycation and polyanion alternating deposit tens even tens layers just can produce the poroid protective layer of three-dimensional of enough volumes when being heated, protection fabric is not by after-flame.In addition, because these fire proofings are all water miscible, so these flame-retardant layers are all difficult to bear washing process in water repeatedly, this point have impact on the application of fire retardant in productive life greatly.So how to prepare more firmly flame-retardant layer by simpler method is the problem that we will solve.
At nature widely, a lot of plant, animal all have super-hydrophobic surface to super-hydrophobic phenomenon.Super hydrophobic surface refers generally to contact angle and is greater than 150 °, the roll angle surface that is less than 10 °.Scientific research shows, superhydrophobic property is jointly determined by coarse surface texture and lower surface energy these two aspects factor.Super hydrophobic surface has a lot of unique surface characteristic: as self-cleaning property, soil resistance, hydrophobicity etc., makes it all have huge application prospect at life, production field.And the super-hydrophobic layer with self-repair function receives more welcome undoubtedly, even blown off by external force once the low-surface energy substance of coating surface is decomposed by ultraviolet or acid rain, the low-surface-energy molecule of coat inside can be spontaneous infiltrate, impaired super hydrophobic surface is repaired, thus extends the service life of super hydrophobic surface.
Summary of the invention
The object of the invention is at a kind of flame-retardant layer efficiently of fabric face preparation, with modifying the super-hydrophobic coat of selfreparing, preparation one can the self-cleaning flame-retardant cotton of long-acting and anti-fouling.Soak through three times, fabric just obtains good flameproof effect and can the super-hydrophobic ability of selfreparing, for providing a new method service life extending super-hydrophobic fire retardant.
The preparation method of self-repairing super hydrophobic flame retardant coating of the present invention, its step is as follows:
1) CATION is constructed primitive, anion constructs primitive respectively water-soluble, ethanol, carrene or toluene, be made into that concentration is 1 ~ 30mg/mL, pH value is the solution of 2 ~ 12; Low-surface-energy molecule is dissolved in ethanol, carrene or toluene, is made into the solution that concentration is 1 ~ 30mg/mL;
2) substrate after cleaning is immersed in respectively CATION to construct primitive and anion and to construct in primitive solution 10 ~ 60 minutes, each soak after substrate is taken out, spend deionized water substrate and the moisture content back-outed in substrate;
3) by step 2) substrate that obtains in the baking oven of 25 ~ 80 DEG C dry 2 ~ 6 hours, thus prepare inflaming retarding membrane at substrate surface;
4) by step 3) substrate that obtains to be immersed in low-surface-energy molecular solution 1 ~ 10 minute, then substrate is taken out from low-surface-energy molecular solution, drying 2 ~ 6 hours in the baking oven of 25 ~ 80 DEG C, thus in substrate, prepare self-repairing super hydrophobic flame retardant coating.
CATION is constructed primitive and anion and is constructed primitive and be combined with each other by electrostatic force, hydrogen bond, Van der Waals force etc.Low-surface-energy molecule is combined with substrate or flame retardant coating by Van der Waals force.
The cleaning of the substrate described in above-mentioned steps:
The substrate that the present invention is used for constructing self-repairing super hydrophobic flame retardant coating is various conventional fabrics, as cotton, burlap, terylene etc., and does not limit by fabric size, shape.Various fabric needed to wash with washing agent before deposited coatings, and rinsed clean.Various substrates are after treatment conducive to layer assembly film directly constructing on its surface.
The selection of constructing primitive described in above-mentioned steps:
The CATION that the present invention uses constructs one or more in primitive employing PAH (PAH), branched polyethylene base imines (PEI), diallyl dimethyl amine hydrochlorate (PDDA) etc., and anion constructs one or more in primitive employing phytic acid (PA), APP (APP), polyphosphate sodium (PSP), imvite (MMT) etc.The low-surface-energy molecule that the present invention uses is C 4~ C 16alkyl or tetrahydrochysene perfluor C 4~ C 16the cage modle polysilsesquioxane of alkyl modified (is called for short R-POSS, general formula (RSiO 3/2) 8, wherein R is eight drift angle Si atom institute linking groups, and this Series Molecules synthesizes according to the method for bibliographical information, bibliography: Angew.Chem.Int.Ed.2008,47,4137).
CATION particularly polycation (foregoing PAH, PEI, PDDA are all polycations) can in various substrate Direct precipitation and do not need finishing or only need simple finishing to increase deposition efficiency.In addition, CATION particularly polycation also containing a large amount of functional groups freely, pH value in a big way in a large amount of positive charges, so just can be carried out the deposition of next step anion easily by laminated assembling technology.
The fire resistance of self-repairing super hydrophobic flame retardant coating:
The flame retardant coating of intumescent is made up of four fundamentals, is acid source, source of the gas, carbon source and crosslinking agent respectively.In the layer assembly system of anions and canons alternating deposit crosslinking agent by anions and canons between and electrostatic force, hydrogen bond or Van der Waals force between ion and fabric serve as.Acid source PSP, APP and PA etc. normally containing phosphate group, when being heated, generation phosphoric acid is decomposed in phosphate group heat absorption fracture, consumes heats a large amount of in surrounding environment; The fabric fibre of carbon containing and poly-zwitterion chain such as PEI, PAH, PDDA etc. are as the carbon source in system, and carbonization of dewatering under the catalytic action of acid source forms heat, gas, the flame separation layer of molten; Meanwhile PEI, PAH, PDDA etc. are again as the source of the gas in system, discharge incombustible gas in combustion, such as ammonia, carbon dioxide etc., by the combustion-supporting gas expulsion around burning situation, this gas overflows from melting layer in addition, makes melting layer occur loose porous foam-like form, the gas beyond more effective isolated system, heat and flame, thus the effective compacting realized the intensity of a fire, stop spreading of flame.
1. the ultra-hydrophobicity of self-repairing super hydrophobic flame retardant coating
According to self-repairing super hydrophobic coating prepared by the method, its contact angle is about 160 °, has good automatically cleaning effect.
2. the super-hydrophobic self-healing properties of self-repairing super hydrophobic flame retardant coating
Preserve 0.5 ~ 4 hour under 25 ~ 80% relative humidity, fabric face is decomposed or the low-surface energy substance destroyed can be resumed, and the contact angle of fabric face returns to initial state immediately, and such reparation destroys can repeat more than 10 times.
The present invention prepares self-repairing super hydrophobic flame retardant coating by laminated assembling technology.The preparation method of this flame retardant coating is very simple, breaches the limitation of the assemble method of original tens layers, but can obtain good flame retardant effect equally, can delay the burning of fabric, stop spreading of flame, the fabric of extraordinary protection bottom.We can protect flame-retardant layer by self-repairing super hydrophobic layer at breakthrough use in addition, prevent the loss after washing or adhesional wetting of water miscible flame-retardant layer, extend the life-span of this coating, broaden application scope.Adopt the preparation method of self-repairing super hydrophobic flame retardant coating of the present invention can be used for designing various self-repairing super hydrophobic and inflaming retarding membrane, and go for diversified textile material, be expected to be widely used in fields such as packaging, household, buildings.
Accompanying drawing explanation
Fig. 1: be a) the combustion case photo of undressed terylene when lighting 4 seconds, flame scorches fabric and automatically removes afterwards for 12 seconds, b) is the photo after fabric self-gravitation; C) being the photo of burlap when lighting 4 seconds with self-repairing super hydrophobic flame retardant coating, d) is this fabric photo that flame removes after scorching 12 seconds, corresponding embodiment 1;
Fig. 2: the state diagram of water droplet on dacron surface before and after ultra-hydrophobicity destroys, a) be that the drop of dyeing before ultra-hydrophobicity destroys is in the state of fabric face, b) be after ultra-hydrophobicity destroys, the drop of dyeing infiltrates the photo of fabric, c) be that b) middle fabric passes through the state of reparation poststaining drop at fabric face, corresponding embodiment 1;
Fig. 3: the SEM figure being modified with the different multiples of the fabric blackening part after combustion of self-repairing super hydrophobic flame-retardant layer, corresponding embodiment 2;
Fig. 4: the water droplet contact angle state diagram being modified with the burlap of self-repairing super hydrophobic flame-retardant layer, corresponding embodiment 2;
Fig. 5: contact angle state diagram after self-repairing super hydrophobic flame retardant coating is etched, corresponding embodiment 2;
Fig. 6: the contact angle state diagram of selfreparing after 4 hours after self-repairing super hydrophobic flame retardant coating is etched, corresponding embodiment 2.
Detailed description of the invention
Illustrate specific embodiment of the invention and result further below by way of some examples, instead of limit the present invention with these examples.
Contact angle is recorded by Dataphysics OCA20 type contact angle measurement.
Vertical combustion test in 12 seconds completes in CZF-3 type horizontal vertical burning analyzer.
Embodiment 1: the preparation of self-repairing super hydrophobic flame retardant coating on terylene surface and fire-retardant application
Terylene to be successively immersed in the PAH aqueous solution (5mg/mL, pH=10) and the PA aqueous solution (30mg/mL, pH=5) each 30 minutes, each soak after by substrate taking-up, spend deionized water substrate and the moisture content back-outed in substrate; In the baking oven of 60 DEG C, drying 4 hours, namely prepares inflaming retarding membrane at substrate surface.
Dried flame-resistant terylene is immersed in the CH of 5mg/mL 3(CH 2) 13in the dichloromethane solution of-POSS 3 minutes, dry that namely obtain can the flame-resistant terylene of self-repairing super hydrophobic.
In this embodiment, changing solution concentration can not make a significant impact constructing of film, if just solution concentration is too low, solute is very few, be then difficult to obtain extraordinary flameproof effect and super-hydrophobic selfreparing effect in so simple deposition process; If excessive concentration, although the process that acceleration film is constructed, may cause the waste of solute, namely in this system, suitable concentration range is 1 ~ 30mg/mL.
Fig. 1 is the photo of 12 seconds vertical combustion test processs, and fabric fixture is fixed in the burning cabinet of horizontal vertical burning analyzer, and lighted a fire by automated procedures, flame scorches fabric end, and after 12 seconds, flame is removed automatically.By (Fig. 1 a) contrasts with undressed terylene, can see c) clearly, d) in the flameproof effect with the terylene of super-hydrophobic flame retardant coating very good, after flame through 12 seconds scorches, terylene does not reduce to flying ashes and smouldering smoke as undressed terylene (Fig. 1 b), but maintain overall integrality, and only there is a fraction of carbonization blackening, the length of carbonized part is only 10cm, remaining fabric still keeps original state, and this illustrates that the self-repairing super hydrophobic coating prepared by this method has good flame retardant effect really.
Fig. 2 a is the form on the terylene surface of water droplet after this modifies after dyeing, and such surface can effectively prevent flame-retardant layer to the dissolving in aqueous phase, and antifouling and automatically cleaning that can be real-time.Material in use can be subject to the impact of acid rain, illumination etc. unavoidably, the hydrophobic layer of deface, and the drop now dyeed will infiltrate (Fig. 2 b) in fabric.In the process of soaked with liquid fabric, a large amount of fire proofings can be walked by water-band, and this will reduce the life-span of flame-retardant layer greatly.The method that the present invention shows can recover super-hydrophobicity in wet environment; after the fabric that surface super hydrophobic layer is destroyed is preserved 2 hours under moist (envionmental humidity is 35% ~ 45%) condition; the state of drop on surface returns to again initial level (Fig. 2 c); and such repair process can repeat many times, realize the long-effective protection to lower floor's flame-retardant layer.
Embodiment 2: the preparation of self-repairing super hydrophobic flame retardant coating on burlap surface and self-repairing super hydrophobic application
Burlap is first immersed in the PDDA aqueous solution (8mg/mL, pH=7) in 20 minutes, then to be immersed in the PSP aqueous solution (25mg/mL, pH=7) 60 minutes, after each immersion, burlap is taken out, spend deionized water burlap and the moisture content back-outed in burlap; Then in the baking oven of 60 DEG C dry 4 hours, namely inflaming retarding membrane is prepared on burlap surface.
Dried flame-retardant linen is immersed in the CF of 3mg/mL 3(CF 2) 7(CH 2) 2in the toluene solution of-POSS 5 minutes, dry that namely obtain can the flame-retardant linen of self-repairing super hydrophobic.
Even if can see from Fig. 3 a and to scorch and carbonization blackening through flame, the integrality of the yarn texture of fabric still can keep, can see in SEM figure (Fig. 3 b) amplified has froth bed clearly at fiber surface, and this illustrates that this coating meets the fire retardant mechanism of intumescent really.
Fig. 4 is the water droplet contact angle state diagram of the burlap after process, and contact angle is 162 °.After oxygen plasma cleaning machine etching, the burlap being modified with super-hydrophobic flame-retardant layer becomes super hydrophilic (Fig. 5), preserves fabric 4 hours under the relative humidity of 35%, finds that contact angle state returns to again initial level (Fig. 6).
Embodiment 3: two principle flame-retardant systems of compound are applied to cotton by self-repairing super hydrophobic flame retardant coating preparation method
Cotton is successively immersed in the PEI aqueous solution (8mg/mL, (concentration of PSP is 25mg/mL to the compound aqueous solution of pH=9), PSP and MMT, pH=7, MMT is 5% of PSP quality) in each 20 minutes, after each immersion, cotton is taken out, spend deionized water cotton and the moisture content back-outed in substrate; In the baking oven of 50 DEG C, drying 5 hours, namely prepares inflaming retarding membrane at cotton surface.
Dried fire-retardant substrate is immersed in the C of 6mg/mL 8h 17in the dichloromethane solution of-POSS 10 minutes, dry that namely obtain can the fire retardant of self-repairing super hydrophobic.
In the compound system of PSP and MMT, the fire retardant mechanism of existing intumescent, also the physical barriers effect of MMT is had, when the preparation method of a kind of self-repairing super hydrophobic flame retardant coating of the present invention is applied to this system, can obtain equally can the flame-retardant cotton of self-gravitation, and the self-repairing super hydrophobic performance of this fire retardant is also very excellent.

Claims (5)

1. a preparation method for self-repairing super hydrophobic flame retardant coating, its step is as follows:
1) CATION is constructed primitive, anion constructs primitive respectively water-soluble, ethanol, carrene or toluene, be made into that concentration is 1 ~ 30mg/mL, pH value is the solution of 2 ~ 12; Low-surface-energy molecule is dissolved in ethanol, carrene or toluene, is made into the solution that concentration is 1 ~ 30mg/mL;
2) fabric substrate after cleaning is immersed in respectively CATION to construct primitive and anion and to construct in primitive solution 10 ~ 60 minutes, each soak after substrate is taken out, spend deionized water substrate and the moisture content back-outed in substrate;
3) by step 2) fabric substrate that obtains in the baking oven of 25 ~ 80 DEG C dry 2 ~ 6 hours, thus prepare inflaming retarding membrane on fabric substrate surface;
4) by step 3) fabric substrate that obtains to be immersed in low-surface-energy molecular solution 1 ~ 10 minute, then fabric substrate is taken out from low-surface-energy molecular solution, drying 2 ~ 6 hours in the baking oven of 25 ~ 80 DEG C, thus in fabric substrate, prepare self-repairing super hydrophobic flame retardant coating.
2. the preparation method of a kind of self-repairing super hydrophobic flame retardant coating as claimed in claim 1, is characterized in that: it is one or more in PAH, branched polyethylene base imines, diallyl dimethyl amine hydrochlorate that CATION constructs primitive.
3. the preparation method of a kind of self-repairing super hydrophobic flame retardant coating as claimed in claim 1, is characterized in that: it is one or more in phytic acid, APP, polyphosphate sodium, imvite that anion constructs primitive.
4. the preparation method of a kind of self-repairing super hydrophobic flame retardant coating as claimed in claim 1, is characterized in that: low-surface-energy molecule is C 4~ C 16alkyl or tetrahydrochysene perfluor C 4~ C 16the cage modle polysilsesquioxane of alkyl modified.
5. the preparation method of a kind of self-repairing super hydrophobic flame retardant coating as claimed in claim 1, is characterized in that: fabric substrate is cotton, burlap or terylene.
CN201510053494.4A 2015-02-02 2015-02-02 Production method of self-repairing super-hydrophobic flame retardation coat layer Pending CN104711856A (en)

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Cited By (5)

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Publication number Priority date Publication date Assignee Title
CN106894224A (en) * 2017-03-10 2017-06-27 吉林大学 A kind of halogen-free flameproof self-repairing super hydrophobic coating glue used for textiles and fire-retardant self-repairing super hydrophobic fabric
CN108505323A (en) * 2018-04-10 2018-09-07 中国科学技术大学 A kind of method that super-hydrophobic oleophobic flame retardant coating arranges base material
CN109137467A (en) * 2018-06-27 2019-01-04 华南理工大学 The method that one kettle way prepares super-hydrophobic fire-retardant textile fabric
CN110314829A (en) * 2019-07-08 2019-10-11 河北大学 It is a kind of that oneself puts out a fire, the preparation method of super hydrophilic, underwater super oleophobic coating
CN112411198A (en) * 2020-10-22 2021-02-26 苏州逸纪杰电子科技有限公司 Flame-retardant temperature-regulating environment-friendly non-woven fabric and preparation method thereof

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CN103321044A (en) * 2013-07-08 2013-09-25 苏州大学 Flame-retardant pure silk and preparation method thereof

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106894224A (en) * 2017-03-10 2017-06-27 吉林大学 A kind of halogen-free flameproof self-repairing super hydrophobic coating glue used for textiles and fire-retardant self-repairing super hydrophobic fabric
CN108505323A (en) * 2018-04-10 2018-09-07 中国科学技术大学 A kind of method that super-hydrophobic oleophobic flame retardant coating arranges base material
CN109137467A (en) * 2018-06-27 2019-01-04 华南理工大学 The method that one kettle way prepares super-hydrophobic fire-retardant textile fabric
CN109137467B (en) * 2018-06-27 2020-04-28 华南理工大学 Method for preparing super-hydrophobic flame-retardant textile fabric by one-pot method
CN110314829A (en) * 2019-07-08 2019-10-11 河北大学 It is a kind of that oneself puts out a fire, the preparation method of super hydrophilic, underwater super oleophobic coating
CN112411198A (en) * 2020-10-22 2021-02-26 苏州逸纪杰电子科技有限公司 Flame-retardant temperature-regulating environment-friendly non-woven fabric and preparation method thereof

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