CN107189686A - A kind of preparation method of composite flame-proof coating - Google Patents

A kind of preparation method of composite flame-proof coating Download PDF

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Publication number
CN107189686A
CN107189686A CN201710458961.0A CN201710458961A CN107189686A CN 107189686 A CN107189686 A CN 107189686A CN 201710458961 A CN201710458961 A CN 201710458961A CN 107189686 A CN107189686 A CN 107189686A
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composite flame
proof coating
suspension
mixed solution
chlorinated paraffin
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CN107189686B (en
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苏毅
陈庆发
王飞风
芦宇峰
夏小飞
黄辉敏
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Electric Power Research Institute of Guangxi Power Grid Co Ltd
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Electric Power Research Institute of Guangxi Power Grid Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D191/00Coating compositions based on oils, fats or waxes; Coating compositions based on derivatives thereof
    • C09D191/06Waxes
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D5/00Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
    • C09D5/08Anti-corrosive paints
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D5/00Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
    • C09D5/18Fireproof paints including high temperature resistant paints
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/18Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20Oxides; Hydroxides
    • C08K3/22Oxides; Hydroxides of metals
    • C08K3/2279Oxides; Hydroxides of metals of antimony
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00Use of organic ingredients
    • C08K5/54Silicon-containing compounds
    • C08K5/5406Silicon-containing compounds containing elements other than oxygen or nitrogen
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K9/00Use of pretreated ingredients
    • C08K9/04Ingredients treated with organic substances
    • C08K9/06Ingredients treated with organic substances with silicon-containing compounds

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Wood Science & Technology (AREA)
  • Organic Chemistry (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
  • Paints Or Removers (AREA)
  • Fireproofing Substances (AREA)

Abstract

The invention discloses a kind of preparation method of composite flame-proof coating, it is related to technical field of coatings, includes preparation Sb2O3The step of 70 suspension of suspension and chlorinated paraffin, by the Sb2O3Suspension and the mixing of the suspension of the chlorinated paraffin 70 and to Sb2O3The step of Silane coupling agent KH550 is added dropwise in the mixed solution of suspension and the suspension of chlorinated paraffin 70 and back flow reaction and suction filtration, the step of drying are carried out to above-mentioned steps resulting solution.The preparation method of the composite flame-proof coating that the present invention is provided is simple, and raw material is easily obtained, and equipment requirement is low, and processing cost is low, and it is superior to obtain composite flame-proof coating property, with good promotion prospect.The composite flame-proof coating obtained can apply to high-tension switch cabinet insulating sheath, polypropylene substrate, busbar heat-shrinkable T bush, sleeve penetrating through cabinet, insulation booth, on pole, additionally provide obtained composite flame-proof coating being coated to high-tension switch cabinet insulating sheath, polypropylene substrate, busbar heat-shrinkable T bush, sleeve penetrating through cabinet, insulation booth, the method on pole.

Description

A kind of preparation method of composite flame-proof coating
Technical field
The present invention relates to technical field of coatings, more particularly to a kind of preparation method of composite flame-proof coating.
Background technology
Guangxi DianKeYuan carries out special sampling observation work in December, 2015, inspects 13 switch cubicles by random samples altogether and carries out shield sleeve flame examination Test, qualification rate is only 23%.Find that high polymer material, which lacks fire resistance, will cause fire from accident forward and result of the test The expansion of calamity.Therefore it is a particularly significant and urgent job to carry out flame retardant treatment to high-molecular organic material, wherein most having One of method of effect is exactly to add anti-flaming dope, and combustible material is converted into flame retardant material, reduces the burning velocity of material, Fire is prevented to expand.
In production work, by the sampling observation of reinforced sheath fire resistance and then effective product can be reached for new purchase switch cubicle Matter management and control, and for there is the switch cubicle sheath of fire resistance defect in fortune, it is necessary to repair its anti-flammability using anti-flaming dope Energy.And the research of current organic fire-resisting coating is concentrated mainly on 4 aspects:(1)For steel construction and the facing type on building surface Anti-flaming dope;(2)For the research and development of high molecular fire retardant monomer, such as flame retardant acrylate's monomer;(3)Novel flame-retardant structure The application of unit or fire retardant in coating, such as phosphorous POSS structure polyurethanes;(4)The exploitation of new flame retarding process, such as nanometer Technology, microcapsule coated technology and layer-by-layer.However, the Special fireproof of the simply coating of these research emphasis concern Property, non-comprehensive study its corrosion resistance, water resistance and corrosion resistance, also lack efficiently, the preparation method for coating of high yield.Based on this, A kind of preparation method for coating of efficient high yield turns into active demand.
The content of the invention
Not enough for more than, the present invention provides a kind of efficient, preparation method of the composite flame-proof coating of high yield, can prepare Go out anti-flammability, corrosion resistance, water resistance and the good composite flame-proof coating of weatherability.Meanwhile, present invention also offers pass through this The composite flame-proof coating that the preparation method of the composite flame-proof coating of disclosure of the invention is obtained is fire-retardant reinforcing switch cubicle insulating sheath Application in property, corrosion resistance, water resistance and weatherability;And strengthen switch cubicle insulating sheath there is provided composite flame-proof coating Anti-flammability, corrosion resistance, the intensifying method of water resistance and weatherability.
To reach above-mentioned purpose, the present invention is adopted the following technical scheme that:
A kind of preparation method of composite flame-proof coating, includes following steps:
Step(One):By Sb2O3Powder is added in the mixed solution of deionized water and absolute ethyl alcohol, the deionized water and nothing The mixed solution of water-ethanol presses 16 by deionized water and absolute ethyl alcohol:1~21:1 volume ratio is formulated, the Sb2O3Institute The concentration stated in the mixed solution of deionized water and absolute ethyl alcohol is 1 ~ 3 g/L, to added with the Sb2O3The deionization of powder The mixed solution of water and absolute ethyl alcohol is stirred, ultrasonication, obtains uniform Sb2O3Suspension;
Step(Two):In the mixed solution that chlorinated paraffin -70 powder is added to deionized water and absolute ethyl alcohol, the deionization The mixed solution of water and absolute ethyl alcohol presses 16 by deionized water and absolute ethyl alcohol:1~21:1 volume ratio is formulated, the chlorine Concentration of the fossil waxes -70 in the mixed solution of the deionized water and absolute ethyl alcohol is 7 ~ 9 g/L, to added with the chlorination The deionized water of the powder of paraffin -70 and the mixed solution of absolute ethyl alcohol are stirred, ultrasonication, obtain uniform chlorination stone The suspension of wax -70;
Step(Three):By the Sb2O3Suspension and chlorinated paraffin -70 suspension mixing, then to Sb2O3Suspension and The mixed solution and dripping of chlorinated paraffin -70 suspension enters Silane coupling agent KH550, and the Silane coupling agent KH550 is in Sb2O3 Concentration in the mixed solution of suspension and chlorinated paraffin -70 suspension is 2 ~ 3 g/L, to added with the silane coupler KH550 Sb2O3The mixed solution of suspension and chlorinated paraffin -70 suspension carries out magnetic agitation, and temperature control is 45 ~ 55 DEG C, obtain chlorinated paraffin -70/Sb after 100 ~ 150 min of stirring2O3Modified mixing fire retardant;
Step(Four):By the chlorinated paraffin -70/Sb2O3Modified mixing fire retardant loads reflux, adds acetone, wherein The acetone and the chlorinated paraffin -70/Sb2O3The volume ratio of modified mixing fire retardant is 1:3~2:3, and make gained mixing molten Liquid temperature degree remains 50 ~ 70 DEG C, carries out the min of magnetic agitation 25 ~ 35, adds concentration for 0.3 ~ 0.5 g/L methyl trichlorine silicon Alkane solution, the methyl trichlorosilane solution and the chlorinated paraffin -70/Sb2O3The volume ratio of modified mixing fire retardant is 1: 1200~1:600, then the h of back flow reaction 22 ~ 26;Be cooled to room temperature after back flow reaction, suction filtration, using isometric concentration hydrochloric acid and The mixed solution washed product and suction filtration of frozen water, reuse distilled water and wash product to neutrality, finally in 45 ~ 55 DEG C of conditions The lower h of drying 22 ~ 26, obtains composite flame-proof coating.
Further, in step(One)In, mixing time is 2 ~ 4 min, and ultrasonic treatment time is 15 ~ 30 min, is surpassed Sonicated temperature is normal temperature.
Further, in step(Two)In, mixing time is 2 ~ 4 min, and ultrasonic treatment time is 15 ~ 30 min, is surpassed Sonicated temperature is normal temperature.
Preferably, in step(One)In, the Sb2O3In the mixed solution of the deionized water and absolute ethyl alcohol Concentration is 2 g/L.
Preferably, in step(Two)In, the chlorinated paraffin -70 is molten in the mixing of the deionized water and absolute ethyl alcohol Concentration in liquid is 8 g/L.
Preferably, in step(Three)In, the Silane coupling agent KH550 is in Sb2O3Suspension and chlorinated paraffin -70 are outstanding Concentration in the mixed solution of supernatant liquid is 2.5 g/L.
Preferably, in step(Four)In, the methyl trichlorosilane solution and the chlorinated paraffin -70/Sb2O3It is modified The volume ratio for mixing fire retardant is 1:800.
The composite flame-proof coating obtained the invention provides the preparation method of the composite flame-proof coating is opened in reinforcing Close cabinet insulating sheath, polypropylene substrate, busbar heat-shrinkable T bush, sleeve penetrating through cabinet, insulation booth, the anti-flammability of pole, corrosion resistance, Application in water resistance and weatherability.The composite flame-proof that the preparation method of composite flame-proof coating of the present invention is obtained Coating can strengthen switch cubicle insulating sheath, polypropylene substrate, busbar heat-shrinkable T bush, sleeve penetrating through cabinet, insulation booth, pole Anti-flammability, corrosion resistance, water resistance and weatherability.
Present invention also offers composite flame-proof coating reinforcing switch cubicle insulating sheath, polypropylene substrate, busbar pyrocondensation Sleeve pipe, sleeve penetrating through cabinet, insulation booth, the anti-flammability of pole, corrosion resistance, the method for water resistance and weatherability, methods described For:Using applicator by the composite flame-proof coating be coated on switch cubicle insulating sheath, polypropylene substrate, busbar heat-shrinkable T bush, Sleeve penetrating through cabinet, insulation booth, on pole, paint thickness is 300 ~ 850 μm, and room temperature is air-dried.
Compared with prior art, the beneficial effects of the invention are as follows:
1st, the preparation method of a kind of composite flame-proof coating that the present invention is provided, can produce with excellent flame retardancy, corrosion resistance, The composite flame-proof coating of water resistance and weatherability;
2nd, the composite flame-proof coating that is obtained of the present invention can apply to switch cubicle insulating sheath, polypropylene substrate, busbar heat-shrinkable T bush, Sleeve penetrating through cabinet, insulation booth, on pole, to strengthen the anti-flammability of switch cubicle insulating sheath, corrosion resistance, water resistance and weather-proof Property;
3rd, the composite flame-proof coating that is obtained of the present invention in switch cubicle insulating sheath, polypropylene substrate, busbar heat-shrinkable T bush, wear cabinet set Pipe, insulation booth, the coating step on pole simply easily realize, composite flame-proof coating and switch cubicle insulating sheath, polypropylene Substrate, busbar heat-shrinkable T bush, sleeve penetrating through cabinet, insulation booth, pole have good adhesion, are coated with composite flame-proof coating Switch cubicle insulating sheath, polypropylene substrate, busbar heat-shrinkable T bush, sleeve penetrating through cabinet, insulation booth, pole simultaneously have it is excellent Anti-flammability, corrosion resistance, water resistance and weatherability;
4th, the preparation method for the composite flame-proof coating that the present invention is provided is simple, and raw material is easily obtained, and equipment requirement is low, processing cost Low, it is superior to obtain composite flame-proof coating property, with good promotion prospect.
Brief description of the drawings
In order to illustrate the technical solution of the embodiments of the present invention more clearly, being used required in being described below to embodiment Accompanying drawing be briefly described.
Fig. 1 is shape appearance figure of the face coat for the polypropylene substrate for being coated with composite flame-proof coating after cross-hatching;
Fig. 2 is macro morphology figure of the face coat for the polypropylene substrate for being coated with composite flame-proof coating after vertical combustion;
Fig. 3 is shape appearance figure of the face coat for the polypropylene substrate for being coated with composite flame-proof coating after water resistance test;
Fig. 4 is to be coated with the shape appearance figure after the face coat of the polypropylene substrate of composite flame-proof coating is tested through acid resistance;
Fig. 5 is to be coated with the shape appearance figure after the face coat of the polypropylene substrate of composite flame-proof coating is tested through salt tolerance;
Fig. 6 is to be coated with the shape appearance figure after the face coat of the polypropylene substrate of composite flame-proof coating is tested through alkali resistance;
Fig. 7 is to be coated with the shape appearance figure after the face coat of the polypropylene substrate of composite flame-proof coating is tested through weatherability.
Embodiment
Below in conjunction with the accompanying drawing in the embodiment of the present invention, the technical scheme in the embodiment of the present invention is carried out clear, complete Site preparation is described.Obviously, described embodiment is only a part of embodiment of the invention, rather than whole embodiments.It is based on Embodiment in the present invention, it is every other that those of ordinary skill in the art are obtained under the premise of creative work is not made Embodiment, belongs to the scope of protection of the invention.
Embodiment 1
The present embodiment provides a kind of preparation method of composite flame-proof coating, is specially:
Step(One):By 2 g Sb2O3Powder is added in the mixed solution of 2000 mL deionized waters and absolute ethyl alcohol, go from The mixed solution of sub- water and absolute ethyl alcohol presses 16 by deionized water and absolute ethyl alcohol:1 volume ratio is formulated, and is stirred with glass bar Mix added with Sb2O3The deionized water of powder and the mixed solution of absolute ethyl alcohol, mixing time are 2 min, are then used at normal temperatures The min of ultrasonic wave decentralized processing 15, obtains uniform Sb2O3Suspension;
Step(Two):14 g chlorinated paraffin -70 powder are added to the mixed solution of 2000 mL deionized waters and absolute ethyl alcohol In, the mixed solution of deionized water and absolute ethyl alcohol presses 16 by deionized water and absolute ethyl alcohol:1 volume ratio is formulated, and is used The mixed solution of deionized water and absolute ethyl alcohol of the glass bar stirring added with chlorinated paraffin -70 powder, mixing time is 2 Min, then uses the min of ultrasonic wave decentralized processing 15, obtains uniform chlorinated paraffin -70 suspension at normal temperatures;
Step(Three):By Sb2O3Suspension and the mixing of chlorinated paraffin -70 suspension, then to Sb2O3Suspension and chlorinated paraffin- The mixed solution and dripping of 70 suspension enters 8 g Silane coupling agent KH550s, to the Sb added with Silane coupling agent KH5502O3It is outstanding The mixed solution of supernatant liquid and chlorinated paraffin -70 suspension carries out magnetic agitation, and modification temperature is controlled at 45 DEG C, stirs 100 min After obtain chlorinated paraffin -70/Sb2O3Modified mixing fire retardant;
Step(Four):By chlorinated paraffin -70/Sb2O3Modified mixing fire retardant loads in three-necked flask, three-necked flask connection backflow Device, adds 700 mL acetone, and gained mixed solution temperature is remained 50 DEG C, carries out the min of magnetic agitation 25, adds 1.7 mL methyl trichlorosilane solution, then the h of back flow reaction 22;Room temperature, suction filtration, using isometric dense are cooled to after back flow reaction The hydrochloric acid of degree and the mixed solution washed product of frozen water and suction filtration, reuse distilled water and wash product to neutrality, finally 45 22 h are dried under the conditions of DEG C, composite flame-proof coating is obtained.
Obtain after composite flame-proof coating, composite flame-proof coating is coated on polypropylene substrate using applicator, coating is thick Spend for 300 μm, room temperature is air-dried.
Embodiment 2
The present embodiment provides a kind of preparation method of composite flame-proof coating, is specially:
Step(One):By 6 g Sb2O3Powder is added in the mixed solution of 2000 mL deionized waters and absolute ethyl alcohol, go from The mixed solution of sub- water and absolute ethyl alcohol presses 21 by deionized water and absolute ethyl alcohol:1 volume ratio is formulated, and is stirred with glass bar Mix added with Sb2O3The deionized water of powder and the mixed solution of absolute ethyl alcohol, mixing time are 4 min, are then used at normal temperatures The min of ultrasonic wave decentralized processing 30, obtains uniform Sb2O3Suspension;
Step(Two):18 g chlorinated paraffin -70 powder are added to the mixed solution of 2000 mL deionized waters and absolute ethyl alcohol In, the mixed solution of deionized water and absolute ethyl alcohol presses 21 by deionized water and absolute ethyl alcohol:1 volume ratio is formulated, and is used The mixed solution of deionized water and absolute ethyl alcohol of the glass bar stirring added with chlorinated paraffin -70 powder, mixing time is 4 Min, then uses the min of ultrasonic wave decentralized processing 30, obtains uniform chlorinated paraffin -70 suspension at normal temperatures;
Step(Three):By Sb2O3Suspension and the mixing of chlorinated paraffin -70 suspension, then to Sb2O3Suspension and chlorinated paraffin- The mixed solution and dripping of 70 suspension enters 12 g Silane coupling agent KH550s, to the Sb added with Silane coupling agent KH5502O3It is outstanding The mixed solution of supernatant liquid and chlorinated paraffin -70 suspension carries out magnetic agitation, and modification temperature is controlled at 55 DEG C, stirs 150 min After obtain chlorinated paraffin -70/Sb2O3Modified mixing fire retardant;
Step(Four):By chlorinated paraffin -70/Sb2O3Modified mixing fire retardant loads in three-necked flask, three-necked flask connection backflow Device, adds 1400 mL acetone, and gained mixed solution temperature is remained 70 DEG C, carries out the min of magnetic agitation 35, then add Enter 6.6 mL methyl trichlorosilane solution, then the h of back flow reaction 26;Room temperature, suction filtration, using isometric are cooled to after back flow reaction The hydrochloric acid of concentration and the mixed solution washed product of frozen water and suction filtration, reuse distilled water and wash product to neutrality, finally exist 26 h are dried under the conditions of 55 DEG C, composite flame-proof coating is obtained.
Obtain after composite flame-proof coating, composite flame-proof coating is coated on polypropylene substrate using applicator, coating is thick Spend for 850 μm, room temperature is air-dried.
Embodiment 3
The present embodiment provides a kind of preparation method of composite flame-proof coating, is specially:
Step(One):By 4 g Sb2O3Powder is added in the mixed solution of 2000 mL deionized waters and absolute ethyl alcohol, go from The mixed solution of sub- water and absolute ethyl alcohol presses 19 by deionized water and absolute ethyl alcohol:1 volume ratio is formulated, and is stirred with glass bar Mix added with Sb2O3The deionized water of powder and the mixed solution of absolute ethyl alcohol, mixing time are 3 min, are then used at normal temperatures The min of ultrasonic wave decentralized processing 20, obtains uniform Sb2O3Suspension;
Step(Two):16 g chlorinated paraffin -70 powder are added to the mixed solution of 2000 mL deionized waters and absolute ethyl alcohol In, the mixed solution of deionized water and absolute ethyl alcohol presses 19 by deionized water and absolute ethyl alcohol:1 volume ratio is formulated, and is used The mixed solution of deionized water and absolute ethyl alcohol of the glass bar stirring added with chlorinated paraffin -70 powder, mixing time is 3 Min, then uses the min of ultrasonic wave decentralized processing 20, obtains uniform chlorinated paraffin -70 suspension at normal temperatures;
Step(Three):By Sb2O3Suspension and the mixing of chlorinated paraffin -70 suspension, then to Sb2O3Suspension and chlorinated paraffin- The mixed solution and dripping of 70 suspension enters 10 g Silane coupling agent KH550s, to the Sb added with Silane coupling agent KH5502O3It is outstanding The mixed solution of supernatant liquid and chlorinated paraffin -70 suspension carries out magnetic agitation, and modification temperature is controlled at 50 DEG C, stirs 120 min After obtain chlorinated paraffin -70/Sb2O3Modified mixing fire retardant;
Step(Four):By chlorinated paraffin -70/Sb2O3Modified mixing fire retardant loads in three-necked flask, three-necked flask connection backflow Device, adds 1000 mL acetone, and gained mixed solution temperature is remained 60 DEG C, carries out the min of magnetic agitation 30, then add Enter 5 mL methyl trichlorosilane solution, then the h of back flow reaction 24;Room temperature, suction filtration, using isometric dense are cooled to after back flow reaction The hydrochloric acid of degree and the mixed solution washed product of frozen water and suction filtration, reuse distilled water and wash product to neutrality, finally 50 24 h are dried under the conditions of DEG C, composite flame-proof coating is obtained.
Obtain after composite flame-proof coating, composite flame-proof coating is coated on polypropylene substrate using applicator, coating is thick Spend for 750 μm, room temperature is air-dried.
The polypropylene substrate that composite flame-proof coating is coated with embodiment 3 is tested.
The face coat for being coated with the polypropylene substrate of composite flame-proof coating is carried out drawing lattice according to GB/T 9286-1988 Its adhesion is evaluated between method cutting, cut is at intervals of 5mm, shown in surface topography Fig. 1.It can be seen that the combination situation of coating Well, smooth in scratching edge, no tilting or obscission, evaluation result are 0 grade(It is highest).In order to further evaluate and test its knot With joint efforts, compartment is drawn away from as defined in being reduced into 1/2 to coating(At intervals of 2.5mm), as a result show, the cut of coating is still without de- Fall, show the adhesion far above 0 grade.
According to GB/T2405-2008, analyzer is burnt to being coated with composite flame-proof coating using CZF-6 horizontal vertical The face coat of polypropylene substrate carries out test anti-flammability test.The polypropylene substrate of composite flame-proof coating is coated with point twice Fall time after fire and be, no twilight sunset phenomenon low without molten drop in 2.6 s, combustion process, finally it is rated V-0 grades.No The sustained combustion after first time igniting 10s of the polypropylene substrate of composite flame-proof coating is coated with, in combustion with molten drop Drippage, until burning completely, shows poor fire resistance.From test result, composite coating can improve the resistance of base material Fire grade.Fig. 2 is the macro morphology figure for being coated with the polypropylene substrate of composite flame-proof coating after vertical combustion, is coated with compound There is most of charing in the polypropylene-base plate surface of anti-flaming dope, but substrate still keeps original form, shows in combustion process In, flame retardant coating absorbs the heat of the overwhelming majority, can be good at protecting the structural intergrity of base material.
According to GB/T 2408-2008, poly- the third of composite flame-proof coating is coated with using the test of JF-3 types oxygen index measurer The face coat of alkenyl plate and be not coated with composite flame-proof coating polypropylene substrate limited oxygen index.Test result table Bright, the oxygen index value for not being coated with the polypropylene substrate of composite flame-proof coating is 17.4%, belongs to combustible material, is coated with multiple The oxygen index value for closing the polypropylene substrate of anti-flaming dope is 30.3%, is fire retardant rank.
Provided according to national standard GB/T 1733-1993, use distilled water or deionized water(Meeting tertiary effluent in GB6682 will Ask), the polypropylene substrate for being coated with composite flame-proof coating is soaked, its water resistance is detected.It is the three of substrate to soak length / bis-, the use of water-bath by water temperature control is 23 ± 2 DEG C, takes out sample from beaker after 72 h, with filter paper by coating table Face moisture is blotted, then is dried up with hair-dryer, and observes whether coating surface the phenomenons such as dull, corrugation, coating shedding occurs And recovery time, as a result see Fig. 3.From the figure 3, it may be seen that be coated with the face coat of the polypropylene substrate of composite flame-proof coating go from Surface after 72h is soaked in sub- water and, without phenomenons such as color and luster change, foaming, corrugations, shows possess good water resistance.
According to national standard GB/T 1763-1979 (1989), applied to being coated with the surface of polypropylene substrate of composite flame-proof coating Layer progress is acidproof, alkaline-resisting, resistant to salt corrosion, detects its corrosion resisting property.
(1)Acid proof detection method:Sulfuric acid is made into 20% aqueous solution with distilled water, is put into beaker.Then, will Beaker is put into water-bath and solution temperature is maintained at into 25 DEG C, in 2/3rds immersion solution of sample, is taken out after 72 hours, Cleaned and blotted coating surface moisture with clear water with filter paper, then dried up with hair-dryer.Whether observation coating surface there is gloss The phenomenons such as dim, foaming, peeling, corrugation, as a result as shown in Figure 4.
From fig. 4, it can be seen that being soaked in sulfuric acid solution after 72h, the surface of the polypropylene substrate of composite flame-proof coating is coated with Its surface color of coating is unchanged, and without bubbling, the phenomenon such as wrinkle, come off, and shows that coating possesses good acid resistance corrosion.
(2)The detection method of salt tolerance:Sodium chloride is made into 3% aqueous solution with distilled water, poured into beaker.Then, will Beaker is put into water-bath and solution temperature is maintained at into 25 DEG C, and sample 2/3rds is immersed in solution, is taken out after 72 h, with clear Water cleans salt marsh and is blotted coating surface moisture with filter paper, then is dried up with hair-dryer.Whether observation coating surface there is gloss The phenomenons such as dim, foaming, peeling, corrugation, as a result as shown in Figure 5.
As seen from Figure 5, the polypropylene substrate of composite flame-proof coating its face coat is coated with to soak in sodium chloride solution Surface is without phenomenons such as color and luster change, foaming, corrugations after 72 h, and coating possesses good water resistance.
(3)The detection method of alkali resistance:Sodium hydroxide is made into 3.5% aqueous solution with distilled water, is put into beaker.So Afterwards, beaker is put into water-bath and solution temperature is maintained at 25 DEG C, in 2/3rds immersion solution of sample, taken after 72 h Go out, cleaned and blotted coating surface moisture with clear water with filter paper, then dried up with hair-dryer.Whether observation coating surface there is light The phenomenons such as damp dim, foaming, peeling, corrugation, as a result as shown in Figure 6.
As seen from Figure 6, the polypropylene substrate of composite flame-proof coating its face coat is coated with to soak in sodium hydroxide solution Steep surface after 72 h and, without phenomenons such as color and luster change, foaming, corrugations, show that coating possesses good water resistance.
The detection of weatherability uses natural climate aging process, and this experimental method is at home and abroad widely used, real Test that results contrast meets reality and experimental cost is low, simple experiment.Provided according to national standard GB/T15596-1995, sample is complete It is exposed to entirely under natural environmental condition, sample is fetched after 720 h, its color, efflorescence degree, cracking degree, foaming is observed Situation etc., as a result as shown in Figure 7.
As seen from Figure 7, it is coated with the exposure 720 in natural climate of its face coat of the polypropylene substrate of composite flame-proof coating Surface shows that coating possesses good weatherability without phenomenons such as color and luster change, foaming, corrugations after h.
The preparation method for the composite flame-proof coating that the present invention is provided is simple, and raw material is easily obtained, and equipment requirement is low, processing cost Low, obtaining composite flame-proof coating has the advantages that anti-flammability, corrosion resistance, water resistance and weatherability, coating and substrate adhesion By force.
The foregoing is only a specific embodiment of the invention, but protection scope of the present invention is not limited thereto, any Those familiar with the art the invention discloses technical scope in, the change or replacement that can be readily occurred in, all should It is included within the scope of the present invention.Therefore, protection scope of the present invention should using the scope of the claims as It is accurate.

Claims (9)

1. a kind of preparation method of composite flame-proof coating, it is characterised in that include following steps:
Step(One):By Sb2O3Powder is added in the mixed solution of deionized water and absolute ethyl alcohol, the deionized water and nothing The mixed solution of water-ethanol presses 16 by deionized water and absolute ethyl alcohol:1~21:1 volume ratio is formulated, the Sb2O3Institute The concentration stated in the mixed solution of deionized water and absolute ethyl alcohol is 1 ~ 3 g/L, to added with the Sb2O3The deionization of powder The mixed solution of water and absolute ethyl alcohol is stirred, ultrasonication, obtains uniform Sb2O3Suspension;
Step(Two):In the mixed solution that chlorinated paraffin -70 powder is added to deionized water and absolute ethyl alcohol, the deionization The mixed solution of water and absolute ethyl alcohol presses 16 by deionized water and absolute ethyl alcohol:1~21:1 volume ratio is formulated, the chlorine Concentration of the fossil waxes -70 in the mixed solution of the deionized water and absolute ethyl alcohol is 7 ~ 9 g/L, to added with the chlorination The deionized water of the powder of paraffin -70 and the mixed solution of absolute ethyl alcohol are stirred, ultrasonication, obtain uniform chlorination stone The suspension of wax -70;
Step(Three):By the Sb2O3Suspension and chlorinated paraffin -70 suspension mixing, then to Sb2O3Suspension and chlorine The mixed solution and dripping of the suspension of fossil waxes -70 enters Silane coupling agent KH550, and the Silane coupling agent KH550 is in Sb2O3It is outstanding Concentration in the mixed solution of supernatant liquid and chlorinated paraffin -70 suspension is 2 ~ 3 g/L, to added with the silane coupler KH550 Sb2O3The mixed solution of suspension and chlorinated paraffin -70 suspension carries out magnetic agitation, and temperature control is 45 ~ 55 DEG C, obtain chlorinated paraffin -70/Sb after 100 ~ 150 min of stirring2O3Modified mixing fire retardant;
Step(Four):By the chlorinated paraffin -70/Sb2O3Modified mixing fire retardant loads reflux, adds acetone, wherein institute State acetone and the chlorinated paraffin -70/Sb2O3The volume ratio of modified mixing fire retardant is 1:3~2:3, and make gained mixed solution Temperature remains 50 ~ 70 DEG C, carries out the min of magnetic agitation 25 ~ 35, adds concentration for 0.3 ~ 0.5 g/L methyl trichlorosilanes Solution, the methyl trichlorosilane solution and the chlorinated paraffin -70/Sb2O3The volume ratio of modified mixing fire retardant is 1:1200 ~1:600, then the h of back flow reaction 22 ~ 26;Room temperature is cooled to after back flow reaction, suction filtration uses the hydrochloric acid and frozen water of isometric concentration Mixed solution washed product and suction filtration, reuse distilled water and wash product to neutrality, finally done under the conditions of 45 ~ 55 DEG C Dry 22 ~ 26 h, obtains composite flame-proof coating.
2. the preparation method of composite flame-proof coating according to claim 1, it is characterised in that:In step(One)In, stirring Time is 2 ~ 4 min, and ultrasonic treatment time is 15 ~ 30 min, and ultrasonication temperature is normal temperature.
3. the preparation method of composite flame-proof coating according to claim 1, it is characterised in that:In step(Two)In, stirring Time is 2 ~ 4 min, and ultrasonic treatment time is 15 ~ 30 min, and ultrasonication temperature is normal temperature.
4. the preparation method of composite flame-proof coating according to claim 1, it is characterised in that:In step(One)In, it is described Sb2O3Concentration in the mixed solution of the deionized water and absolute ethyl alcohol is 2 g/L.
5. the preparation method of composite flame-proof coating according to claim 1, it is characterised in that:In step(Two)In, it is described Concentration of the chlorinated paraffin -70 in the mixed solution of the deionized water and absolute ethyl alcohol is 8 g/L.
6. the preparation method of composite flame-proof coating according to claim 1, it is characterised in that:In step(Three)In, it is described Silane coupling agent KH550 is in Sb2O3Concentration in the mixed solution of suspension and chlorinated paraffin -70 suspension is 2.5 g/L.
7. the preparation method of composite flame-proof coating according to claim 1, it is characterised in that:In step(Four)In, it is described Methyl trichlorosilane solution and the chlorinated paraffin -70/Sb2O3The volume ratio of modified mixing fire retardant is 1:800.
8. the composite flame-proof coating that the preparation method of the composite flame-proof coating according to claim any one of 1-7 is obtained Reinforcing switch cubicle insulating sheath, polypropylene substrate, busbar heat-shrinkable T bush, sleeve penetrating through cabinet, insulation booth, pole it is fire-retardant Application in property, corrosion resistance, water resistance and weatherability.
9. composite flame-proof coating reinforcing switch cubicle insulating sheath according to claim 8, polypropylene substrate, busbar thermal shrinkable sleeve Pipe, sleeve penetrating through cabinet, insulation booth, the anti-flammability of pole, corrosion resistance, the method for water resistance and weatherability, it is characterised in that The composite flame-proof coating is coated on switch cubicle insulating sheath, polypropylene substrate using applicator, busbar heat-shrinkable T bush, cabinet is worn Sleeve pipe, insulation booth, on pole, paint thickness is 300 ~ 850 μm, and room temperature is air-dried.
CN201710458961.0A 2017-06-16 2017-06-16 A kind of preparation method of composite flame-proof coating Active CN107189686B (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107778511A (en) * 2017-11-18 2018-03-09 桂林全州燎原科技有限责任公司 Fire-retardant high polymer material

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101624834A (en) * 2009-07-30 2010-01-13 天津市耀新科技发展有限公司 Antiflaming puncture-resisting water-proof sheet and manufacturing method thereof
CN104130638A (en) * 2014-07-18 2014-11-05 安徽千和新材料科技发展有限公司 Aqueous fire-proof corrosion-proof paint for steel structure and preparation method thereof
CN105694665A (en) * 2016-01-28 2016-06-22 浙江港流高分子科技有限公司 Flame-retardant coiled material and preparation method thereof

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101624834A (en) * 2009-07-30 2010-01-13 天津市耀新科技发展有限公司 Antiflaming puncture-resisting water-proof sheet and manufacturing method thereof
CN104130638A (en) * 2014-07-18 2014-11-05 安徽千和新材料科技发展有限公司 Aqueous fire-proof corrosion-proof paint for steel structure and preparation method thereof
CN105694665A (en) * 2016-01-28 2016-06-22 浙江港流高分子科技有限公司 Flame-retardant coiled material and preparation method thereof

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
周丛等: "阻燃电线套管专用料的研究", 《黑龙江石油化工》 *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107778511A (en) * 2017-11-18 2018-03-09 桂林全州燎原科技有限责任公司 Fire-retardant high polymer material

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