CN108485352A - A kind of expansion type flame-retarding fire prevention water paint of decalescence and preparation method thereof - Google Patents
A kind of expansion type flame-retarding fire prevention water paint of decalescence and preparation method thereof Download PDFInfo
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- CN108485352A CN108485352A CN201810381037.1A CN201810381037A CN108485352A CN 108485352 A CN108485352 A CN 108485352A CN 201810381037 A CN201810381037 A CN 201810381037A CN 108485352 A CN108485352 A CN 108485352A
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- polyethylene glycol
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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
- C09D—COATING 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
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/18—Fireproof paints including high temperature resistant paints
- C09D5/185—Intumescent paints
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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
- C09D—COATING 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
- C09D151/00—Coating compositions based on graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Coating compositions based on derivatives of such polymers
- C09D151/08—Coating compositions based on graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Coating compositions based on derivatives of such polymers grafted on to macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
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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
- C09D—COATING 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
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
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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
- C09D—COATING 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
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/63—Additives non-macromolecular organic
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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
- C09D—COATING 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
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/65—Additives macromolecular
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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
- C09D—COATING 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
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/70—Additives characterised by shape, e.g. fibres, flakes or microspheres
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/32—Phosphorus-containing compounds
- C08K2003/321—Phosphates
- C08K2003/322—Ammonium phosphate
- C08K2003/323—Ammonium polyphosphate
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/32—Phosphorus-containing compounds
- C08K2003/321—Phosphates
- C08K2003/328—Phosphates of heavy metals
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
Abstract
The invention discloses a kind of expansion type flame-retarding of decalescence fire prevention water paints, include each component below by mass fraction：5 35 parts of 35 75 parts of polyethylene glycol phase transformation self-crosslinking acrylic ester filming emulsion, 5 25 parts of galactolipin Intumescent Retardant System and expandable filler material.Latent heat is absorbed using phase-changing energy storage materials such as polyethylene glycol and galactolipins resist temperature rise in fire hazard environment, utilize the burning of the Intumescent Retardant System retarder of the compositions such as ammonium polyphosphate and galactolipin, highly effective flame-retardant fire prevention may be implemented, phase transformation absorb heat it is huge, cooling flameproof effect it is notable, be suitable for furniture, wall, steel construction, automobile, steamer, tunnel fire-retardant fireproof；Coating is charing expanded at 250 DEG C or so, forms expanded foam layer of charcoal, can be effectively heat-insulated oxygen barrier, hinders fuel gas release, small fire is inhibited to develop to form big fire, reduce fire chance of occurrence, reduce fire damage.
Description
Technical field
The invention belongs to a kind of aqueous paintings of the expansion type flame-retarding of functional paint manufacturing field more particularly to decalescence fire prevention
Material and preparation method thereof.
Background technology
Fire-retardant fireproof is the important topic of relationship people life property safety.In various disasters, fire is most frequently, most
Generally threaten one of the major casualty of public security and social development.It is counted according to the Fire-Fighting Bureau under the Ministry of Public Security, 2015, the whole nation connects altogether
Fire 33.8 ten thousand is reported, causes 1742 people death, 1112 people injured, 39.5 hundred million yuan of direct property loss.On May 25th, 2015,
Special fire disaster accident occurs for Pingdingshan City, Henan Province Lushan County health and happiness garden apartment for elderly people, causes 39 people death, 6 people injured,
745.8 square metres of burnt area, 2064.5 ten thousand yuan of direct economic loss, causes extremely severe social influence.
Expansion type flame retardant has three acid source, charcoal source and air source fundamentals.Being generated in 150 DEG C of temperature range acid sources can ester
Change polyalcohol and can be used as the acid of dehydrating agent；At slightly higher temperature, acid and carbon source progress esterification, and the amido in system
Then as the catalyst of esterification, accelerate reaction；System is melted before esterification and in esterification process, is produced in reaction process
Raw non-flammable gases keep the system for being in molten condition expanded foamed, at the same time, polyalcohol and ester dehydration carbonization, shape
At inorganic matter and carbon residue, system further foams；When reaction is nearly completed, system gelatinization and solidification eventually form porous
Foam layer of charcoal.Expanding fire retardant and resin act synergistically the foam layer of charcoal to be formed under Fire Conditions, have heat-insulated, oxygen barrier, suppression
Cigarette, antidrip and other effects, be low cigarette, low toxicity, non-corrosive gas generate green high-efficient flame-retarded technology method.
Phase-change material has the ability for changing its physical state in certain temperature range.By taking solid-liquid phase change as an example, adding
When heat is to fusion temperature, the phase transformation from solid-state to liquid is just generated, during fusing, phase-change material is absorbed and stored a large amount of
Latent heat；When phase-change material cools down, the heat of storage will be dispersed into environment within the scope of certain temperature, be carried out from liquid
To solid reverse transformation.In both phase transition process, stored or release energy is known as latent heat of phase change.Physical state occurs
When variation, the temperature of material itself almost remains unchanged before phase transformation completion, a wide temperature platform is formed, although temperature is not
Become, but the latent heat for absorbing or discharging is quite big.
Chinese invention patent 201410614087.1 discloses a kind of novel water base property expansion heat-insulating, fire-preventing anti-flaming dope,
It is made of color stuffings, coating additive, the water such as filming emulsion, phosphorus-nitrogen-carbon series flame retardant material, titanium dioxide etc..
Chinese invention patent 201310723631.1 discloses a kind of expanded water-based fireproof anti-flaming dope and its preparation side
Method, the expanded water-based fireproof anti-flaming dope include the following raw material according to mass fraction meter：80-90 parts of styrene-acrylic emulsion, trimerization
15-18 parts of cyanamide, 13-15 parts of hydroxymethyl cellulose, 10-12 parts of carbamide, 7-10 parts of nano-titanium dioxide, calgon 8-
12 parts, 2-5 parts of pentaerythrite, 10-16 parts of precipitated calcium carbonate, 0.5-1 parts of microcrystalline wax, 90-95 parts of water.
Chinese invention patent 201410064461.5 discloses a kind of water expansion heat-insulating flame-retardant suppression for woodwork
Cigarette coating, preparation process are：In the modified polyurethane emulsion that mass percent is 25-40%, mass percent, which is added, is
The dispersant of 1-10%, under stirring, hollow glass powder, mass percent that mass percent is 5-15%, which is added, is
The halogen-free expansion fire retardant of 20-35%, mass percent are 0.01-1% antifoaming agent, and after stirring evenly, quality hundred is added
Divide the water than being 0.1-30%, adjust to appropriate viscosity, to which water expansion heat-insulating flame-retardant suppression cigarette coating be made.
Chinese invention patent 201510422702.3 discloses a kind of ultra-thin weather formed steel construction fireproof coating and its preparation
Method, ultra-thin weather formed steel construction fireproof coating include that component and weight ratio are as follows：Base-material 12-20%, Intumescent Retardant System 40-
50%, color stuffing 10-18%, solvent 12-20%, auxiliary agent 2-5%；Intumescent Retardant System includes that component and weight ratio are as follows：It is de-
Water catalyst 42-52%, carbon forming agent 25-45%, foaming agent 10-25%.
Chinese invention patent 200810222372.3 discloses a kind of thermal control paint and preparation method thereof, which is
By in common coating or functional paint add organic inorganic composite phase-change material be made, organic inorganic composite phase-change material be by
Expanded perlite, attapulgite, zeolite or the compound paraffin of sepiolite or octadecane obtain.
Chinese invention patent number 201510056434.8 discloses a kind of phase-change microcapsule type modified building heat-insulating and energy-saving painting
Material and preparation method thereof, including：30-40 parts of water, 0.4-1.0 parts of thickeners, 0.1-0.3 parts of multifunctional assistants, 0.3-1 parts it is anti-ageing
Change auxiliary agent, 0.2-0.5 parts of wetting agents, 0.8-2.0 parts of dispersants, 0.8-1.5 portions of preservatives, 0.4-1.0 parts of mould inhibitors, 0.2-
0.5 part of antifoaming agent, 2-5 parts of coalescents, 10-20 parts of pigment, 4-10 parts of phase-change microcapsules, 30-45 parts of lotions are through being mixed.
The phase-change microcapsule is that the product batch number that Yantai Rui Long chemical technologies Co., Ltd provides is in RL30A, RL25A and RL20A
It is one or more.
Chinese invention patent number 201210064888.6 discloses a kind of phase transformation heat-insulation and heat-preservation interior wall coating, it is characterised in that
Consisting of：Elastic emulsion, water, dispersant, wetting agent, thickener, preservative, hollow polyaminoester microball, nano-titanium dioxide,
Opacifying polymers and water.Wherein, polyethylene glycol has been coated in hollow polyaminoester microball, molecular weight is between 1000-2000.
Chinese invention patent number 201510967146.8 discloses a kind of phase-change coating and the preparation method and application thereof, described
Phase-change coating includes paraffin and montmorillonite Composite phase-change material, filler, adhesive, dispersant, water repellent agent, thickener and water, institute
The paraffin stated is formed with montmorillonite Composite phase-change material by paraffin and montmorillonite Composite.
Although the above research work achieves some gratifying achievements, existing intumescent fire-retardant coating material cannot be in middle low temperature
Temperature rapid increase for range inhibition, and fire protection efficiency is not high, and existing phase-change coating does not have fire-retardant fireproof effect, and therefore, initiative is a kind of
Middle low temperature phase change absorbs heat, the decalescence expandable flame retardant fireproof coating of high-temperature expansion layer of charcoal thermal insulation protection is very important.
Invention content
The technical problem to be solved by the present invention is to overcome the shortcomings of to mention in background above technology and defect, provide one
Low temperature phase change heat absorption inhibits the decalescence expansion type flame-retarding fire prevention of flare, high-temperature expansion layer of charcoal thermal insulation protection internal material in kind
Coating and preparation method thereof is suitable for the fire-retardant fireproof of furniture, wall, steel construction, automobile, steamer, tunnel.
In order to solve the above technical problems, technical solution proposed by the present invention is to provide a kind of expansion type flame-retarding of decalescence
Fire prevention water paint, includes each component below by mass fraction：Polyethylene glycol phase transformation self-crosslinking acrylic ester filming emulsion 35-
75 parts, 5-35 parts of 5-25 parts of galactolipin Intumescent Retardant System and expandable filler material；The polyethylene glycol phase transformation self-crosslinking acrylic
Ester filming emulsion is obtained by polyethylene glycol-4000, acrylic acid and catalyst after acetone soln dissolves heating stirring；The gala
Sugared Intumescent Retardant System includes ammonium polyphosphate, galactolipin, mannitol, pentaerythrite and melamine；The expandable filler material packet
Include expansible graphite, perlite, vermiculite, trbasic zinc phosphate, silane coupling agent, solubilizer polyethylene glycol -400 and water.
The expansion type flame-retarding fire prevention water paint of above-mentioned decalescence, it is preferred that the polyethylene glycol phase transformation self-crosslinking
In acrylate filming emulsion, the mass ratio of polyethylene glycol-4000, acrylic acid and catalyst is 100:(1.6-2.5):(0.05-
0.1)；The catalyst includes dodecyl benzene sulfonic acid or p-methyl benzenesulfonic acid.
Preferably, in the galactolipin Intumescent Retardant System, ammonium polyphosphate, galactolipin, mannitol, pentaerythrite and three
The mass ratio of poly cyanamid is (10-20):(15~35):(5~20):(5-10):(5-20)；The polymerization degree n of the ammonium polyphosphate>
1000。
Preferably, in the expandable filler material, expansible graphite, perlite, vermiculite, trbasic zinc phosphate, silane coupling agent, increasing
The mass ratio of solvent polyethylene glycol-400 and water is (20-30):(20-30):(20-30):(5-7):(5-8):(30-40):
(30-50)。
Preferably, the expansion type flame-retarding fire prevention water paint of the decalescence further includes dispersant, thickener, wetting
One or more of agent, preservative, film forming solvent, antifoaming agent, pigment and water.
The expansion type flame-retarding fire prevention water paint of the decalescence of the present invention, integrated utilization " decalescence inhibition flare ",
Technologies such as " foamed char thermal insulation protections " are absorbed using phase-changing energy storage materials such as polyethylene glycol and galactolipins in fire hazard environment and are dived
Heat resist temperature rise utilizes the burning of the Intumescent Retardant System retarder of the compositions such as ammonium polyphosphate and galactolipin, Ke Yishi
Existing highly effective flame-retardant is prevented fires, and the heat that phase transformation absorbs is huge, cooling flameproof effect is notable, is suitable for furniture, wall, steel construction, vapour
The fire-retardant fireproof of vehicle, steamer, tunnel；Coating is charing expanded at 250 DEG C or so, formed expanded foam layer of charcoal, can effectively every
Heat is oxygen barrier, hinders fuel gas release, small fire is inhibited to develop to form big fire, reduce fire chance of occurrence, reduce fire damage；It applies
The thickness of material is 3.0mm, and the fire resistance period 90-120min of coating, coating expansion multiplying power is 8-25 times, 800 DEG C of residual qualities
For 36-48%.
The present invention is pioneering using galactolipin/mannitol as the carbon source of Intumescent Retardant System, and polyethylene glycol and galactolipin/sweet
Dew alcohol is all phase-changing energy storage material, and the phase transition temperature of polyethylene glycol is 30-60 DEG C, latent heat of phase change 175J/g, the phase transformation of galactolipin
Temperature is 189 DEG C, latent heat of phase change 340J/g, and the phase transition temperature of mannitol is 165 DEG C, latent heat of phase change 326J/g；At 160-190 DEG C
Temperature range, galactolipin/mannitol can resist temperature rise as phase-changing energy storage material by decalescence；On 250 DEG C of left sides
The right side, galactolipin/mannitol can be dehydrated into charcoal reaction as polyol under acid source effect, poly- with melting
Ethylene glycol, galactolipin, mannitol etc. form expanded foam layer of charcoal together, can effectively heat-insulated oxygen barrier obstruction material decomposition combustion.
The present invention makees filler using expansible graphite, perlite and vermiculite, they expand reaction in high temperature sintering,
Absorb the expansion heat of transformation；The expansion of these fillers causes foam layer of charcoal to thicken, heat-blocking action enhancing.
Based on a total technical concept, it is aqueous that the present invention correspondingly provides a kind of expansion type flame-retarding fire prevention of decalescence
The preparation method of coating, includes the following steps：
(1) water, acetone and polyethylene glycol-4000 are mixed, heating to 55~65 DEG C makes its stirring and dissolving, adds
Enter catalyst and first time acrylic acid, continue to be stirred to react after heating to 100~120 DEG C, add second of acrylic acid,
Continue to heat to 130~150 DEG C and continue to be stirred to react, obtains polyethylene glycol phase transformation self-crosslinking acrylic ester after reaction
Filming emulsion；
(2) ammonium polyphosphate, galactolipin, mannitol, pentaerythrite and melamine are sanded after mixing and arrive fineness ＜
50 μm, obtain galactolipin Intumescent Retardant System；
(3) by expansible graphite, perlite, vermiculite, trbasic zinc phosphate, silane coupling agent, solubilizer polyethylene glycol -400 and water
Shearing dispersion is carried out, then carries out being sanded and arrives 50 μm of fineness ＜, filtering obtains expandable filler material；
(4) by one kind in preservative, film forming solvent, thickener, dispersant, antifoaming agent and wetting agent under stirring at low speed
Or it is several into the water, after mixing, by the galactolipin Intumescent Retardant System obtained after the step (2), the step (3)
The expandable filler material and pigment obtained afterwards is added in the vortex stirred, and the step is added after dispersion under stirring at low speed
(1) the polyethylene glycol phase transformation self-crosslinking acrylic ester filming emulsion obtained after adjusts pH value, carries out high shear agitation, uses water
And/or thickener adjusts viscosity, and the expansion type flame-retarding fire prevention water paint when the decalescence is obtained after sieving discharging.
Above-mentioned preparation method, it is preferred that in the step (1), the quality of first time acrylic acid addition and for the second time third
The mass ratio that olefin(e) acid is added is 6-7:3-4 stirs 5~7h, is warming up to 130~150 DEG C and continues to stir after being warming up to 100~120 DEG C
Mix 1~3h of reaction.
Preferably, in the step (3), the time for shearing dispersion is 20-40min.
Preferably, in the step (4), the speed of stirring at low speed is 140~160r/min, the speed of high shear agitation
Time for 800~1200r/min, high shear agitation is 15~25min, and adjustment pH value is 4~6.
Preferably, in the step (4), wetting agent is polyethylene glycol-8 00, and the thickener is polyethylene glycol-1000,
The preservative is 1,2-benzisothiazolin-3-one, and the film forming solvent is acetone, and the dispersant is waterglass, described
Antifoaming agent is dimethyl silicone polymer.
Phase-changing energy storage material polyethylene glycol and acroleic acid polymerization are prepared filming emulsion by the present invention, in normal use situation
Under, polyethylene glycol is the film forming matter in coating；When encountering flame calcination, polyethylene glycol undergoes phase transition heat absorption, resists temperature
Rise, effective protection coating and internal material are not invaded by flame；Polyethylene glycol has the function of various rolls in coating, can
To effectively reduce cost, increase latent heat of phase change, improves fire-retardant fireproof efficiency.
The present invention prepares film forming matter, galactolipin/mannitol as carbon forming agent, poly- second using polyethylene glycol-4000 simultaneously
Glycol -400 makees solubilizer, polyethylene glycol-1000 makees thickener, while using a variety of phase-changing energy storage materials, phase-changing energy storage material
Accounting is more than 50% in the coating, is constituted from 30-200 DEG C of large-scale absorbing and cooling temperature system, thus can under Fire Conditions
Effectively to inhibit the raising of coating and its internal material temperature, material combustion is prevented, fire is avoided；Phase-changing energy storage material structure
At the various ingredients of coating, phase transformation absorb heat it is huge, cooling flameproof effect it is notable；It is one multi-purpose, both reduce raw material
Consumption, reduce cost, and improve the density of decalescence.
Compared with prior art, beneficial effects of the present invention are：
1, the expansion type flame-retarding fire prevention water paint of decalescence of the invention, " decalescence inhibits fire to integrated utilization
The technologies such as seedling ", " foamed char thermal insulation protection " are inhaled in fire hazard environment using phase-changing energy storage materials such as polyethylene glycol and galactolipins
Receiving latent heat resistance temperature rise can using the burning of the Intumescent Retardant System retarder of the compositions such as ammonium polyphosphate and galactolipin
To realize that highly effective flame-retardant is prevented fires, the heat that phase transformation absorbs is huge, cooling flameproof effect is notable, is suitable for furniture, wall, steel knot
The fire-retardant fireproof of structure, automobile, steamer, tunnel；Coating is charing expanded at 250 DEG C or so, forms expanded foam layer of charcoal, can be effective
Ground is heat-insulated oxygen barrier, hinders fuel gas release, small fire is inhibited to develop to form big fire, reduce fire chance of occurrence, reduces fire damage
It loses；The thickness of coating is 3.0mm, and the fire resistance period 90-120min of coating, coating expansion multiplying power is 8-25 times, 800 DEG C of remnants
Quality is 36-48%.
2, phase-changing energy storage material polyethylene glycol and acroleic acid polymerization are prepared filming emulsion by the present invention, in normal use situation
Under, polyethylene glycol is the film forming matter in coating；When encountering flame calcination, polyethylene glycol undergoes phase transition heat absorption, resists temperature
Rise, effective protection coating and internal material are not invaded by flame；Polyethylene glycol has the function of various rolls in coating, can
To effectively reduce cost, increase latent heat of phase change, improves fire-retardant fireproof efficiency.
3, the present invention is pioneering using galactolipin/mannitol as the carbon source of Intumescent Retardant System, and polyethylene glycol and galactolipin/
Mannitol is all phase-changing energy storage material, and the phase transition temperature of polyethylene glycol is 30-60 DEG C, latent heat of phase change 175J/g, the phase of galactolipin
Temperature is 189 DEG C, latent heat of phase change 340J/g, and the phase transition temperature of mannitol is 165 DEG C, latent heat of phase change 326J/g；In 160-190
DEG C temperature range, galactolipin/mannitol can resist temperature rise as phase-changing energy storage material by decalescence；At 250 DEG C
Left and right, galactolipin/mannitol can be dehydrated into charcoal reaction, with melting as polyol under acid source effect
Polyethylene glycol, galactolipin, mannitol etc. form expanded foam layer of charcoal together, can effectively heat-insulated oxygen barrier obstruction material decomposition combustion
It burns.
4, the present invention simultaneously using polyethylene glycol-4000 prepare film forming matter, galactolipin/mannitol as carbon forming agent, gather
Ethylene glycol -400 makees solubilizer, polyethylene glycol-1000 makees thickener, while using a variety of phase-changing energy storage materials, phase-change accumulation energy material
Accounting is more than 50% to material in the coating, is constituted from 30-200 DEG C of large-scale absorbing and cooling temperature system, under Fire Conditions
The raising of coating and its internal material temperature can effectively be inhibited, material combustion is prevented, avoid fire；Phase-changing energy storage material
The various ingredients of coating are constituted, the heat that phase transformation absorbs is huge, cooling flameproof effect is notable；It is one multi-purpose, both reduce former material
The consumption of material reduces cost, and improves the density of decalescence.
5, the present invention makees filler using expansible graphite, perlite and vermiculite, they are expanded instead in high temperature sintering
It answers, absorbs the expansion heat of transformation；The expansion of these fillers causes foam layer of charcoal to thicken, heat-blocking action enhancing.
Specific implementation mode
To facilitate the understanding of the present invention, the present invention is done below in conjunction with preferred embodiment and more comprehensively, is meticulously described,
But protection scope of the present invention is not limited to following specific examples.
Unless otherwise defined, all technical terms used hereinafter are generally understood meaning phase with those skilled in the art
Together.Technical term used herein is intended merely to the purpose of description specific embodiment, is not intended to the limitation present invention's
Protection domain.
Unless otherwise specified, various raw material, reagent, the instrument and equipment etc. used in the present invention can pass through city
Field is commercially available or can be prepared by existing method.
Embodiment 1：
A kind of expansion type flame-retarding fire prevention water paint of the decalescence of the present invention, preparation method include the following steps：
(1) preparation of polyethylene glycol phase transformation self-crosslinking acrylic ester filming emulsion：300kg water and 50kg acetone are added anti-
It answers in kettle, 500kg polyethylene glycol-4000 (4000 be the degree of polymerization of polyethylene glycol) is added, stirring heats to 60 DEG C, stirs
Mix dissolving；0.25kg catalyst dodecyl benzene sulfonic acid (p-methyl benzenesulfonic acid) and 5kg acrylic acid are added, continues to heat to
110 DEG C, it is stirred to react 6h；3kg acrylic acid is added, heats to 140 DEG C, continues to be stirred to react 2h, reaction terminates, and obtains
Polyethylene glycol phase transformation self-crosslinking acrylic ester filming emulsion；
(2) preparation of galactolipin Intumescent Retardant System：By 100kg ammonium polyphosphate APPs (n>1000) (acid source), 150kg half
Lactose, 100kg mannitol and 50kg pentaerythrites (carbon source), 100kg melamines (air source), stirred evenly in sand mill,
50 μm of fineness ＜ is sanded, obtains galactolipin Intumescent Retardant System；
(3) preparation of expandable filler material：By 100kg expansible graphites, 100kg perlites, 100kg vermiculites, 20kg phosphoric acid
Zinc adds 30kg silane coupling As -172,200kg solubilizer polyethylene glycol -400 and 150kg water, is sheared in high speed dispersor
Disperse 20min, is transferred to be sanded in sand mill and arrives 50 μm of fineness ＜, filtered with bag filter, obtain expandable filler material；
(4) 10kg water is put into homogenizer, the poly- second of 2kg thickeners is sequentially added under 150r/min stirring at low speed
Glycol -1000 (1000 be the degree of polymerization of polyethylene glycol), (800 be the polymerization of polyethylene glycol to 3kg wetting agents polyethylene glycol-8 00
Degree), after mixing, prepared by the 20kg galactolipins Intumescent Retardant System of above-mentioned steps (2) preparation, 25kg above-mentioned steps (3)
Expandable filler material be slowly added in the vortex that impeller stirs, after dispersion, be gradually added under 150r/min stirring at low speed
Polyethylene glycol phase transformation self-crosslinking acrylic ester filming emulsion prepared by 50kg above-mentioned steps (1), adjustment pH value is 6, in 1000r/
Min high shear agitation 20min, sieving discharging obtain the expansion type flame-retarding fire prevention water paint of decalescence.
The expansion type flame-retarding fire prevention water paint of the decalescence, is made using polyethylene glycol phase transformation self-crosslinking acrylic ester
Membrane substance, galactolipin make expandable flame retardant carbon source, and a variety of main components of coating are made of phase-changing energy storage material, and phase transformation absorbs
Heat it is huge, cooling flameproof effect it is notable.The expansion type flame-retarding of the decalescence is prevented fires water paint, can be applied to furniture,
The fire-retardant fireproof of interior wall, automobile, steamer, steel construction, tunnel.
Embodiment 2：
A kind of expansion type flame-retarding fire prevention water paint of the decalescence of the present invention, preparation method include the following steps：
(1) preparation of polyethylene glycol phase transformation self-crosslinking acrylic ester filming emulsion：300kg water and 50kg acetone are added anti-
It answers in kettle, 450kg polyethylene glycol-4000 (4000 be the degree of polymerization of polyethylene glycol) is added, stirring heats to 60 DEG C, stirs
Mix dissolving；0.25kg catalyst dodecyl benzene sulfonic acid (p-methyl benzenesulfonic acid) and 5kg acrylic acid are added, continues to heat to
110 DEG C, it is stirred to react 6h；3kg acrylic acid is added, heats to 140 DEG C, continues to be stirred to react 2h, reaction terminates, and obtains
Polyethylene glycol phase transformation self-crosslinking acrylic ester filming emulsion；
(2) preparation of galactolipin Intumescent Retardant System：By 100kg ammonium polyphosphate APPs (n>1000) (acid source), 120kg half
Lactose, 120kg mannitol and 60kg pentaerythrites (carbon source), 100kg melamines (air source), stirred evenly in sand mill,
50 μm of fineness ＜ is sanded, obtains galactolipin Intumescent Retardant System；
(3) preparation of expandable filler material：By 110kg expansible graphites, 90kg perlites, 80kg vermiculites, 20kg trbasic zinc phosphates,
Add 30kg silane coupling As -172,200kg solubilizer polyethylene glycol -400 and 150kg water, dispersion is sheared in high speed dispersor
20min is transferred to be sanded in sand mill and arrives 50 μm of fineness ＜, filtered with bag filter, obtain expandable filler material；
(4) 10kg water is put into homogenizer, the poly- second of 2kg thickeners is sequentially added under 150r/min stirring at low speed
Glycol -1000 (1000 be the degree of polymerization of polyethylene glycol), (800 be the polymerization of polyethylene glycol to 3kg wetting agents polyethylene glycol-8 00
Degree), after mixing, prepared by the 25kg galactolipins Intumescent Retardant System of above-mentioned steps (2) preparation, 20kg above-mentioned steps (3)
Expandable filler material be slowly added in the vortex that impeller stirs, after dispersion, be gradually added under 150r/min stirring at low speed
Polyethylene glycol phase transformation self-crosslinking acrylic ester filming emulsion prepared by 50kg above-mentioned steps (1), adjustment pH value is 6, in 1000r/
Min high shear agitation 20min, sieving discharging obtain the expansion type flame-retarding fire prevention water paint of decalescence.
The expansion type flame-retarding fire prevention water paint of the decalescence, is made using polyethylene glycol phase transformation self-crosslinking acrylic ester
Membrane substance, galactolipin make expandable flame retardant carbon source, and a variety of main components of coating are made of phase-changing energy storage material, and phase transformation absorbs
Heat it is huge, cooling flameproof effect it is notable.The expansion type flame-retarding of the decalescence is prevented fires water paint, can be applied to furniture,
The fire-retardant fireproof of interior wall, automobile, steamer, steel construction, tunnel.
Comparative example：
This comparative example is a kind of manufacturing method of the acrylic resin water paint without phase-changing energy storage material, including following
Step：
(1) 50kg water is added in reaction kettle, 40kg styrene, 20kg acrylic acid is added, stirring heats to 80
DEG C, stirring and dissolving；Add 0.25kg catalyst dodecyl benzene sulfonic acid and 4kg acrylic acid, be added 0.25kg ammonium persulfates after
It is continuous to heat to 110 DEG C, it is stirred to react 6h；1kg acrylic acid is added, heats to 140 DEG C, continues to be stirred to react 2h,
Reaction terminates, and obtains self-crosslinking acrylic ester filming emulsion；
(2) by 10kg ammonium polyphosphate APPs (n>1000) (acid source), 10kg pentaerythrites (carbon source), 10kg melamine (gas
Source), it stirred evenly in sand mill, be sanded and arrive 50 μm of fineness ＜, obtain pentaerythrite Intumescent Retardant System；
(3) by 300kg titanium dioxides, 20kg trbasic zinc phosphates, add 3kg silane coupling A -172,15kg water, in high speed dispersor
Middle shearing disperses 20min, is transferred to be sanded in sand mill and arrives 50 μm of fineness ＜, is filtered with bag filter, obtain titanium dioxide and fill out
Material；
(4) 10kg water is put into homogenizer, 2kg thickener carboxylic first is sequentially added under 150r/min stirring at low speed
Base cellulose, 3kg wetting agent sodium dioctyl sulfosuccinates, after mixing, 20kg seasons penta 4 prepared by above-mentioned steps (2)
Titanium dioxide filler prepared by alcohol Intumescent Retardant System, 25kg above-mentioned steps (3) is slowly added in the vortex that impeller stirs.Dispersion
After, the self-crosslinking acrylic ester film forming breast of 50kg above-mentioned steps (1) preparation is gradually added under 150r/min stirring at low speed
Liquid, adjustment pH value, in 1000r/min high shear agitation 20min, sieving discharging obtains acrylic resin water paint.
Embodiment 1-2 and the water paint performance indicator obtained by this comparative example are as shown in table 1.
Table 1：The fire retardant performance index of acrylic intumescent type water flame-proof paint
By table 1 as it can be seen that the decalescence that embodiment 1 and 2 preparation method using the present invention of embodiment are prepared it is swollen
Swollen type fire-retardant fireproof water paint, for the acrylic resin water paint that comparative example 1 obtains, mean heat capacity, expansion
The indexs such as multiplying power, carbonization time, fire endurance time and carbon yield significantly rise, Heat liberation unit and smoke release significantly under
Drop.This says that phase transformation prepared by the technologies such as integrated utilization of the present invention " decalescence inhibition flare ", " foamed char thermal insulation protection " is inhaled
Anti-flaming dope is thermally expanded, every fire retardant performance index is excellent, and highly effective flame-retardant fire prevention may be implemented.
The foregoing is only a preferred embodiment of the present invention, is not intended to restrict the invention, for the skill of this field
For art personnel, the invention may be variously modified and varied.All within the spirits and principles of the present invention, any made by repair
Change, equivalent replacement, improvement etc., should all be included in the protection scope of the present invention.
Claims (10)
- The water paint 1. expansion type flame-retarding of decalescence a kind of is prevented fires, which is characterized in that by mass fraction include below each Component：35-75 parts of polyethylene glycol phase transformation self-crosslinking acrylic ester filming emulsion, 5-25 parts of galactolipin Intumescent Retardant System and can be swollen Swollen filler 5-35 parts；The polyethylene glycol phase transformation self-crosslinking acrylic ester filming emulsion is by polyethylene glycol-4000, acrylic acid and urges Agent obtains after acetone soln dissolves heating stirring；The galactolipin Intumescent Retardant System includes ammonium polyphosphate, galactolipin, sweet Reveal alcohol, pentaerythrite and melamine；The expandable filler material includes expansible graphite, perlite, vermiculite, trbasic zinc phosphate, silane Coupling agent, solubilizer polyethylene glycol -400 and water.
- 2. the expansion type flame-retarding fire prevention water paint of decalescence according to claim 1, which is characterized in that the poly- second In glycol phase transformation self-crosslinking acrylic ester filming emulsion, the mass ratio of polyethylene glycol-4000, acrylic acid and catalyst is 100: (1.6-2.5):(0.05-0.1)；The catalyst includes dodecyl benzene sulfonic acid or p-methyl benzenesulfonic acid.
- 3. the expansion type flame-retarding fire prevention water paint of decalescence according to claim 1, which is characterized in that the gala In sugared Intumescent Retardant System, ammonium polyphosphate, galactolipin, mannitol, pentaerythrite and melamine mass ratio be (10-20): (15~35):(5~20):(5-10):(5-20)；The polymerization degree n of the ammonium polyphosphate>1000.
- 4. the expansion type flame-retarding fire prevention water paint of decalescence according to claim 1, which is characterized in that described can be swollen In swollen filler, expansible graphite, perlite, vermiculite, trbasic zinc phosphate, silane coupling agent, solubilizer polyethylene glycol -400 and water matter Amount is than being (20-30):(20-30):(20-30):(5-7):(5-8):(30-40):(30-50).
- 5. according to the expansion type flame-retarding of any one of claim 1-4 decalescences fire prevention water paint, which is characterized in that The decalescence expansion type flame-retarding fire prevention water paint further include dispersant, thickener, wetting agent, preservative, film forming it is molten One or more of agent, antifoaming agent, pigment and water.
- 6. a kind of preparation side of the expansion type flame-retarding fire prevention water paint of decalescence as described in any one of claim 1-5 Method includes the following steps：(1) water, acetone and polyethylene glycol-4000 are mixed, heating to 55~65 DEG C makes its stirring and dissolving, addition urge Agent and first time acrylic acid continue to be stirred to react after heating to 100~120 DEG C, add second of acrylic acid, continue It heats to 130~150 DEG C to continue to be stirred to react, obtains polyethylene glycol phase transformation self-crosslinking acrylic ester film forming after reaction Lotion；(2) ammonium polyphosphate, galactolipin, mannitol, pentaerythrite and melamine are sanded after mixing and arrive 50 μm of fineness ＜, Obtain galactolipin Intumescent Retardant System；(3) expansible graphite, perlite, vermiculite, trbasic zinc phosphate, silane coupling agent, solubilizer polyethylene glycol -400 and water are carried out Then shearing dispersion carries out being sanded and arrives 50 μm of fineness ＜, filtering obtains expandable filler material；(4) by one kind in preservative, film forming solvent, thickener, dispersant, antifoaming agent and wetting agent or several under stirring at low speed Kind into the water, after mixing, will obtain after the galactolipin Intumescent Retardant System obtained after the step (2), the step (3) To expandable filler material and pigment be added in the vortex that stirs, after the step (1) is added under stirring at low speed after dispersion Obtained polyethylene glycol phase transformation self-crosslinking acrylic ester filming emulsion adjusts pH value, carries out high shear agitation, with water and/or Thickener adjusts viscosity, and the expansion type flame-retarding fire prevention water paint when the decalescence is obtained after sieving discharging.
- 7. preparation method according to claim 6, which is characterized in that in the step (1), what first time acrylic acid was added The mass ratio that quality and second of acrylic acid are added is 6-7:3-4 stirs 5~7h, is warming up to 130 after being warming up to 100~120 DEG C ~150 DEG C are continued to be stirred to react 1~3h.
- 8. preparation method according to claim 6, which is characterized in that in the step (3), the time for shearing dispersion is 20-40min。
- 9. preparation method according to claim 6, which is characterized in that in the step (4), the speed of stirring at low speed is 140~160r/min, the speed of high shear agitation are 800~1200r/min, time of high shear agitation is 15~ 25min, adjustment pH value are 4~6.
- 10. according to the preparation method described in any one of claim 6-9, which is characterized in that in the step (4), wetting agent For polyethylene glycol-8 00, the thickener is polyethylene glycol-1000, and the preservative is 1,2-benzisothiazolin-3-one, institute It is acetone to state film forming solvent, and the dispersant is waterglass, and the antifoaming agent is dimethyl silicone polymer.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109370290A (en) * | 2018-10-26 | 2019-02-22 | 青岛瑞利特新材料科技有限公司 | A kind of expanded graphite packing outer wall heat-insulating coating and preparation method thereof |
| CN111423757A (en) * | 2020-03-24 | 2020-07-17 | 吉利汽车研究院（宁波）有限公司 | Fireproof coating, preparation method and application thereof, and fireproof coating |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106675304A (en) * | 2016-12-28 | 2017-05-17 | 中南林业科技大学 | Decalescence intumescent flame-retardant fireproof waterborne coating and preparation method thereof |
-
2018
- 2018-04-25 CN CN201810381037.1A patent/CN108485352A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106675304A (en) * | 2016-12-28 | 2017-05-17 | 中南林业科技大学 | Decalescence intumescent flame-retardant fireproof waterborne coating and preparation method thereof |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109370290A (en) * | 2018-10-26 | 2019-02-22 | 青岛瑞利特新材料科技有限公司 | A kind of expanded graphite packing outer wall heat-insulating coating and preparation method thereof |
| CN111423757A (en) * | 2020-03-24 | 2020-07-17 | 吉利汽车研究院（宁波）有限公司 | Fireproof coating, preparation method and application thereof, and fireproof coating |
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