CN108864793A - A kind of expandable flame retardant coating and preparation method thereof - Google Patents
A kind of expandable flame retardant coating and preparation method thereof Download PDFInfo
- Publication number
- CN108864793A CN108864793A CN201810641221.5A CN201810641221A CN108864793A CN 108864793 A CN108864793 A CN 108864793A CN 201810641221 A CN201810641221 A CN 201810641221A CN 108864793 A CN108864793 A CN 108864793A
- Authority
- CN
- China
- Prior art keywords
- flame retardant
- parts
- coating
- retardant coating
- added
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- 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
-
- 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
- C09D183/00—Coating compositions based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Coating compositions based on derivatives of such polymers
- C09D183/04—Polysiloxanes
- C09D183/08—Polysiloxanes containing silicon bound to organic groups containing atoms other than carbon, hydrogen, and oxygen
-
- 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
- C09D4/00—Coating compositions, e.g. paints, varnishes or lacquers, based on organic non-macromolecular compounds having at least one polymerisable carbon-to-carbon unsaturated bond ; Coating compositions, based on monomers of macromolecular compounds of groups C09D183/00 - C09D183/16
-
- 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
- C09D7/20—Diluents or solvents
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/22—Polysiloxanes containing silicon bound to organic groups containing atoms other than carbon, hydrogen and oxygen
- C08G77/26—Polysiloxanes containing silicon bound to organic groups containing atoms other than carbon, hydrogen and oxygen nitrogen-containing groups
-
- 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
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Paints Or Removers (AREA)
- Laminated Bodies (AREA)
Abstract
The invention discloses a kind of expandable flame retardant coatings and preparation method thereof, belong to flame retardant coating technical field.The flame retardant coating is made of raw material from the following weight：Film forming agent：1-2 parts；Miscellaneous -10- phospho hetero phenanthrene -10- the oxide of 9,10- dihydro-9-oxy：4-6 parts；Silane coupling agent：2-3 parts；Ammonium polyphosphate：2-4 parts；Calcium gluconate：1-3 parts；Wetting agent：1-2 parts；Ethyl alcohol：50-120 parts.Film forming agent of the invention, 9, miscellaneous -10- phospho hetero phenanthrene -10- the oxide of 10- dihydro-9-oxy, silane coupling agent play filming function simultaneously, calcium gluconate has good self-expanding under heating condition, the effect of carbon source and gas source is played when compounding with ammonium polyphosphate simultaneously, the coating is using ethyl alcohol as solvent, and raw material is environmentally friendly reagent in whole system, non-hazardous with operator to environment；The coating production is simple, and flame retarding efficiency is high.
Description
Technical field
The present invention relates to a kind of expandable flame retardant coatings and preparation method thereof, belong to flame retardant coating technical field.
Background technique
Engineering plastics are widely used in because of its good hot property, chemical stability, weatherability and high mechanical strength
In daily production and living.But since it easily burns, there is the hidden danger for threatening public safety and social development, seriously limit it
Purposes, therefore it is implemented fire-retardant very urgent.
In recent years, researcher is fire-retardant to engineering plastics to have done a large amount of work, and achieve a large amount of achievement.Its
In most simple, most common mode be that fire retardant is directly added in engineering plastics, melt blending therewith, realize it is fire-retardant, but this
There are drawbacks for one method, such as fire retardant additive amount is very high can be only achieved ideal flame retardant effect, this will certainly seriously destroy work
The mechanical property of engineering plastics.In order to solve these problems, researchers synthesize many efficient flame-retarding agents, though a small amount of additive amount
Significant flame retardant effect can be reached, but still had a certain impact to the mechanical property of engineering plastics.
And flame retardant coating not only has the advantages that highly effective flame-retardant, applicability are wide, but also to the mechanical property shadow of engineering plastics
Sound is little, becomes a kind of fire-retardant means of great development prospect.But flame retardant coating is applied to macromolecule engineering frosting
There is also some problems to be solved, as the binding force of coating and engineering plastics matrix is weak and the flexibility of coating is inadequate.
Main cause has following two：The surface polarity for being firstly because macromolecule engineering plastics is low, hydrophobicity is higher, cause coating with
The binding force of matrix reduces, and is easy to fall off, good flame retardant effect is not achieved；The flexibility of followed by coating is inadequate, be difficult with
Certain macromolecule engineering plastics are adapted, and need to add various ingredients just can make coating keep good flexibility.Therefore, use is fire-retardant
The mode of coating solves the problems, such as the inflammable of macromolecule engineering plastics, needs to consider binding force, the film flexibility of coating and matrix.
Chinese patent CN101962514A discloses " a kind of super-hydrophobic automatic cleaning coating material of long wearing and its preparation
Method ", the coating are configured by nanoparticle, low surface free energy polymer, crosslinking agent, dispersing agent, defoaming agent and levelling agent
It forms.With super-hydrophobicity and self-cleaning performance, preparation process condition is mild, but its flame retardant property is limited, it is not specified that applies
The flexibility and binding force with matrix of layer.
Chinese patent CN102218883A discloses " a kind of Wood plastic boards for applying silicon flame retardant coating ", flame retardant coating tool
Have the advantages that small density, high mechanical strength, air-breathing gas permeability be low, heat-resisting and flame retardant property, while Wood plastic boards burning can be reduced
When the smoke and corrosive gas amount that generate.But its thickness is thicker, and does not refer to flame retardant coating and wood-plastic board in the patent
Binding force between material does not illustrate the flame retardant property of coating yet.
Chinese patent CN106833259A discloses " a kind of frosting flame retardant coating and preparation method thereof ", the fire-retardant painting
Layer is made of film forming agent, fire retardant, curing agent, levelling agent, coupling agent, filler and ethylene glycol monobutyl ether solvent.The coating and poly-
Polypropylene matrix material binding force is strong, not easily to fall off, does not influence the mechanical property of polypropylene matrix material, but its complicated component, behaviour
Make complex steps, and V1 rank is only tested by UL-94, does not have good flame retardant property.
Chinese patent CN105694543B discloses " a kind of flame retardant coating and preparation method thereof ", the flame retardant coating mainly at
It is divided into inorganic filming substance matter and inorganic filler, inorganic filming substance matter Phosphate adhesive, inorganic filler is metal oxide, alkali gold
Belonging to hydroxide and boric acid to form in different quality ratio, this method production cost is low, and it is easy to operate, it is chiefly used in timber and steel
On, the report applied to engineering plastics is unknown.
Chinese patent CN102220066B discloses " a kind of wood plastic composite flame retardant coating containing inorganic fire retardants ",
The flame retardant coating ingredient is by epoxy resin, ethyl alcohol, titanate coupling agent, KH570 silane coupling agent, curing agent, aluminium hydroxide, hydrogen
Magnesia, aluminium oxide, microcapsule red phosphorus, expansible graphite, zinc borate are constituted.The coating is solved because magnalium flame retardant is filled
Expect it is excessively high, make material processing performance or its physical and mechanical property reduce the shortcomings that.Flame-retardant composition is complex, not easy enough,
And the binding force of coating and matrix is not referred in the patent.
Summary of the invention
The present invention is intended to provide a kind of expandable flame retardant coating and preparation method thereof, occurs during the preparation process between each raw material
Reaction, generates a kind of expansible flame retardant coating, and the coating production is simple, has good anti-flammability and flexibility.
Film forming agent of the invention, the miscellaneous -10- phospho hetero phenanthrene -10- oxide of 9,10- dihydro-9-oxy, silane coupling agent rise simultaneously
To filming function, three's collective effect can form high quality and the film forming matter with toughness.Calcium gluconate prepares raw material letter
Singly it is easy to get, production cost is low, and it is environmentally protective, there is good self-expanding under heating condition, it is same when being compounded with ammonium polyphosphate
Good synergistic effect is played in the effect of Shi Fahui carbon source and gas source in Intumescent Retardant System, before wide application
Scape.The coating is using ethyl alcohol as solvent, and all raw materials are environmentally friendly reagent in whole system, to environment and operator
Member is non-hazardous；The coating operation is simple, and flame retarding efficiency is high, and polyacrylic limit oxygen index LOI can be made to reach 34.1% and pass through
UL-94（1.6mm）V0 rank is tested, and does not influence the mechanical property of matrix, can not be fallen off as polypropylene deforms together.
The present invention provides a kind of expandable flame retardant coatings, are made of raw material from the following weight：
1-2 parts of film forming agent；
2-4 parts of ammonium polyphosphate；
4-6 parts of 9,10- dihydro-9-oxy miscellaneous -10- phospho hetero phenanthrene -10- oxide；
2-3 parts of silane coupling agent；
1-3 parts of calcium gluconate；
1-2 parts of wetting agent；
50-120 parts of ethyl alcohol；
Obtained flame-retardant coating is firmly combined with matrix, and adhesion strength can reach 4-5B rank.
Further, the film forming agent is polyvinyl formal acetal, polyvinyl alcohol, polyalkenylalcohols acetal, polyvinyl alcohol
The one or two of butyral or polyvinyl formal；When selecting the two, the mass ratio of the two is 1:1.
Further, the silane coupling agent is γ-glycidyl ether oxygen propyl trimethoxy silicane, 3- aminopropyl
One or both of triethoxysilane, N- aminoethyl-γ-aminopropyltrimethoxysilane；When choosing two kinds, mol ratio
It is 1:1.
Further, the wetting agent is lauryl sodium sulfate, xylitol acid anhydride aliphatic ester, polyoxyethylene sorbitan mountain
One or both of pears alcohol monoleate, polyoxyethylene fatty acid esters or polyethylene glycol oxide alkyl phenyl ether；Choose two kinds
When, quality proportioning 1:1.
The present invention provides the preparation methods of above-mentioned expandable flame retardant coating, include the following steps：
（1）Ethyl alcohol is added in beaker, control mixing speed is 800-1000r/min, and film forming agent is then added, continues after adding
Stir 10-15min；
（2）Add 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide under 800-1000r/min stirring, persistently stirs 5-
10min；
（3）It is added with stirring ammonium polyphosphate in 800-1000r/min, persistently stirs 10-20min；
（4）At a temperature of 70 °C ~ 75 °C, silane coupling agent is added into above-mentioned solution, constant temperature stirs 10-30min；
（5）To step（4）Calcium gluconate is added in resulting mixing liquid, 20-30min is sufficiently stirred；
（6）Again to step（5）Middle addition wetting agent, adjust mixing speed be 400-600r/min, the item that temperature is 80-100 °C
Under part, make ethanol evaporation, until stopping heating when slurry viscosity reaches 350-400 mPas；
（7）Take step（6）Sticky flame retardant paste by film applicator be coated in matrix on.
Further, the matrix is one of plastics batten, paper, timber or metal material.
Further, the plastics batten is one of polypropylene, polyethylene, polystyrene or polyester plastics.
In the above method, the coating layer thickness prepared is 1-400 μm.
Beneficial effects of the present invention：
（1）Work of the coating in film forming agent, the miscellaneous -10- phospho hetero phenanthrene -10- oxide of 9,10- dihydro-9-oxy and silane coupling agent
Under, the flexible high adhesion strength coating of densification is formed, coating is made to be achieved with excellent flame retardant effect in the lower situation of thickness；
（2）The coating has good cohesive force, can be firmly adhered to engineering plastics such as polypropylene, polyethylene, polyphenyl second
The surfaces such as alkene, polyester have good ageing-resistant property such as water resistance, ultra-violet resistance matter；
（3）The coating is little to the Effect on Mechanical Properties of matrix, and flame retardant coating flexibility with higher and adhesion strength, in base
Body deform when can deformation occurs together with matrix, will not fall off because of fracture；
（4）Using ethyl alcohol as solvent in the coating preparation process, while flame retardant coating can be dissolved in ethyl alcohol, thus realize matrix with
Recycling is separately recovered in fire retardant, does not have any harm to environment；
（5）The coating preparation process is simple and easy, only needs to dry in baking oven when being applied to matrix surface, not need ultraviolet
Solidification, preparation method are simple, it is easy to accomplish industrialized production；
（6）The coating is applicable not only to engineering plastics, can also be applied to the fire-retardant of timber, steel and fabric etc..
Detailed description of the invention
Fig. 1 be 1 gained PP/ expandable flame retardant coating of embodiment, various sample under different coating layer thicknesses, oxygen index (OI)
Change curve.
Fig. 2 is 1 gained PP/ expandable flame retardant coating of embodiment, and various sample is under different coating layer thicknesses, vertical combustion
Fire-retardant rank figure.
Fig. 3 is the heat release rate curve of 1 gained PP/ expandable flame retardant coating various sample taper calorimetric of embodiment test.
Fig. 4 is after 1 gained PP/ expandable flame retardant coating taper calorimetric of embodiment test taper calorimetric is tested into charcoal macrograph
Picture（A, a1Carbon residue top view and main view digital photograph respectively after the taper calorimetric of PP/ expandable flame retardant coating）And micro image
（B, b1Different amplification figure under layer of charcoal scanning electron microscope respectively after the taper calorimetric of PP/ expandable flame retardant coating, wherein b: ×
500, b1: ×2000）.
Fig. 5 is photo after 1 gained expandable flame retardant coating of embodiment and the test of polypropylene surface adhesion strength.
Fig. 6 is 1 gained PP/ expandable flame retardant coating various sample of embodiment under identical coating layer thickness, tensile strength
Change curve.
Specific embodiment
The present invention is further illustrated below by embodiment, but is not limited to following embodiment.
Embodiment 1：
50 parts of ethyl alcohol are added in beaker, 2 parts of film forming agent are added under the stirring condition of 800r/min, respectively polyvinyl alcohol contracts
First and second aldehyde and polyvinyl formal（The two mass ratio 1：1）, continue to stir 10min after adding；4 are added under same revolving speed
Part miscellaneous -10- phospho hetero phenanthrene -10- oxide of 9,10- dihydro-9-oxy persistently stirs 5min；Then 3 parts of poly- phosphorus under same revolving speed
Sour ammonium, persistently stirs 10min；Under 70 °C, 25 parts of silane coupling agents are added into above-mentioned solution：N- aminoethyl-γ-aminopropyl
Trimethoxy silane and 3-aminopropyltriethoxysilane（The two molar ratio 1：1）, constant temperature stirring 10min；It is mixed to resulting
It closes and 2 parts of calcium gluconates is added in liquid, 20min is sufficiently stirred；Add under the stirring condition of 400r/min into the above solution
Enter 1 part of wetting agent, in the case where temperature is 80 °C, make ethanol evaporation, until stopping heating when viscous pasty state.
Viscous paste is coated on polypropylene batten by film applicator, then dries, coating expansible can be prepared
The PP composite material of flame retardant coating, the coating layer thickness that is related to is 40 μm -200 μm in the present invention.By changing film applicator
The thickness of spin coating revolving speed and time control coating is to obtain polypropylene/expansible flame retardant coating composite wood of different-thickness
Material.The method is also suitble in the frostings prepares coating such as metal and polyethylene, polystyrene, polyester.
1g is represented for every part in the embodiment of the present invention.
During above-mentioned prepares coating, under identical preparation condition, change adding for calcium gluconate and ammonium polyphosphate
Add ratio, obtains sample 1-4.Ammonium polyphosphate and the adding proportion of calcium gluconate are respectively 1 in sample 1-4:2,1:1,2:
1,3:1, different performance tests is carried out for sample 1-4, as shown in Figure 1 and 2.
Fig. 1 is four kinds of samples of gained PP/ expansible flame retardant coating or more under different coating layer thicknesses, oxygen index (OI)
Change curve.It can be seen from the figure that oxygen index (OI) is improved with the increase of thickness when coating composition is identical；When painting thickness
When spending identical, oxygen index (OI) is improved as ammonium polyphosphate and calcium gluconate adding proportion increase.When ammonium polyphosphate and glucose
Sour calcium adding proportion is 3:1, when coating layer thickness is 220 μm, oxygen index (OI) reaches 34.1%, is indicated above novel swollen in the present invention
Swollen flame retardant coating has good anti-flammability.
Fig. 2 is four kinds of samples of gained PP/ expansible flame retardant coating or more under different coating layer thicknesses, vertical combustion
Datagram.
Fig. 3 is that the heat release rate curve of 1 gained PP/ expansible flame retardant coating taper calorimetric of embodiment test is released from heat
It puts in curve as can be seen that the hot rate peak value of sample 1-4 and virgin pp peak value are substantially reduced very much, and have all delayed to reach
The time of peak value, this is highly beneficial for fire rescue and personnel's relief.
Fig. 4 is after 1 gained PP/ expansible flame retardant coating taper calorimetric of embodiment is tested into charcoal both macro and micro figure
Picture.As can be seen from the figure burn after layer of charcoal, not only dilatancy is good, and institute it is closely knit at layer of charcoal, can reach well every
Hot anoxybiotic effect.
Fig. 5 is photo after 1 gained expansible flame retardant coating of embodiment and the test of polypropylene surface adhesion strength.To this implementation
Example gained PP/ expansible flame retardant coating carries out adhesion strength test, and reference standard ASTM D3359-09 uses 3M adhesive tape adhesion strength
Method of testing tests the adhesion strength between coating and matrix, and as can be seen from the figure the edge of notch is all very smooth, without one
A grid falls off, therefore the adhesiveness of the coating can achieve 5B rank, and flame retardant coating can be firmly adhered to polypropylene surface.
Fig. 6 is four kinds of samples of gained PP/ expansible flame retardant coating or more under identical coating layer thickness, ess-strain
Curve.It can be seen from the figure that the tensile strength of the tensile strength of sample 1-4, elongation at break and virgin pp is close, stress
Strain curve is very close, this shows that flame retardant coating does not have any influence for the mechanical property of matrix.
Embodiment 2
80 parts of ethyl alcohol are added in beaker, 2 parts of polyvinyl formal are added under the stirring condition of 900r/min, adds subsequent
Continuous stirring 15min；Miscellaneous -10- phospho hetero phenanthrene -10- the oxide of 5 parts of 9,10- dihydro-9-oxies is added under same revolving speed persistently to stir
8min；Then 2 parts of ammonium polyphosphate under same revolving speed, persistently stir 15min；Under 70 °C, 25 are added into above-mentioned solution
Part silane coupling agent：γ-glycidyl ether oxygen propyl trimethoxy silicane and 3-aminopropyltriethoxysilane（The two mole
Than 1：1）, constant temperature stirring 10min；1 part of above-mentioned calcium gluconate is added into resulting mixing liquid, 30min is sufficiently stirred；?
1 part of wetting agent is added under the stirring condition of 400r/min into the above solution, in the case where temperature is 90 °C, steams ethyl alcohol
Hair, until stopping heating when viscous pasty state.
Viscous paste is coated in polyester spline surfaces by film applicator, then dries, coating expansible can be prepared
The polyester composite of flame retardant coating, the coating layer thickness that is related to is 30 μm -400 μm in the present invention.By changing film applicator rotation
The thickness of revolving speed and time control coating is applied to obtain polyester/expansible flame retardant coating composite material of different-thickness.
Embodiment 3
100 parts of ethyl alcohol are added in beaker, 2 parts of polyvinyl formal acetal are added under the stirring condition of 1000r/min, adds
After continue stir 15min；Miscellaneous -10- phospho hetero phenanthrene -10- the oxide of 6 parts of 9,10- dihydro-9-oxies is added under same revolving speed to continue
Stir 10min；Then 3 parts of ammonium polyphosphate under same revolving speed, persistently stir 15min；Under 75 °C, add into above-mentioned solution
Enter 30 parts of silane coupling agent γ-glycidyl ether oxygen propyl trimethoxy silicanes and N- aminoethyl-γ-aminopropyl trimethoxy silicon
Alkane（The two molar ratio 1：1）, constant temperature stirring 20min；1 part of above-mentioned calcium gluconate is added into resulting mixing liquid, sufficiently
Stir 20min；1 part of wetting agent is added into the above solution under the stirring condition of 500r/min, the case where temperature is 100 °C
Under, make ethanol evaporation, until stopping heating when viscous pasty state.
Viscous paste is coated in metal spline surfaces by film applicator, then dries, coating expansible can be prepared
The metallic composite of flame retardant coating coating, the coating layer thickness that is related to is 5 μm -80 μm in the present invention.By changing film applicator
The thickness of spin coating revolving speed and time control coating is to obtain metal/expansible flame retardant coating composite material of different-thickness.
Embodiment 4
120 parts of ethyl alcohol are added in beaker, 2 parts of film forming agents are added under the stirring condition of 1000r/min：Polyvinyl alcohol contracting first and second
Aldehyde and polyvinyl butyral（The two mass ratio 1：1）, continue to stir 15min after adding；6 part 9 is added under same revolving speed,
Miscellaneous -10- phospho hetero phenanthrene -10- the oxide of 10- dihydro-9-oxy persistently stirs 5min；Then 2 parts of poly- phosphorus are added under same revolving speed
Sour ammonium, persistently stirs 20min；Under 75 °C, 30 parts of silane coupling agent 3- aminopropyl triethoxies are added into above-mentioned solution
Silane, constant temperature stir 30min；3 parts of calcium gluconates are added into resulting mixing liquid, stir 25min；400r/min's
2 parts of wetting agents are added under stirring condition into the above solution, in the case where temperature is 100 °C, make ethanol evaporation, until sticky
Stop heating when state.
Viscous paste is coated in timber spline surfaces by film applicator, then dries, coating expansible can be prepared
The Wood composite material of flame retardant coating, the coating layer thickness that is related to is 100 μm of -0.3mm in the present invention.By changing film applicator rotation
The thickness of revolving speed and time control coating is applied to obtain timber/expansible flame retardant coating composite material of different-thickness.
Embodiment 5
100 parts of ethyl alcohol are added in beaker, 1 part of film forming agent is added under the stirring condition of 950r/min：Polyvinyl formal
With polyvinyl butyral（The two mass ratio 1：1）, continue to stir 10min after adding；4 part 9 is added under same revolving speed,
Miscellaneous -10- phospho hetero phenanthrene -10- the oxide of 10- dihydro-9-oxy persistently stirs 10min；Then 4 parts of poly- phosphorus are added under same revolving speed
Sour ammonium, persistently stirs 30min；Under 70 °C, 10 parts of silane coupling agents are added into above-mentioned solution：γ-glycidyl ether oxygen third
Base trimethoxy silane and 3-aminopropyltriethoxysilane（The two molar ratio 1：1）, constant temperature stirring 30min；To resulting
1 part of calcium gluconate is added in mixing liquid, 20min is sufficiently stirred；Under the stirring condition of 600r/min into the above solution
1 part of wetting agent is added, in the case where temperature is 80 °C, makes ethanol evaporation, until stopping heating when viscous pasty state.
Thick slurry is coated in paper surface by film applicator, is then dried, so that it is fire-retardant to obtain paper/expansible
Coating, coating layer thickness are 1 μm -15 μm.Coating layer thickness can be controlled by changing film applicator spin coating revolving speed and time.
Claims (8)
1. a kind of expandable flame retardant coating, it is characterised in that：It is made of raw material from the following weight：
1-2 parts of film forming agent；
2-4 parts of ammonium polyphosphate；
4-6 parts of 9,10- dihydro-9-oxy miscellaneous -10- phospho hetero phenanthrene -10- oxide；
2-3 parts of silane coupling agent；
1-3 parts of calcium gluconate；
1-2 parts of wetting agent；
50-120 parts of ethyl alcohol.
2. expandable flame retardant coating according to claim 1, it is characterised in that：Obtained flame-retardant coating layer thickness is 1-400 μm, resistance
Combustion coating is firmly combined with matrix, and adhesion strength can reach 4-5B rank.
3. expandable flame retardant coating according to claim 1, it is characterised in that：The film forming agent is polyvinyl alcohol contracting first and second
The one or two of aldehyde, polyvinyl alcohol, polyalkenylalcohols acetal, polyvinyl butyral or polyvinyl formal；When selection two
When person, the mass ratio of the two is 1:1.
4. expandable flame retardant coating according to claim 1, it is characterised in that：The silane coupling agent is that γ-shrink is sweet
Oily ether oxygen propyl trimethoxy silicane, 3-aminopropyltriethoxysilane, N- aminoethyl-γ-aminopropyltrimethoxysilane
One or both of；When choosing two kinds, mol ratio 1:1.
5. expandable flame retardant coating according to claim 1, it is characterised in that：The wetting agent is dodecyl sulphate
Sodium, xylitol acid anhydride aliphatic ester, polyoxyethylene 20 sorbitan monooleate, polyoxyethylene fatty acid esters or polyethylene glycol oxide
One or both of alkyl phenyl ether；When choosing two kinds, quality proportioning 1:1.
6. a kind of preparation method of the described in any item expandable flame retardant coatings of claim 1 ~ 5, it is characterised in that：Including following step
Suddenly：
（1）Ethyl alcohol is added in beaker, control mixing speed is 800-1000r/min, and film forming agent is then added, continues after adding
Stir 10-15min；
（2）Add 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide under 800-1000r/min stirring, persistently stirs 5-
10min；
（3）It is added with stirring ammonium polyphosphate in 800-1000r/min, persistently stirs 10-20min；
（4）At a temperature of 70 °C ~ 75 °C, silane coupling agent is added into above-mentioned solution, constant temperature stirs 10-30min；
（5）To step（4）Calcium gluconate is added in resulting mixing liquid, 20-30min is sufficiently stirred；
（6）Again to step（5）Middle addition wetting agent, adjust mixing speed be 400-600r/min, the item that temperature is 80-100 °C
Under part, make ethanol evaporation, until stopping heating when slurry viscosity reaches 350 ~ 400 mPas；
（7）Take step（6）Sticky fire retardant slurries by film applicator be coated in matrix on.
7. the preparation method of expandable flame retardant coating according to claim 6, it is characterised in that：The matrix is plastic-like
One of item, paper, timber or metal material.
8. the preparation method of expandable flame retardant coating according to claim 7, it is characterised in that：The plastics batten is poly- third
One of alkene, polyethylene, polystyrene or polyester plastics.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810641221.5A CN108864793A (en) | 2018-06-21 | 2018-06-21 | A kind of expandable flame retardant coating and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810641221.5A CN108864793A (en) | 2018-06-21 | 2018-06-21 | A kind of expandable flame retardant coating and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN108864793A true CN108864793A (en) | 2018-11-23 |
Family
ID=64340123
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810641221.5A Pending CN108864793A (en) | 2018-06-21 | 2018-06-21 | A kind of expandable flame retardant coating and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN108864793A (en) |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109535461A (en) * | 2018-11-30 | 2019-03-29 | 成都其其小数科技有限公司 | A kind of preparation method of the gradient flame retardant coating for frosting |
| CN110733093A (en) * | 2019-10-25 | 2020-01-31 | 毛克升 | fir flame-retardant modification treatment method |
| CN110982155A (en) * | 2019-12-24 | 2020-04-10 | 远东电缆有限公司 | Halogen-free phosphorus-free flame-retardant thermoplastic alloy and preparation method thereof |
| CN113045800A (en) * | 2021-04-06 | 2021-06-29 | 什邡市太丰新型阻燃剂有限责任公司 | Novel flame retardant based on APP and DOPO and preparation method thereof |
| CN114653563A (en) * | 2022-02-11 | 2022-06-24 | 北新国际木业有限公司 | Surface flame-retardant treatment method for OSB (oriented strand board) and flame-retardant OSB |
| CN116790157A (en) * | 2023-06-29 | 2023-09-22 | 华鼎国联四川电池材料有限公司 | Flame-retardant protective film based on polyethylene and intumescent flame retardant, and preparation method and application thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102220066A (en) * | 2011-05-16 | 2011-10-19 | 南京赢嘉包装有限责任公司 | Wood-plastic composite inflaming-retarding coating containing inorganic fire retardant |
| CN106189566A (en) * | 2016-07-25 | 2016-12-07 | 太原理工大学 | A kind of expandable flame retardant coating for engineering plastic surface and preparation method thereof |
| CN108084660A (en) * | 2017-12-27 | 2018-05-29 | 福建师范大学 | A kind of expansion type fire retarding epoxide resin and preparation method thereof |
-
2018
- 2018-06-21 CN CN201810641221.5A patent/CN108864793A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102220066A (en) * | 2011-05-16 | 2011-10-19 | 南京赢嘉包装有限责任公司 | Wood-plastic composite inflaming-retarding coating containing inorganic fire retardant |
| CN106189566A (en) * | 2016-07-25 | 2016-12-07 | 太原理工大学 | A kind of expandable flame retardant coating for engineering plastic surface and preparation method thereof |
| CN108084660A (en) * | 2017-12-27 | 2018-05-29 | 福建师范大学 | A kind of expansion type fire retarding epoxide resin and preparation method thereof |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109535461A (en) * | 2018-11-30 | 2019-03-29 | 成都其其小数科技有限公司 | A kind of preparation method of the gradient flame retardant coating for frosting |
| CN110733093A (en) * | 2019-10-25 | 2020-01-31 | 毛克升 | fir flame-retardant modification treatment method |
| CN110982155A (en) * | 2019-12-24 | 2020-04-10 | 远东电缆有限公司 | Halogen-free phosphorus-free flame-retardant thermoplastic alloy and preparation method thereof |
| CN113045800A (en) * | 2021-04-06 | 2021-06-29 | 什邡市太丰新型阻燃剂有限责任公司 | Novel flame retardant based on APP and DOPO and preparation method thereof |
| CN114653563A (en) * | 2022-02-11 | 2022-06-24 | 北新国际木业有限公司 | Surface flame-retardant treatment method for OSB (oriented strand board) and flame-retardant OSB |
| CN116790157A (en) * | 2023-06-29 | 2023-09-22 | 华鼎国联四川电池材料有限公司 | Flame-retardant protective film based on polyethylene and intumescent flame retardant, and preparation method and application thereof |
| CN116790157B (en) * | 2023-06-29 | 2024-05-07 | 华鼎国联四川电池材料有限公司 | Flame-retardant protective film based on polyethylene and intumescent flame retardant, and preparation method and application thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN108864793A (en) | A kind of expandable flame retardant coating and preparation method thereof | |
| CN101654604B (en) | Composition of acrylic pressure-sensitive adhesive and surface finishing material comprising the same | |
| CN106700920B (en) | A kind of response type polysiloxanes flame retardant coating and preparation method thereof | |
| US3301804A (en) | Aqueous emulsion comprising reaction product of liquid epoxy resin and amino boric acid ester | |
| US9133617B2 (en) | Intumescent coating compositions | |
| US8536263B2 (en) | Polyurethane-acrylic polymer dispersions and uses thereof | |
| WO2014009298A2 (en) | Two component cement composition | |
| JPS6372781A (en) | Mastic and coking composition and composite article | |
| CN101817906A (en) | Aqueous acrylic acid series wooden ware sealing paint and method for preparing special emulsion thereof | |
| CN101323727A (en) | Environment-friendly aqueous expansion type fireproof coating and preparation thereof | |
| CN105246690A (en) | Plate carrier having a grid pattern for a self-inking stamp and production method | |
| CN101445681A (en) | Aqueous emulsion copolymer compositions | |
| CN104371508A (en) | Weather-resistant coating composite film | |
| GB2070635A (en) | Highly filled crosslinkable polymer emulsions | |
| CN110577803B (en) | Flame-retardant pressure-sensitive adhesive, flame-retardant pressure-sensitive adhesive sheet and preparation method thereof | |
| JP2004323558A (en) | Aqueous sealer composition | |
| JP3218359B2 (en) | Foamed refractory laminate and method of forming the same | |
| CN101445682A (en) | Aqueous composition with homopolymer | |
| US2902459A (en) | Aqueous dispersion containing oxidizing acid, phenol-aldehyde resin, and polymer of vinyl acetate | |
| CN101210111B (en) | Organic/inorganic composite material and fire-proof plate containing the same | |
| CN105238322A (en) | Interpenetrated network structural type aqueous polyurethane for medicine packaging and preparation method thereof | |
| CN105131673B (en) | A kind of ultraviolet cured flame-retardant primer base and preparation method thereof | |
| JP2013006932A (en) | Resin composition for sealer | |
| Mustapa et al. | Performance of palm oil clinker as a bio-filler with hybrid fillers in intumescent fire protective coatings for steel | |
| CN116218355A (en) | Preparation method of self-cleaning environment-friendly water-based inorganic flame-retardant luminescent coating |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20181123 |
|
| RJ01 | Rejection of invention patent application after publication |