CN105906779A - High-strength flame-retardant modified polyurethane composite material - Google Patents
High-strength flame-retardant modified polyurethane composite material Download PDFInfo
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- CN105906779A CN105906779A CN201610249120.4A CN201610249120A CN105906779A CN 105906779 A CN105906779 A CN 105906779A CN 201610249120 A CN201610249120 A CN 201610249120A CN 105906779 A CN105906779 A CN 105906779A
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Abstract
The invention discloses a high-strength flame-retardant modified polyurethane composite material including: hydroxyl-terminated polybutadiene, polytetrahydrofuran ether glycol, polypropylene glycol, toluene diisocynate, 4,4'-diphenylmethane diisocynate, bisphenol A, dibromoneopentyl glycol, dimethythiotoluene diamine, diaminodiphenylmethane, 2-ethyl-4-methylimidazole, dibutyltin dilaurate, diglycidyl resorcinol ether, a filling material, melamine, ammonium polyphosphate, and N,N'-bis(2-thio-5,5-dimethyl-1,3,2-dioxaphosphocyclohexyl)ethylenediamine. The high-strength flame-retardant modified polyurethane composite material has high strength, is excellent flame-retardant performance and can satisfy use demands in various fields.
Description
Technical field
The present invention relates to polyurethanes technology field, particularly relate to a kind of high-strength fire-retarding modified polyurethane composite.
Background technology
Polyurethane is the general designation on main chain containing the macromolecular compound repeating carbamate groups, has excellent
The characteristics such as different wear-resisting, oil resistant, tear-resistant, resistance to chemical attack, its purposes is very wide, can substitute for rubber,
Plastics, nylon etc., for airport, hotel, building materials, automobile factory, colliery factory, cement plant, condo,
The fields such as villa, landscaping, colored stone art, park.But common polyurethane material easily burns, from
And make its mechanical property drastically decline, during application, there is the biggest fire safety evaluating hidden danger, the big day of one's doom
Make polyurethane material application in practice.
Summary of the invention
The technical problem existed based on background technology, it is multiple that the present invention proposes a kind of high-strength fire-retarding modified polyurethane
Condensation material, its intensity is high, and excellent fireproof performance can meet the use requirement of multiple fields.
A kind of high-strength fire-retarding modified polyurethane composite that the present invention proposes, its raw material includes by weight:
End hydroxy butadiene 20-35 part, PTMG 10-30 part, polypropylene glycol 2-15 part, toluene
Diisocyanate 25-50 part, 4,4 ' methyl diphenylene diisocyanate 20-50 parts, bisphenol-A 2-5 part,
Dibromoneopentyl glycol 2-8 part, dimethythiotoluene diamine 1-2 part, diaminodiphenyl-methane 2-8 part, 2-second
Base-4-methylimidazole 0.01-0.1 part, dibutyl tin laurate 0.01-0.1 part, resorcinol two shrink sweet
Oil ether 10-30 part, filler 10-20 part, tripolycyanamide 2-15 part, APP 1-5 part, N, N'-bis-(2-sulfur
Generation-5,5-dimethyl-1,3,2-dioxy phosphorus heterocycle cyclohexyl) ethylenediamine 8-20 part.
Preferably, in its raw material, end hydroxy butadiene, PTMG, polypropylene glycol, first
Phenylene diisocyanate, the weight ratio of 4,4 ' methyl diphenylene diisocyanates are 25-33:17-26:6-13:
29-44:27-45.
Preferably, in its raw material, tripolycyanamide, APP, N, N'-bis-(2-sulfur generation-5,5-dimethyl
-1,3,2-dioxy phosphorus heterocycle cyclohexyl) weight ratio of ethylenediamine is 5-13:2.8-4.3:10-17.
Preferably, its raw material includes by weight: end hydroxy butadiene 28-32 part, PTMG two
Alcohol 19-23 part, polypropylene glycol 8-12 part, toluene di-isocyanate(TDI) 36-40 part, 4,4 ' diphenyl methanes two
Isocyanates 38-42 part, bisphenol-A 3.8-4.3 part, dibromoneopentyl glycol 5.5-6.2 part, dimethyl sulphur-based toluene
Diamidogen 1.3-1.6 part, diaminodiphenyl-methane 5-6.5 part, 2-ethyl-4-methylimidazole 0.03-0.08 part,
Dibutyl tin laurate 0.02-0.08 part, resorcinolformaldehyde resin 15-22 part, filler 13-17 part,
Tripolycyanamide 9-11 part, APP 3.2-4 part, N, N'-bis-(2-sulfur generation-5,5-dimethyl-1,3,2-dioxy
Phosphorus heterocycle cyclohexyl) ethylenediamine 11-15 part.
Preferably, its raw material includes by weight: end hydroxy butadiene 30 parts, PTMG
20 parts, polypropylene glycol 11 parts, toluene di-isocyanate(TDI) 38.5 parts, 4,4 ' methyl diphenylene diisocyanates
40 parts, bisphenol-A 4.2 parts, dibromoneopentyl glycol 5.9 parts, dimethythiotoluene diamine 1.5 parts, diaminourea two
Phenylmethane 5.7 parts, 2-ethyl-4-methylimidazole 0.05 part, dibutyl tin laurate 0.06 part, isophthalic
Diphenol diglycidyl ether 20 parts, filler 16 parts, tripolycyanamide 10 parts, APP 3.7 parts, N, N'-bis-
(2-sulfur generation-5,5-dimethyl-1,3,2-dioxy phosphorus heterocycle cyclohexyl) ethylenediamine 13.5 parts.
Preferably, the molecular weight of described polypropylene glycol be 500,700,1000,1200,1300,1500,
One or more mixture in 2000.
Preferably, described filler is compounded mix, and described compounded mix is prepared according to following technique: press
2-5 part silane coupler TM551 and 2-10 part anilinomethyl triethoxysilane are added 30-50 part by weight portion
Toluene stirs, be subsequently adding 10-20 part white carbon black, 3-15 part aluminium hydroxide, 2-10 part nano-zinc borate,
3-15 part nano-calcium carbonate, 1-5 part nano titanium oxide, 2-15 part montmorillonite and 3-12 part attapulgite are super
It is stirred at room temperature reaction 3-5h after sound dispersion 5-15min, reacts after terminating through being centrifuged, wash, be dried, grinding
It is milled to below 200 mesh and obtains described compounded mix.
Preferably, described filler is compounded mix, and described compounded mix is prepared according to following technique: press
3.2 parts of silane coupler TM551 and 7 parts of anilinomethyl triethoxysilanes are added in 42 parts of toluene by weight portion
Stir, be subsequently adding 17 parts of white carbon blacks, 12 parts of aluminium hydroxide, 5 parts of nano-zinc borates, 12 parts of nano-calcium carbonates
Calcium, 3.2 parts of nano titanium oxides, 11 parts of montmorillonites and 10 parts of attapulgites, in room after ultrasonic disperse 10min
Temperature lower stirring reaction 3.6h, reaction obtains institute through being centrifuged, wash, be dried, be ground to below 200 mesh after terminating
State compounded mix;In the preparation process of compounded mix, with silane coupler TM551 and anilinomethyl three ethoxy
Base silane is modifying agent, with white carbon black, aluminium hydroxide, nano-zinc borate, nano-calcium carbonate, nanometer titanium dioxide
Titanium, montmorillonite and attapulgite are inorganic filler, and the condition reacted by control makes the hydroxyl that modifying agent hydrolyzes
Base there occurs reaction with the active group of inorganic filler surface, thus introduces in a large number on the surface of inorganic filler
Amino and phenyl ring obtained compounded mix, by compounded mix addition system, in system, be uniformly dispersed,
On the one hand with the dibromoneopentyl glycol in system, tripolycyanamide, APP, N, N'-bis-(2-sulfur generation-5,5-
Dimethyl-1,3,2-dioxy phosphorus heterocycle cyclohexyls) ethylenediamine cooperation, give the anti-flammability that composite is excellent, separately
On the one hand, because introducing substantial amounts of amino on its surface, can react with isocyano and generate urea bond, thus
System is formed new crosslinking points, significantly improves the mechanical property of composite, on the other hand, because of at body
System introduces benzene ring structure, further increases thermostability and the resistance to ag(e)ing of composite.
Preferably, described white carbon black be white carbon black N220, one in white carbon black N330, white carbon black N990, white carbon black N550
Or multiple mixture.
Preferably, the mean diameter of described nano-zinc borate is 20-45nm, the average particle of described nano-calcium carbonate
Footpath is 25-50nm;The mean diameter of described nano titanium oxide is 30-50nm, and specific surface area is 85-120m2/g。
High-strength fire-retarding modified polyurethane composite of the present invention can be according to conventional compound polyurethane material
Preparation technology is prepared from.
High-strength fire-retarding modified polyurethane composite of the present invention, have selected end hydroxy butadiene, poly-four
Hydrogen furan ether glycol, polypropylene glycol, toluene di-isocyanate(TDI) and 4,4 ' methyl diphenylene diisocyanates are
Urethane monomer, the polyurethane obtained has the mechanical strength of brilliance, has the thermostability and resistance to of excellence simultaneously
Aqueous;In N, N'-bis-(2-sulfur generation-5,5-dimethyl-1,3,2-dioxy phosphorus heterocycle cyclohexyls) ethylenediamine addition system,
It is possible not only to produce substantial amounts of acid and promote into charcoal under high temperature action, also can produce substantial amounts of non-combustible simultaneously
Gas, prevents the burning of polyurethane, with tripolycyanamide, APP and chain extender dibromoneopentyl glycol
After cooperation, multiple fire-retardant mode is worked in coordination with, and significantly improves the anti-flammability of composite, coordinates with filler simultaneously
Improve hot strength and the resistance to water of composite, it addition, bisphenol-A, dibromoneopentyl glycol, dimethyl sulphur-based
Toluenediamine, diaminodiphenyl-methane coordinate as chain extender, can improve the crosslinking degree of composite,
Improve the thermostability of composite, there is autocatalysis simultaneously, improve the chain extension speed of composite.
Detailed description of the invention
Below, by specific embodiment, technical scheme is described in detail.
Embodiment 1
A kind of high-strength fire-retarding modified polyurethane composite that the present invention proposes, its raw material includes by weight:
End hydroxy butadiene 20 parts, PTMG 30 parts, polypropylene glycol 2 parts, toluene di-isocyanate(TDI)
50 parts, 4,4 ' methyl diphenylene diisocyanate 20 parts, bisphenol-A 5 parts, dibromoneopentyl glycol 2 parts, two
(methylthiomethyl) diamidogen 2 parts, diaminodiphenyl-methane 2 parts, 2-ethyl-4-methylimidazole 0.1 part, February
Dilaurylate 0.01 part, resorcinolformaldehyde resin 30 parts, filler 10 parts, tripolycyanamide 15 parts,
APP 1 part, N, N'-bis-(2-sulfur generation-5,5-dimethyl-1,3,2-dioxy phosphorus heterocycle cyclohexyl) ethylenediamine 20
Part.
Embodiment 2
A kind of high-strength fire-retarding modified polyurethane composite that the present invention proposes, its raw material includes by weight:
End hydroxy butadiene 35 parts, PTMG 10 parts, polypropylene glycol 15 parts, toluene diisocynate
Ester 25 parts, 4,4 ' methyl diphenylene diisocyanate 50 parts, bisphenol-A 2 parts, dibromoneopentyl glycol 8 parts,
Dimethythiotoluene diamine 1 part, diaminodiphenyl-methane 8 parts, 2-ethyl-4-methylimidazole 0.01 part, two
Dibutyl tin laurate 0.1 part, resorcinolformaldehyde resin 10 parts, filler 20 parts, tripolycyanamide 2 parts,
APP 5 parts, N, N'-bis-(2-sulfur generation-5,5-dimethyl-1,3,2-dioxy phosphorus heterocycle cyclohexyl) ethylenediamine 8 parts.
Embodiment 3
A kind of high-strength fire-retarding modified polyurethane composite that the present invention proposes, its raw material includes by weight:
End hydroxy butadiene 28 parts, PTMG 23 parts, polypropylene glycol 8 parts, toluene di-isocyanate(TDI)
40 parts, 4,4 ' methyl diphenylene diisocyanate 38 parts, bisphenol-A 4.3 parts, dibromoneopentyl glycol 5.5 parts,
Dimethythiotoluene diamine 1.6 parts, diaminodiphenyl-methane 5 parts, 2-ethyl-4-methylimidazole 0.08 part,
Dibutyl tin laurate 0.02 part, resorcinolformaldehyde resin 22 parts, filler 13 parts, tripolycyanamide
11 parts, APP 3.2 parts, N, N'-bis-(2-sulfur generation-5,5-dimethyl-1,3,2-dioxy phosphorus heterocycle cyclohexyl)
Ethylenediamine 15 parts;
Wherein, described filler is compounded mix, and described compounded mix is prepared according to following technique: by weight
2 parts of silane coupler TM551 and 10 parts of anilinomethyl triethoxysilanes are added in 30 parts of toluene by amount part to be stirred
Uniformly, 20 parts of white carbon black N220,15 parts of aluminium hydroxide, 2 parts of nano-zinc borates, 15 parts of nano-calcium carbonates it are subsequently adding
Calcium, 1 part of nano titanium oxide, 15 parts of montmorillonites and 3 parts of attapulgites, after ultrasonic disperse 15min at room temperature
Stirring reaction 3h, reaction obtains described compound through being centrifuged, wash, be dried, be ground to below 200 mesh after terminating
Filler;The mean diameter of described nano-zinc borate is 20nm, and the mean diameter of described nano-calcium carbonate is 50nm;
The mean diameter of described nano titanium oxide is 30nm, and specific surface area is 120m2/g。
Embodiment 4
A kind of high-strength fire-retarding modified polyurethane composite that the present invention proposes, its raw material includes by weight:
End hydroxy butadiene 32 parts, PTMG 19 parts, polypropylene glycol 12 parts, toluene diisocynate
Ester 36 parts, 4,4 ' methyl diphenylene diisocyanate 42 parts, bisphenol-A 3.8 parts, dibromoneopentyl glycol 6.2
Part, dimethythiotoluene diamine 1.3 parts, diaminodiphenyl-methane 6.5 parts, 2-ethyl-4-methylimidazole 0.03
Part, dibutyl tin laurate 0.08 part, resorcinolformaldehyde resin 15 parts, filler 17 parts, trimerization
Cyanamide 9 parts, APP 4 parts, N, N'-bis-(2-sulfur generation-5,5-dimethyl-1,3,2-dioxy phosphorus heterocycle cyclohexyl)
Ethylenediamine 11 parts;
Wherein, described polypropylene glycol be molecular weight be that the polypropylene glycol of 700 and 1000 is by the mixing of 1:3 weight ratio
Thing;
Described filler is compounded mix, and described compounded mix is prepared according to following technique: by weight by 5
Part silane coupler TM551 and 2 parts of anilinomethyl triethoxysilanes 50 parts of toluene of addition stir, so
3 parts of white carbon black N330 of rear addition, 3 parts of white carbon black N990,4 parts of white carbon black N550,3 parts of aluminium hydroxide, 10 parts of nanometer boron
Acid zinc, 3 parts of nano-calcium carbonates, 5 parts of nano titanium oxides, 2 parts of montmorillonites and 12 parts of attapulgites, ultrasonic point
It is stirred at room temperature reaction 5h after dissipating 5min, reacts after terminating through being centrifuged, wash, be dried, be ground to 200 mesh
Hereinafter obtain described compounded mix;Wherein, the mean diameter of described nano-zinc borate is 45nm, described nanometer
The mean diameter of calcium carbonate is 25nm;The mean diameter of described nano titanium oxide is 50nm, and specific surface area is
85m2/g。
Embodiment 5
A kind of high-strength fire-retarding modified polyurethane composite that the present invention proposes, its raw material includes by weight:
End hydroxy butadiene 30 parts, PTMG 20 parts, polypropylene glycol 11 parts, toluene diisocynate
Ester 38.5 parts, 4,4 ' methyl diphenylene diisocyanate 40 parts, bisphenol-A 4.2 parts, dibromoneopentyl glycol
5.9 parts, dimethythiotoluene diamine 1.5 parts, diaminodiphenyl-methane 5.7 parts, 2-ethyl-4-methyl miaow
Azoles 0.05 part, dibutyl tin laurate 0.06 part, resorcinolformaldehyde resin 20 parts, filler 16 parts,
Tripolycyanamide 10 parts, APP 3.7 parts, N, N'-bis-(2-sulfur generation-5,5-dimethyl-1,3,2-dioxy phospha
Cyclohexyl) ethylenediamine 13.5 parts;
Wherein, the molecular weight of described polypropylene glycol is 500;
Described filler is compounded mix, and described compounded mix is prepared according to following technique: by weight will
3.2 parts of silane coupler TM551 and 7 parts of anilinomethyl triethoxysilanes 42 parts of toluene of addition stir,
It is subsequently adding 5 parts of white carbon black N220,8 parts of white carbon black N330,2 parts of white carbon black N990,2 parts of white carbon black N550,12 parts of hydrogen-oxygens
Change aluminum, 5 parts of nano-zinc borates, 12 parts of nano-calcium carbonates, 3.2 parts of nano titanium oxides, 11 parts of montmorillonites and
10 parts of attapulgites, are stirred at room temperature reaction 3.6h after ultrasonic disperse 10min, reaction terminate after through centrifugal,
Wash, be dried, be ground to below 200 mesh and obtain described compounded mix;Wherein, described nano-zinc borate is flat
All particle diameters are 30nm, and the mean diameter of described nano-calcium carbonate is 40nm;Described nano titanium oxide average
Particle diameter is 40nm, and specific surface area is 100m2/g。
The above, the only present invention preferably detailed description of the invention, but protection scope of the present invention not office
Being limited to this, any those familiar with the art is in the technical scope that the invention discloses, according to this
The technical scheme of invention and inventive concept thereof in addition equivalent or change, all should contain the protection in the present invention
Within the scope of.
Claims (10)
1. a high-strength fire-retarding modified polyurethane composite, it is characterised in that its raw material includes by weight:
End hydroxy butadiene 20-35 part, PTMG 10-30 part, polypropylene glycol 2-15 part, toluene
Diisocyanate 25-50 part, 4,4 ' methyl diphenylene diisocyanate 20-50 parts, bisphenol-A 2-5 part,
Dibromoneopentyl glycol 2-8 part, dimethythiotoluene diamine 1-2 part, diaminodiphenyl-methane 2-8 part, 2-
Ethyl-4-methylimidazole 0.01-0.1 part, dibutyl tin laurate 0.01-0.1 part, resorcinol two shrink
Glycerin ether 10-30 part, filler 10-20 part, tripolycyanamide 2-15 part, APP 1-5 part, N, N'-bis-(2-
Sulfur generation-5,5-dimethyl-1,3,2-dioxy phosphorus heterocycle cyclohexyl) ethylenediamine 8-20 part.
High-strength fire-retarding modified polyurethane composite the most according to claim 1, it is characterised in that it is former
In material, end hydroxy butadiene, PTMG, polypropylene glycol, toluene di-isocyanate(TDI), 4,4 '
The weight ratio of methyl diphenylene diisocyanate is 25-33:17-26:6-13:29-44:27-45.
High-strength fire-retarding modified polyurethane composite the most according to claim 1 or claim 2, it is characterised in that its
In raw material, tripolycyanamide, APP, N, N'-bis-(2-sulfur generation-5,5-dimethyl-1,3,2-dioxy phosphas
Cyclohexyl) weight ratio of ethylenediamine is 5-13:2.8-4.3:10-17.
4. according to high-strength fire-retarding modified polyurethane composite according to any one of claim 1-3, its feature
Being, its raw material includes by weight: end hydroxy butadiene 28-32 part, PTMG 19-23
Part, polypropylene glycol 8-12 part, toluene di-isocyanate(TDI) 36-40 part, 4,4 ' diphenylmethane diisocyanates
Ester 38-42 part, bisphenol-A 3.8-4.3 part, dibromoneopentyl glycol 5.5-6.2 part, dimethythiotoluene diamine
1.3-1.6 part, diaminodiphenyl-methane 5-6.5 part, 2-ethyl-4-methylimidazole 0.03-0.08 part, two
Dibutyl tin laurate 0.02-0.08 part, resorcinolformaldehyde resin 15-22 part, filler 13-17 part,
Tripolycyanamide 9-11 part, APP 3.2-4 part, N, N'-bis-(2-sulfur generation-5,5-dimethyl-1,3,2-dioxy
Phosphorus heterocycle cyclohexyl) ethylenediamine 11-15 part.
5. according to high-strength fire-retarding modified polyurethane composite according to any one of claim 1-4, its feature
Being, its raw material includes by weight: end hydroxy butadiene 30 parts, PTMG 20 parts,
Polypropylene glycol 11 parts, toluene di-isocyanate(TDI) 38.5 parts, 4,4 ' methyl diphenylene diisocyanate 40 parts,
Bisphenol-A 4.2 parts, dibromoneopentyl glycol 5.9 parts, dimethythiotoluene diamine 1.5 parts, diamino-diphenyl first
5.7 parts of alkane, 2-ethyl-4-methylimidazole 0.05 part, dibutyl tin laurate 0.06 part, resorcinol two
Glycidyl ether 20 parts, filler 16 parts, tripolycyanamide 10 parts, APP 3.7 parts, N, N'-bis-(2-sulfur generation
-5,5-dimethyl-1,3,2-dioxy phosphorus heterocycle cyclohexyl) ethylenediamine 13.5 parts.
6. according to high-strength fire-retarding modified polyurethane composite according to any one of claim 1-5, its feature
Being, the molecular weight of described polypropylene glycol is in 500,700,1000,1200,1300,1500,2000
One or more mixture.
7. according to high-strength fire-retarding modified polyurethane composite according to any one of claim 1-6, its feature
Being, described filler is compounded mix, and described compounded mix is prepared according to following technique: by weight
2-5 part silane coupler TM551 and 2-10 part anilinomethyl triethoxysilane are added in 30-50 part toluene
Stir, be subsequently adding 10-20 part white carbon black, 3-15 part aluminium hydroxide, 2-10 part nano-zinc borate, 3-15
Part nano-calcium carbonate, 1-5 part nano titanium oxide, 2-15 part montmorillonite and 3-12 part attapulgite, ultrasonic point
It is stirred at room temperature reaction 3-5h after dissipating 5-15min, reacts after terminating through being centrifuged, wash, be dried, being ground to
Described compounded mix is obtained below 200 mesh.
8. according to high-strength fire-retarding modified polyurethane composite according to any one of claim 1-7, its feature
Being, described filler is compounded mix, and described compounded mix is prepared according to following technique: by weight
3.2 parts of silane coupler TM551 and 7 parts of anilinomethyl triethoxysilanes are added in 42 parts of toluene and stirs all
Even, be subsequently adding 17 parts of white carbon blacks, 12 parts of aluminium hydroxide, 5 parts of nano-zinc borates, 12 parts of nano-calcium carbonates, 3.2
Part nano titanium oxide, 11 parts of montmorillonites and 10 parts of attapulgites, be stirred at room temperature after ultrasonic disperse 10min
Reaction 3.6h, reaction obtains described compound fill out through being centrifuged, wash, be dried, be ground to below 200 mesh after terminating
Material.
9. according to high-strength fire-retarding modified polyurethane composite described in claim 7 or 8, it is characterised in that institute
State white carbon black be white carbon black N220, one or more mixing in white carbon black N330, white carbon black N990, white carbon black N550
Thing.
10. according to high-strength fire-retarding modified polyurethane composite according to any one of claim 7-9, its feature
Being, the mean diameter of described nano-zinc borate is 20-45nm, and the mean diameter of described nano-calcium carbonate is
25-50nm;The mean diameter of described nano titanium oxide is 30-50nm, and specific surface area is 85-120m2/g。
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CN107722606A (en) * | 2017-11-08 | 2018-02-23 | 安徽省瑞发复合材料制造有限公司 | A kind of special heat-and corrosion-resistant compound polyurethane material of circuit board |
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