CN106589458A - Flame retardant, application of flame retardant, flame-retardant polyurethane foam and preparation method of flame-retardant polyurethane foam - Google Patents

Flame retardant, application of flame retardant, flame-retardant polyurethane foam and preparation method of flame-retardant polyurethane foam Download PDF

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CN106589458A
CN106589458A CN201611128268.9A CN201611128268A CN106589458A CN 106589458 A CN106589458 A CN 106589458A CN 201611128268 A CN201611128268 A CN 201611128268A CN 106589458 A CN106589458 A CN 106589458A
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weight
flyash
fire retardant
polyurethane foam
retardant
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CN106589458B (en
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董阳
卓锦德
赖世燿
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China Energy Investment Corp Ltd
National Institute of Clean and Low Carbon Energy
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Shenhua Group Corp Ltd
National Institute of Clean and Low Carbon Energy
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K7/00Use of ingredients characterised by shape
    • C08K7/22Expanded, porous or hollow particles
    • C08K7/24Expanded, porous or hollow particles inorganic
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00Polymeric products of isocyanates or isothiocyanates
    • C08G18/06Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/28Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
    • C08G18/40High-molecular-weight compounds
    • C08G18/48Polyethers
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J9/00Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
    • C08J9/04Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent
    • C08J9/12Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a physical blowing agent
    • C08J9/14Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a physical blowing agent organic
    • C08J9/141Hydrocarbons
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/18Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20Oxides; Hydroxides
    • C08K3/22Oxides; Hydroxides of metals
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/34Silicon-containing compounds
    • C08K3/36Silica
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G2110/00Foam properties
    • C08G2110/0083Foam properties prepared using water as the sole blowing agent
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2203/00Foams characterized by the expanding agent
    • C08J2203/14Saturated hydrocarbons, e.g. butane; Unspecified hydrocarbons
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2375/00Characterised by the use of polyureas or polyurethanes; Derivatives of such polymers
    • C08J2375/04Polyurethanes
    • C08J2375/08Polyurethanes from polyethers
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/18Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20Oxides; Hydroxides
    • C08K3/22Oxides; Hydroxides of metals
    • C08K2003/2227Oxides; Hydroxides of metals of aluminium
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00Properties
    • C08L2201/02Flame or fire retardant/resistant
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2203/00Applications
    • C08L2203/14Applications used for foams

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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Polyurethanes Or Polyureas (AREA)
  • Compositions Of Macromolecular Compounds (AREA)

Abstract

The invention relates to the field of polyurethane foam flame retarding, and discloses a flame retardant, application of the flame retardant, flame-retardant polyurethane foam and a preparation method of the flame-retardant polyurethane foam. The flame retardant contains expandable graphite and pulverized fuel ash, and the weight ratio of the expandable graphite to the pulverized fuel ash is (1-5):1. The flame-retardant polyurethane foam provided and obtained through the pulverized fuel ash has the excellent flame retardant property.

Description

A kind of fire retardant and its application and resistance combustion polyurethane foam and preparation method thereof
Technical field
The present invention relates to polyurethane foam flame retardant area, in particular it relates to a kind of fire retardant and its in polyurethane foam Application, a kind of and resistance combustion polyurethane foam and preparation method thereof.
Background technology
RPUF is a kind of macromolecular material with excellent thermal insulation effect, high specific strength, extensively should For the industry such as build, freeze.
The fire retardant for being generally used for improving flame retardant of plastic performance is halogen containing flame-retardant, but at present people recognize such resistance Combustion agent causes serious harm to environmental and biological materials.Therefore halogen-free flame retardants how is provided for RPUF It is fire-retardant to become study hotspot.
《Research of the expansible graphite in hard polyurethane foams fire resistance》(Hu Xingsheng, Hao Jianwei, plastics, 2004 The phase of volume 33 the 1st year, 45-47 page) fire resistance of the expansible graphite in rigid polyurethane foam has been investigated, referred to using oxygen Number have studied expansible graphite and APP (APP), triethyl phosphate (TEP), tripolycyanamide (MA), tripolycyanamide cyanurate Fire retardation of the salt (MCA) to polyurethane foam.
《The Effects of Intumescent Flame Retardant Including Ammonium Polyphosphae/Pentaerythritol and Fly Ash Fillers on the Physicomechanical Properties of Rigid Polyurethane Foams》(Ali Riza Tarakcilar,Journal of Applied Polymer Science, Vol.120,2095-2102 (2011)) APP is reported with tetramethylolmethane expansion System is used cooperatively with the flyash of 5wt%, the fire resistance to rigid polyurethane foam.
But remain a need for how making good use of flyash, there is provided the polyurethane foam with more preferable fire resistance.
The content of the invention
The invention aims to make polyurethane foam that there is better flame resistance and powder is made good use of using flyash Coal ash, there is provided a kind of fire retardant and its application and resistance combustion polyurethane foam and preparation method thereof.
To achieve these goals, the present invention provides a kind of fire retardant, wherein, the fire retardant contains expansible graphite and powder Coal ash, expansible graphite is (1~5) with the weight ratio of the flyash:1.
Present invention also offers a kind of application of fire retardant of the present invention in polyurethane foam.
Present invention also offers a kind of resistance combustion polyurethane foam, wherein, the gross weight with the resistance combustion polyurethane foam is as base Standard, the resistance combustion polyurethane foam contains the fire retardant of 29~43 weight %, the polyurethane of 57~71 weight %;The fire retardant contains There are expansible graphite and flyash, expansible graphite is (1~5) with the weight ratio of the flyash:1.
Present invention also offers a kind of method for preparing resistance combustion polyurethane foam, the method includes:Will be containing catalyst, many Component A of first alcohol, foam stabiliser, foaming agent and fire retardant, is reacted with component B containing isocyanates;It is described fire-retardant Agent contains expansible graphite and flyash, and expansible graphite is (1~5) with the weight ratio of the flyash:1.
By above-mentioned technical proposal, the invention provides a kind of fire retardant containing expansible graphite and flyash, can be swollen There can be synergy at fire-retardant aspect according to the mixing of specific ratio between swollen graphite and flyash, can better profit from Fire resistance of the coal ash lifting for polyurethane foamed material.
The present invention can also make flyash increase new purposes.
Other features and advantages of the present invention will be described in detail in subsequent specific embodiment part.
Specific embodiment
The specific embodiment of the present invention is described in detail below.It should be appreciated that described herein concrete Embodiment is merely to illustrate and explains the present invention, is not limited to the present invention.
Herein the end points and any value of disclosed scope is not limited to the accurate scope or value, these scopes or Value should be understood to the value comprising close these scopes or value.For numerical range, between the endpoint value of each scope, respectively Between the endpoint value of individual scope and single point value, and individually one or more can be obtained with combination with one another between point value New numerical range, these numerical rangies should be considered concrete open herein.
A kind of the first object of the present invention, there is provided fire retardant, wherein, the fire retardant contains expansible graphite and flyash, Expansible graphite is (1~5) with the weight ratio of the flyash:1.
Preferably, expansible graphite and the weight ratio of the flyash are (1~4.9):1.
According to the present invention, when preparing according to aforementioned proportion between expansible graphite and the flyash, can mutually cooperate with, More efficiently flame retardant effect is provided.When expansible graphite and the flyash configuration proportion not within the above range when, use Effective flame retardant effect can not be obtained in resistance combustion polyurethane foam.Under preferable case, on the basis of the gross weight of the fire retardant, The content of expansible graphite is 50~83 weight % in the fire retardant, and the content of the flyash is 17~50 weight %.
In the present invention, it is a kind of preferred embodiment, in the fire retardant, on the basis of the gross weight of the fire retardant, The content of expansible graphite is 50~83 weight %, and the content of the flyash is 17~50 weight %;Expansible graphite and institute The weight ratio for stating flyash is (1~5):1, preferably (1~4.9):1.
, according to the invention it is preferred in the case of, it is 90~99.9 weight % that carbon content is fixed in expansible graphite, and water content is Below 1 weight %.Expansible graphite is known substance, can be contained with commercially available Qingdao day and the product of graphite company limited, fixed carbon Measure as 99 weight %, water content is 0.5 weight %.
, according to the invention it is preferred in the case of, the flyash is the solid particle obtained after coal combustion, the flyash Mean diameter is less than 30 μm;On the basis of the gross weight of the flyash, the flyash contains more than 60 weight % SiO2And Al2O3.Meet above-mentioned condition from flyash, there can be preferably coordination to match with expansible graphite, there is provided more to have The flame retardant effect of effect.For example can be with the specifically used flyash from Guohua Electric Power company Beijing Thermal Power Plant, mean diameter is 3 μ M, consists of:The SiO of 41.25 weight %2, the Al of 35.58 weight %2O3, the CaO of 10.14 weight %, 5.94 weight % Fe2O3
A kind of the second object of the present invention, there is provided application of fire retardant of the present invention in polyurethane foam.Using this Bright fire retardant can provide polyurethane foam with good fire resistance, and realize the utilization of flyash.
The third object of the present invention, as one kind preferred embodiment, there is provided a kind of resistance combustion polyurethane foam, wherein, On the basis of the gross weight of the resistance combustion polyurethane foam, containing the fire retardant of 29~43 weight % in the resistance combustion polyurethane foam, The polyurethane of 57~71 weight %;The fire retardant contains expansible graphite and flyash, expansible graphite and the flyash Weight ratio be (1~5):1.
In the resistance combustion polyurethane foam that the present invention is provided, the fire retardant contains expansible graphite and flyash according to above-mentioned When proportion is prepared, for resistance combustion polyurethane foam effective flame retardant effect could be obtained.
Preferably, on the basis of the gross weight of the fire retardant, in the fire retardant content of expansible graphite be 50~ 83 weight %, the content of the flyash is 17~50 weight %.Expansible graphite is known substance, can with commercially available Qingdao day and The product of graphite company limited is obtained.The flyash is the solid particle that obtains after coal combustion, the average grain of the flyash Footpath is less than 30 μm;On the basis of the gross weight of the flyash, the flyash contains SiO more than 60 weight %2With Al2O3
In the present invention, it is a kind of preferred embodiment, in the resistance combustion polyurethane foam, with the gross weight of the fire retardant On the basis of, the content of expansible graphite is 50~83 weight %, and the content of the flyash is 17~50 weight %;Inflatable stone The black weight ratio with the flyash is (1~5):1, preferably (1~4.9):1.
, according to the invention it is preferred in the case of, the fire resistance of the resistance combustion polyurethane foam is UL94V0 grades.The resistance Combustion performance can be determined by UL-94 methods.
The fourth object of the present invention, there is provided a kind of method for preparing resistance combustion polyurethane foam, the method includes:Will be containing urging Component A of agent, polyhydric alcohol, foam stabiliser, foaming agent and fire retardant, is reacted with component B containing isocyanates;Institute State fire retardant and contain expansible graphite and flyash, expansible graphite is (1~5) with the weight ratio of the flyash:1.
Preferably, on the basis of the gross weight of the fire retardant, in the fire retardant content of expansible graphite be 50~ 83 weight %, the content of the flyash is 17~50 weight %.Expansible graphite is known substance, can with commercially available Qingdao day and The product of graphite company limited is obtained.The flyash is the solid particle that obtains after coal combustion, the average grain of the flyash Footpath is less than 30 μm;On the basis of the gross weight of the flyash, the flyash contains SiO more than 60 weight %2With Al2O3
In the present invention, it is a kind of preferred embodiment, in the resistance combustion polyurethane foam, with the gross weight of the fire retardant On the basis of, the content of expansible graphite is 50~83 weight %, and the content of the flyash is 17~50 weight %;Inflatable stone The black weight ratio with the flyash is (1~5):1, preferably (1~4.9):1.
In the present invention, the polyhydric alcohol can be polyhydric alcohol commonly used in the art, for example, can be PEPA And/or polyether polyol.It is highly preferred that the polyhydric alcohol is polyether polyol, such as selected from polypropylene oxide alcohol and/or epoxy third Alkane end-blocking alcohol, for example, polyoxypropyleneglycol, polypropylene oxide triol, polypropylene oxide tetrol, expoxy propane end-blocking two At least one in the tetrol of alcohol, the triol of expoxy propane end-blocking and expoxy propane end-blocking.Preferably, the polyether polyol Hydroxyl value is 280~440mgKOH/g.The polyhydric alcohol is known substance, for example can be with the limited public affairs of commercially available Jiangsu Lv Yuan new materials The product of department is obtained.
In the present invention, the isocyanates can be isocyanates commonly used in the art, for example, can be diphenyl At least one in methylene diisocyanate (MDI), toluene di-isocyanate(TDI) (TDI) and poly isocyanate.The isocyanide Acid esters is known substance, for example, can be obtained with the product of commercially available Guangzhou Li Tai insulation materials Science and Technology Ltd..
In the present invention, the foaming agent is used in the reaction obtain the foaming structure of polyurethane, can be water and/or penta Alkane.
In the present invention, the foam stabiliser can be used for the foaming foam that temperature is formed in the reaction and uniform point Cloth.Preferably organic silicon surfactant, can be polydimethylsiloxane and/or silicone oil.
According to the present invention, the reaction is mainly the isocyanates in the polyhydric alcohol in component A and component B, Reaction is carried out in the presence of the catalyst and forms polyurethane;Simultaneously foaming agent produces foaming effect, forms foaming structure;And And the foam stabiliser described in the course of reaction stablizes foam and makes foam be evenly distributed.
According to the present invention, as long as the consumption satisfaction of each component prepares flame retardant polyurethane bubble in component A and component B Foam.Under preferable case, relative to the polyhydric alcohol of 100 weight portions, the addition of fire retardant is 100~150 weight portions, isocyanide The addition of acid esters is 100~150 weight portions;The addition of the foam stabiliser is 1~9 weight portion, the foaming agent Addition is 1~9 weight portion.
According to the present invention, the catalyst includes stanniferous element compound and amino-contained compound.It is described containing tin element Compound can be tin catalyst commonly used in the art, it is preferable that the stanniferous element compound is urged selected from organic tin Agent, more preferably stannous octoate and/or dibutyl tin laurate.The amino-contained compound can be that this area routinely makes Amines catalyst, it is preferable that the amino-contained compound be triethanolamine, diethanolamine and triethylene diamine at least It is a kind of.At least one can be added using amines catalyst.
, according to the invention it is preferred in the case of, relative to the polyhydric alcohol of 100 weight portions, the stanniferous element compound plus It is 0.05~1 weight portion to enter amount, and the addition of the amino-contained compound is 1~5 weight portion.
According to the present invention, the condition of the reaction can not be particularly limited, under preferable case, the temperature of the reaction For 60~70 DEG C, the time of the reaction is 10~24h.
Hereinafter will be described the present invention by embodiment.
Burning examination is carried out to the resistance combustion polyurethane foam prepared in following examples and comparative example according to the method for UL-94 Test.
Flyash is 3 μm from Guohua Electric Power company Beijing Thermal Power Plant, mean diameter, is consisted of:41.25 weight % SiO2, the Al of 35.58 weight %2O3, the CaO of 10.14 weight %, the Fe of 5.94 weight %2O3
Expansible graphite comes from Qingdao day and graphite company limited, and fixed carbon content is 99 weight %, and water content is 0.5 Weight %.
In following examples, can by preparing resistance combustion polyurethane foam during raw material the determination that feeds intake it is obtained fire-retardant The content of each component in polyurethane foam.
Embodiment 1
This example demonstrates that the fire retardant of the present invention and the method for preparing resistance combustion polyurethane foam.
(1) fire retardant is prepared
The expansible graphite of the flyash of 50 weight portions and 50 weight portions is uniformly mixed, fire retardant S1 is obtained.
(2) resistance combustion polyurethane foam is prepared
By the polyether polyol 4110 (hydroxyl value is 430 ± 10mgKOH/g) of 100 weight portions, the fire retardant of 150 weight portions S1, the dibutyl tin laurate of 0.5 weight portion, the silicone oil of 2 weight portions, the water of 2 weight portions, the triethylene diamine of 1 weight portion Uniformly mix with the triethanolamine of 3 weight portions, obtain blending ingredients A1.
The blending ingredients A1 is mixed with the MDI (MDI) of 100 weight portions, and 70 DEG C, react 24 hours under normal pressure, obtain resistance combustion polyurethane foam PU1, wherein, the content of fire retardant S1 is 43 weight %.
Embodiment 2
This example demonstrates that the fire retardant of the present invention and the method for preparing polyurethane foam.
(1) fire retardant is prepared
The expansible graphite of the flyash of 17 weight portions and 83 weight portions is uniformly mixed, fire retardant S2 is obtained.
(2) resistance combustion polyurethane foam is prepared
By the polyether polyol 4110 (hydroxyl value is 430 ± 10mgKOH/g) of 100 weight portions, the fire retardant of 120 weight portions S2, the dibutyl tin laurate of 0.05 weight portion, the silicone oil of 9 weight portions, the water of 1 weight portion, the triethylene diamine of 2 weight portions Uniformly mix with the triethanolamine of 3 weight portions, obtain blending ingredients A2.
The blending ingredients A2 is mixed with the MDI (MDI) of 150 weight portions, and 60 DEG C, react 24 hours under normal pressure, obtain resistance combustion polyurethane foam PU2, wherein, the content of fire retardant S2 is 29 weight %.
Embodiment 3
This example demonstrates that the fire retardant of the present invention and the method for preparing polyurethane foam.
(1) fire retardant is prepared
The expansible graphite of the flyash of 40 weight portions and 60 weight portions is uniformly mixed, fire retardant S3 is obtained.
(2) resistance combustion polyurethane foam is prepared
By the polyether polyol 4110 (hydroxyl value is 430 ± 10mgKOH/g) of 100 weight portions, the fire retardant of 150 weight portions S3, the dibutyl tin laurate of 1 weight portion, the silicone oil of 1 weight portion, the pentane of 9 weight portions, the triethylene diamine of 1 weight portion Uniformly mix with the triethanolamine of 1 weight portion, obtain blending ingredients A3.
The blending ingredients A3 is mixed with the MDI (MDI) of 120 weight portions, and 70 DEG C, react 24 hours under normal pressure, obtain resistance combustion polyurethane foam PU3, wherein, the content of fire retardant S3 is 31 weight %.
Comparative example 1
According to the method for embodiment 1, except for the difference that, expansible graphite is replaced with DMMP (dimethyl methyl phosphonate), so as to Prepared polyurethane foam DPU1.
Comparative example 2
According to the method for embodiment 1, except for the difference that, fly ash content is 0 in fire retardant, and expansible graphite content is 100%, so as to polyurethane foam DPU2 is obtained.
Comparative example 3
According to the method for embodiment 1, except for the difference that, fly ash content is 100% in fire retardant, and expansible graphite content is 0, so as to polyurethane foam DPU3 is obtained.
Comparative example 4
According to the method for embodiment 1, except for the difference that, fly ash content is 10% in fire retardant, and expansible graphite content is 90%, so as to polyurethane foam DPU4 is obtained.
Comparative example 5
According to the method for embodiment 1, except for the difference that, fly ash content is 90% in fire retardant, and expansible graphite content is 10%, so as to polyurethane foam DPU5 is obtained.
Test case
Resistance combustion polyurethane foam PU1, PU2, PU3 and DPU1, DPU2, DUP3, DPU4, DPU5 are entered according to UL-94 standards Row fire resistance is tested, and specifically, it is 13.0 ± 0.5mm, length that polyurethane foamed material is formed into thickness for 1.6mm, width For the test sample of 125 ± 5mm, the length of flame of burner is 20mm, implements the sample test of 2 × 10s, and according to table 1 The UL-94 test classes of shown each sample of standard determination.
Polyurethane foamed material test result prepared by embodiment and comparative example is as shown in table 2.
Table 1UL-94 testing standards
Grade Flame height The maximum combustion time Maximum total burning time Cotton is burnt
V-0 3/4” 10s 50s(F) Nothing
V-1 3/4” 30s 250s(F) Nothing
V-2 3/4” 30s 250s(F) Allow
NR does not have grade 3/4” >30s >250 Allow
Table 2UL94 test results
In above-mentioned table 2, by by embodiment 1-3 and comparative example 1-5 be compared as can be seen that flyash with it is inflatable Graphite coordinates the fire retardant as polyurethane foam to have synergy, and compositionss can show excellent resistance using flyash Fuel efficiency fruit, reaches the V0 levels in UL-94 grades.
Expansible graphite or flyash, expansible graphite and fine coal used in comparative example 4,5 are used alone in comparative example 2,3 Ash combination can not form the synergism of expansible graphite and flyash, it is impossible to obtain right not within the restriction of the present invention The effective flame retardant effect of polyurethane foam.

Claims (10)

1. a kind of fire retardant, it is characterised in that the fire retardant contains expansible graphite and flyash, expansible graphite and the powder The weight ratio of coal ash is (1~5):1.
2. fire retardant according to claim 1, wherein, on the basis of the gross weight of the fire retardant, in the fire retardant The content of expansible graphite is 50~83 weight %, and the content of the flyash is 17~50 weight %.
3. fire retardant according to claim 1 and 2, wherein, carbon content is fixed in expansible graphite for 90~99.9 weights Amount %, water content is below 1 weight %;The flyash is the solid particle that obtains after coal combustion, the flyash it is average Particle diameter is less than 30 μm;On the basis of the gross weight of the flyash, the flyash contains SiO more than 60 weight %2With Al2O3
4. application of the fire retardant in a kind of claim 1-3 described in any one in polyurethane foam.
5. a kind of resistance combustion polyurethane foam, it is characterised in that on the basis of the gross weight of the resistance combustion polyurethane foam, this is fire-retardant poly- Urethane foam contains the fire retardant of 29~43 weight %, the polyurethane of 57~71 weight %;The fire retardant contains inflatable stone Ink and flyash, expansible graphite is (1~5) with the weight ratio of the flyash:1.
6. resistance combustion polyurethane foam according to claim 5, wherein, the fire resistance of the resistance combustion polyurethane foam is UL94V0 grades.
7. a kind of method for preparing resistance combustion polyurethane foam, the method includes:Will containing catalyst, polyhydric alcohol, foam stabiliser, Component A of foaming agent and fire retardant, is reacted with component B containing isocyanates;The fire retardant contains expansible graphite And flyash, expansible graphite is (1~5) with the weight ratio of the flyash:1.
8. method according to claim 7, wherein, relative to the polyhydric alcohol of 100 weight portions, the addition of the fire retardant For 100~150 weight portions, the addition of isocyanates is 100~150 weight portions, the addition of the foam stabiliser is 1~ 9 weight portions, the addition of the foaming agent is 1~9 weight portion.
9. method according to claim 7, wherein, the catalyst includes stanniferous element compound and amino-contained chemical combination Thing;Relative to the polyhydric alcohol of 100 weight portions, the addition of the stanniferous element compound is 0.05~1 weight portion, described containing amine The addition of based compound is 1~5 weight portion.
10. the method according to any one in claim 7-9, wherein, the temperature of the reaction is 60~70 DEG C, described The time of reaction is 10~24h.
CN201611128268.9A 2016-12-09 2016-12-09 A kind of fire retardant and its application and resistance combustion polyurethane foam and preparation method thereof Active CN106589458B (en)

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CN107788740A (en) * 2017-10-27 2018-03-13 公安部四川消防研究所 Flame-retardant sofa
CN112585185A (en) * 2018-08-23 2021-03-30 美国圣戈班性能塑料公司 Polyurethane foam and method of forming same
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