CN102911334A - B1-grade high-fire-retardant low-smoke-generation rigid polyurethane foam - Google Patents
B1-grade high-fire-retardant low-smoke-generation rigid polyurethane foam Download PDFInfo
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- CN102911334A CN102911334A CN201210456255XA CN201210456255A CN102911334A CN 102911334 A CN102911334 A CN 102911334A CN 201210456255X A CN201210456255X A CN 201210456255XA CN 201210456255 A CN201210456255 A CN 201210456255A CN 102911334 A CN102911334 A CN 102911334A
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Abstract
Disclosed is B1-grade high-fire-retardant low-smoke-generation rigid polyurethane foam which is good in fire retardant effect and low in combustion smoke generation. The foam is prepared by subjecting premixed polyether polyol and polymeric diphenylmethane diisocyanate (MDI) to mixing and foaming according to the weight part ratio of 1: (1-1.5), and the premixed polyether polyol is composed of the following raw materials of, by weight, 30-50 parts of phenolic resin polyol, 20-50 parts of polyether polyol A, 0-50 parts of polyether polyol B, 0-30 parts of polyester polyol C, 1.5-3.0 parts of an organosilicone foam stabilizer, 3.0-6.0 of a composite catalyst, 0-10 parts of a liquid fire retardant, 0.5-1.5 parts of water, 10-25 parts of a physical foaming agent and 7-25 pars of graphite slurries.
Description
Technical field
The present invention relates to a kind of hard polyurethane foams, relate in particular to the low hard polyurethane foams of being fuming of a kind of B1 level high flame retardant.
Background technology
Rigid urethane foam has that insulation effect is good, lightweight, chemicals-resistant is good, soundproof effect reaches well the characteristics such as easy construction, and it has been widely used in industry and the civilian departments such as aerospace, boats and ships, oil, transportation, food, building.Because polyurethane foam contains that flammable hydrocarbon segment, density are little, specific surface area is large, belong to inflammable substance without the polyurethane foam of fire-retardant finish, meet fire and namely fire, and produce a large amount of toxic smogs.
The fire-retardant of present polyurethane material mainly is divided into two kinds, and a kind of is by adding fire retardant material; Another kind is the reaction-type flame-retarding material that contains flame retarding construction in the molecular structure.Add fire retardant such as phosphoric acid ester, halogenated phosphate, clorafin, aluminium hydroxide etc., along with although the increase of addition can improve flame retardant effect, but the physical and mechanical properties of material declines to a great extent, and along with the prolongation of the time of interpolation, thereby migration can occur so that Flame Retardancy can descend in the liquid flame retardant in the material.
Reaction-type flame-retarding is that the structures such as ignition-proof element phosphorus, halogen, nitrogen or phenyl ring are imported in the polyol structure at the same time or separately by chemical reaction, and makes polyurethane foamed material have flame retardant properties.Reactive flame retardant participates in reaction as a kind of reacted constituent, and little on the material property impact, flame retarding construction stably is attached in the polyurethane macromolecular matrix, is that urethane itself contains flame-retardant composition, can not separate out in the life-time service process and reduces flame retardant effect.As: three (dipropylene glycol) phosphorous acid ester (being commonly called as P430), three (polyoxygenated alkene) phosphoric acid ester, three (polyoxygenated alkene) phosphorous acid ester, bromination tetramethylolmethane or PHT4 fire-retardant polyvalent alcohol, melamine derivative polyvalent alcohol etc.Chinese patent CN200910024674.4 and CN200910024675.9 disclose a kind of structure-type flame-proof polyol for preparing with Viscotrol C after bromination and alcoholysis.Halogen-containing polyurethane foam, halogen can be emitted the corrodibility toxic gases such as hydrogen halide when burning, and the burning smoke density is large, not only dirt settling and environment is damaged the escape when more being unfavorable for fire and rescue.Chinese patent CN201110425843.2 discloses a kind of phenolic aldehyde polyol resin for the production of resistance combustion polyurethane foam, this patent is take phenol and formaldehyde or Paraformaldehyde 96 as raw material synthesized micromolecule amount resol, cooperate again glycerol and olefin oxide ring-opening polymerization to obtain containing in the molecule polyvalent alcohol of resol structure, prepare hard polyurethane foams with this polyvalent alcohol and have good flame retardant effect.
Expansible black lead (EG) is a kind of compound between graphite layers that is obtained after chemical oxidization method or electrochemical oxidation process processing by natural flake graphite, and with regard to structure, EG is a kind of nanocomposite.Common H
2SO
4Redox reaction occurs between sulfuric acid and the graphite carbon atom in the EG that oxidation makes when being subject to more than 200 ℃ high temperature, produce a large amount of SO
2, CO
2And water vapor, make EG begin to expand, and in the time of 1100 ℃, reach maximum volume, when its final volume can reach initial 280 times.This characteristic is so that EG can pass through the moment increase of volume with fray-out of flame when fire occurs.The fire retardant mechanism of EG belongs to the coagulation phase fire retardant mechanism, and is fire-retardant by delaying or interrupt by solid matter generation inflammable substance.EG is heated to a certain degree, will begin to expand, and the graphite after the expansion becomes the very low vermiform of density by original flakey, thereby forms good thermal insulation layer.Graphite flake after the expansion is the charcoal source in the intumescent system, is again thermal insulation layer, can be effectively heat insulation, the decomposition that delays and stop polymkeric substance; Simultaneously, in a large number heat absorption has reduced system temperature in the expansion process; And in the expansion process, the acid ion in the release jacket coating promotes dehydration carbonization.EG is as a kind of halogen-free environment-friendly flame-proof agent, and its advantage is: nontoxic, do not generate poisonous and corrosive gases when being heated, and the flue gas of generation is seldom, addition is little, and without drippage, environmental compatibility is strong, non-migratory phenomenon, UV stable and good light stability, the source is sufficient, and manufacturing process is simple.Therefore, EG has been widely used in the various fire-retardant fireproof materials.Such as " polyurethane industrial " 2011,26 (2) " DMMP and the EG fire-retardant synergistic researchs in RPUF ", " polymer material science and engineering " 2009,25 (6) " preparations of the fire-retardant steeping in water for reconstitution slabstock polyurethane foam of expansible black lead ", " Chinese Plastics " 2006,20 (4) " research of different-grain diameter expansible black lead halogen-free flameproof high-density hard polyurethane porous plastics " have all been set forth EG as the good flame retardant effect of halogen-free flame retardants to hard polyurethane foams.But expansible black lead is as a kind of fire retardant of solid, and the addition in the polyvalent alcohol prescription is certain, and along with the increase of EG addition can greatly increase the viscosity of polyol component and cause the mobile variation of foamable reaction.
Therefore, adopting the composite flame-proof technology, obtain all good flame retarded rigid polyurethane foams of flame retardant effect, foam process and foaming properties, is the key of promoting the use of flame retarded rigid polyurethane foams.
Summary of the invention
The purpose of this invention is to provide the low hard polyurethane foams of being fuming of the low B1 level high flame retardant of a kind of good flame retardation effect, burning fuming amount.
For achieving the above object, the technical solution used in the present invention is: the low hard polyurethane foams of being fuming of a kind of B1 level high flame retardant, made by combined polyether glycol and polymeric MDI mixed foaming, combined polyether and polymeric MDI be 1:1 ~ 1.5 according to ratio of weight and number, described combined polyether is comprised of the raw material of following weight part ratio:
Resol polyvalent alcohol: 30 ~ 50;
Polyether glycol A: 20 ~ 50;
Polyether glycol B: 0 ~ 50;
Polyester polyol C: 0 ~ 30;
Silicon foams stablizer: 1.5 ~ 3.0;
Composite catalyst: 3.0 ~ 6.0;
Liquid flame retardant: 0 ~ 10;
Water: 0.5 ~ 1.5;
Pneumatogen: 10 ~ 25;
Black lead wash: 7 ~ 25;
Described resol polyvalent alcohol is to be made by sea, Shandong hat Chemical Industry Science Co., Ltd, and the polyvalent alcohol hydroxyl value is 380 ± 20mgKOH/g, and viscosity is 4000 ~ 6000 (mPa.s/25 ℃).
Described polyether glycol A is polyether polyvalent alcohol take sucrose as compound initiator, typical polyethers be sucrose and glycerol as 835 polyethers of compound initiator, or sucrose and propylene glycol or ethylene glycol or Diethylene Glycol are 4110 polyethers of compound initiator.
Described polyether glycol B is the polyether polyvalent alcohol take sorbyl alcohol or N.F,USP MANNITOL as compound initiator, and typical polyethers is that sorbyl alcohol and glycerol are 635 polyethers of compound initiator.
Described polyester polyol C is the polyester polyol of O-phthalic phthalic anhydride or terephthalic acid and polyol condensating reaction acquisition, is typically the PS-3152 of Nanjing, Nanjing Si Taipan chemistry company limited.
Described silicon foams stablizer is the foam tensio-active agent that is obtained by the allyl polyether graft polysiloxane, typical products is beautiful AK-8803, the AK-8805 that thinks Dehua limited-liability company in Nanjing, or the B 8462 of German high Schmidt company, or the L-6900 of U.S. Mai Tu company, L-5440 etc.
Described composite catalyst comprises tertiary amine catalyst and metallic salt catalyzer.Wherein tertiary amine is triethylenediamine, triethylamine, dimethylcyclohexylamine, two (2-dimethylaminoethyl) ether, five methyl diethylentriamine, dimethylethanolamine, trolamine, dimethyl benzylamine or diethyl piperazine; Metallic salt is potassium acetate, isocaprylic acid potassium, isocaprylic acid zinc, potassium oleate.
Described liquid flame retardant is phosphoric acid ester or halogenated phosphate, is in three (dipropylene glycol) phosphorous acid ester, three (polyoxygenated alkene) phosphoric acid ester, three (polyoxygenated alkene) phosphorous acid ester, methyl-phosphoric acid dimethyl ester (DMMP), ethyl phosphonic acid diethyl ester (DEEP), phosphoric acid (2-chloroethyl) three esters (TCEP), phosphoric acid (2-chloropropyl) three esters (TCPP), phosphoric acid (two chloropropyls) three esters (TDCP) one or more.
Described pneumatogen is one or more in HCFC-141b, pentamethylene, Skellysolve A, the iso-pentane.
Described black lead wash is to adopt organo-silicon coupling agent through suitably art breading acquisition by expansible black lead (EG).The treatment process that adopts is for take general rigid-foam polyether polyol as dispersion liquid, and expansible black lead (EG) physical compounding is become the black lead wash of 50wt%, adds an amount of organo-silicon coupling agent, grinds 30 ~ 60min through three-roll grinder and gets final product.The organo-silicon coupling agent of selecting is a kind of in γ-aminopropyl triethoxysilane, γ-glycidyl ether oxygen base propyl trimethoxy silicane, γ-methacryloxypropyl trimethoxy silane, N-β-(aminoethyl)-γ aminopropyl methyl dimethoxysilane or N-β-(the aminoethyl)-γ aminopropyl trimethoxysilane.The organo-silicon coupling agent consumption is 0.3 ~ 1.5wt% of EG.
Advantageous effect of the present invention is: owing to adopt the composite flame-proof technology, so the urethane foam flame retardant properties that makes reaches the B1 grade standard; Used resol polyvalent alcohol and expanded graphite all have good flame retardation effect, advantage that the burning fuming amount is low, and flame retardant effect is lasting.
Embodiment
The invention will be further described below in conjunction with specific embodiment:
Embodiment 1
Black lead wash is formed composite grinding 40min and is obtained by following:
Polyether glycol 4110: 100g;
Expanded graphite: 100g;
γ-aminopropyl triethoxysilane: 0.5g;
B1 level high flame retardant is low, and the hard polyurethane foams combined polyether of being fuming is comprised of the raw material of following weight part ratio:
Resol polyvalent alcohol: 40;
Polyether glycol 835: 45;
Polyester polyol PS-3152: 15;
Organic silicon surfactant B 8462: 2.0;
Five methyl diethylentriamine: 1.5;
Dimethylcyclohexylamine: 1.2;
Potassium oleate: 0.6;
Phosphoric acid (2-chloropropyl) three esters (TCPP): 7.0;
Water: 1.2;
Pentamethylene: 12.0;
Black lead wash: 16.0;
After according to aforementioned proportion each component being mixed, it is mixed according to mass ratio 1:1.2 with polymeric MDI, make the low hard polyurethane foams of being fuming of B1 level high flame retardant after the reaction foaming.
Embodiment 2
Black lead wash is formed composite grinding 50min and is obtained by following:
Polyether glycol 635: 100g;
Expanded graphite: 100g;
γ-glycidyl ether oxygen base propyl trimethoxy silicane: 0.5g;
B1 level high flame retardant is low, and the hard polyurethane foams combined polyether of being fuming is comprised of the raw material of following weight part ratio:
Resol polyvalent alcohol: 45;
Polyether glycol 4110:45;
Polyether glycol 635:10;
Organic silicon surfactant AK-8805: 2.0;
Two (2-dimethylaminoethyl) ether: 0.5;
Dimethylcyclohexylamine: 3.2;
Different potassium zincate: 1.6;
Phosphoric acid (2-chloropropyl) three esters (TCPP): 7.0;
Ethyl phosphonic acid diethyl ester (DEEP): 3.0;
Water: 1.2;
Skellysolve A/iso-pentane (35/65): 12.0;
Black lead wash: 18.0;
After according to aforementioned proportion each component being mixed, it is mixed according to mass ratio 1:1.1 with polymeric MDI, make the low hard polyurethane foams of being fuming of B1 level high flame retardant after the reaction foaming.
Embodiment 3
Black lead wash is formed composite grinding 60min and is obtained by following:
Polyether glycol 835:100g;
Expanded graphite: 100g;
N-β-(aminoethyl)-γ aminopropyl trimethoxysilane: 1.0g;
B1 level high flame retardant is low, and the hard polyurethane foams combined polyether of being fuming is comprised of the raw material of following weight part ratio:
Resol polyvalent alcohol: 50;
Polyether glycol 835: 20;
Polyester polyol PS-3152: 30;
Organic silicon surfactant L-6900: 2.0;
Dimethylcyclohexylamine: 3.2;
Isocaprylic acid potassium: 1.6;
Water: 1.2;
HCFC-141b?：20.0；
Black lead wash: 25.0;
After according to aforementioned proportion each component being mixed, it is mixed according to mass ratio 1:1.5 with polymeric MDI, make the low hard polyurethane foams of being fuming of B1 level high flame retardant after the reaction foaming.
Embodiment 4
Black lead wash is formed composite grinding 30min and is obtained by following:
Polyether glycol 303: 100g;
Expanded graphite: 100g;
γ-aminopropyl triethoxysilane: 1.0g;
B1 level high flame retardant is low, and the hard polyurethane foams combined polyether of being fuming is comprised of the raw material of following weight part ratio:
Resol polyvalent alcohol: 45;
Polyether glycol 4110: 20;
Polyether glycol 635: 20;
Polyester polyol PS-3152: 15;
Organic silicon surfactant AK-8803:2.0;
Dimethylcyclohexylamine: 3.5;
Potassium acetate: 1.6;
Three (dipropylene glycol) phosphorous acid ester: 10.0;
Water: 1.3;
Pentamethylene: 13.0;
Black lead wash: 22.0;
After according to aforementioned proportion each component being mixed, it is mixed according to mass ratio 1:1.2 with polymeric MDI, make the low hard polyurethane foams of being fuming of B1 level high flame retardant after the reaction foaming.
After testing, embodiment 1～4 gained hard polyurethane foams salient features sees the following form:
| Performance | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 |
| Density/kgm 3 | 42.3 | 41.8 | 42.1 | 41.7 |
| Compressive strength/kPa | 178 | 165 | 182 | 175 |
| Thermal conductivity/mW (mK) -1 | 20.6 | 20.5 | 20.2 | 21.3 |
| Oxygen index/% | 32.1 | 32.2 | 32.9 | 32.2 |
| Smoke density | 44 | 43 | 36 | 41 |
| Flame retardant rating | B1 | B1 | B1 | B1 |
The present invention is intended to adopt the composite flame-proof technology, resol polyvalent alcohol in the Chinese patent CN201110425843.2 is as the reaction-type flame-retarding polyvalent alcohol, take surface treated expansible black lead (EG) as halogen-free flame retardants, be aided with a small amount of phosphoric acid ester or halogenated phosphate liquid flame retardant, the low hard polyurethane foams of being fuming of preparation B1 level high flame retardant.
Claims (5)
1. a B1 level high flame retardant is hanged down the hard polyurethane foams of being fuming, made by combined polyether glycol and polymeric MDI mixed foaming, the mass ratio of combined polyether and polymeric MDI is 1:1 ~ 1.5, and described combined polyether is comprised of the raw material of following weight part proportioning: resol polyvalent alcohol: 30 ~ 50; Polyether glycol A: 20 ~ 50; Polyether glycol B: 0 ~ 50; Polyester polyol C: 0 ~ 30; Silicon foams stablizer 1.5 ~ 3.0; Composite catalyst: 3.0 ~ 6.0; Liquid flame retardant: 0 ~ 10; Water: 0.5 ~ 1.5; Pneumatogen: 10 ~ 25; Black lead wash: 7 ~ 25.
2. B1 level high flame retardant according to claim 1 is hanged down the hard polyurethane foams of being fuming, and described combined polyether is comprised of the raw material of following weight part proportioning: resol polyvalent alcohol 40; Polyether glycol 835:45; Polyester polyol PS-3152:15;
Organic silicon surfactant B8462:2.0; Five methyl diethylentriamine: 1.5; Dimethylcyclohexylamine: 1.2; Potassium oleate: 0.6; Phosphoric acid (2-chloropropyl) three esters (TCPP): 7.0; Water: 1.2; Pentamethylene: 12.0; Black lead wash: 16.0; Wherein black lead wash is formed composite grinding 40min and is obtained by following: polyether glycol 4110:100g; Expanded graphite: 100g; γ-aminopropyl triethoxysilane: 0.5g; After according to aforementioned proportion each component being mixed, it is mixed according to mass ratio 1:1.2 with polymeric MDI, make the low hard polyurethane foams of being fuming of B1 level high flame retardant after the reaction foaming.
3. B1 level high flame retardant according to claim 2 is hanged down the hard polyurethane foams of being fuming, and described combined polyether is comprised of the raw material of following weight part proportioning: resol polyvalent alcohol: 45; Polyether glycol 4110: 45; Polyether glycol 635:10; Organic silicon surfactant AK-8805:2.0; Two (2-dimethylaminoethyl) ether: 0.5; Dimethylcyclohexylamine: 3.2; Different potassium zincate: 1.6; Phosphoric acid (2-chloropropyl) three esters (TCPP): 7.0; Ethyl phosphonic acid diethyl ester (DEEP): 3.0; Water: 1.2; Skellysolve A/iso-pentane (35/65): 12.0; Black lead wash: 18.0; Wherein black lead wash is formed composite grinding 50min and is obtained by following: polyether glycol 635: 100g; Expanded graphite: 100g; γ-glycidyl ether oxygen base propyl trimethoxy silicane: 0.5g; After according to aforementioned proportion each component being mixed, it is mixed according to mass ratio 1:1.1 with polymeric MDI, make the low hard polyurethane foams of being fuming of B1 level high flame retardant after the reaction foaming.
4. B1 level high flame retardant according to claim 3 is hanged down the hard polyurethane foams of being fuming, and described combined polyether is comprised of the raw material of following weight part proportioning: resol polyvalent alcohol: 50; Polyether glycol 835:20; Polyester polyol PS-3152: 30; Organic silicon surfactant L-6900:2.0; Dimethylcyclohexylamine: 3.2; Isocaprylic acid potassium: 1.6; Water: 1.2; HCFC-141b: 20.0; Black lead wash: 25.0; Wherein black lead wash is formed composite grinding 60min and is obtained by following: polyether glycol 835: 100g; Expanded graphite: 100g; N-β-(aminoethyl)-γ aminopropyl trimethoxysilane: 1.0g; After according to aforementioned proportion each component being mixed, it is mixed according to mass ratio 1:1.5 with polymeric MDI, make the low hard polyurethane foams of being fuming of B1 level high flame retardant after the reaction foaming.
5. B1 level high flame retardant according to claim 4 is hanged down the hard polyurethane foams of being fuming, and described combined polyether is comprised of the raw material of following weight part proportioning: resol polyvalent alcohol: 45; Polyether glycol 4110:20; Polyether glycol 635: 20; Polyester polyol PS-3152: 15; Organic silicon surfactant AK-8803: 2.0; Dimethylcyclohexylamine: 3.5; Potassium acetate: 1.6; Three (dipropylene glycol) phosphorous acid ester: 10.0; Water: 1.3; Pentamethylene: 13.0; Black lead wash: 22.0; Wherein black lead wash is formed composite grinding 30min and is obtained by following: polyether glycol 303: 100g; Expanded graphite: 100g; γ-aminopropyl triethoxysilane: 1.0g; After according to aforementioned proportion each component being mixed, it is mixed according to mass ratio 1:1.2 with polymeric MDI, make the low hard polyurethane foams of being fuming of B1 level high flame retardant after the reaction foaming.
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Application publication date: 20130206 |