CN101781395B - Hard polyurethane adiabatic heat-insulation foam material and preparation method thereof - Google Patents
Hard polyurethane adiabatic heat-insulation foam material and preparation method thereof Download PDFInfo
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- CN101781395B CN101781395B CN2010101347270A CN201010134727A CN101781395B CN 101781395 B CN101781395 B CN 101781395B CN 2010101347270 A CN2010101347270 A CN 2010101347270A CN 201010134727 A CN201010134727 A CN 201010134727A CN 101781395 B CN101781395 B CN 101781395B
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Abstract
The invention relates to a hard polyurethane adiabatic heat-insulation foam material and a preparation method thereof. The material contains the following components: polyether glycol, polymethylene polyphenyl isocyanate, chopped glass fiber powder, physical foaming agent, water, fire retardant, catalyst and foam stabilizer. The preparation method comprises that the surface of the chopped glass fiber powder is treated through silane coupling agent; and the polyether glycol, polymethylene polyphenyl isocyanate and the surface-treated chopped glass fiber powder are dried, mixing treatment and polymerization foaming treatment are sequentially conducted thereafter, curing treatment is conducted after a pouring mould blank is obtained and the mould is removed, and finally hard polyurethane foam is obtained. Since the invention adopts the third-generation zero-ozone-consumption latent-energy hydrofluorocarbon foaming agent and the halogen-free high-efficiency fire retardant, the foam material has the advantages of environmental protection, low density and excellent compression property and is suitable for use in the heat insulation field.
Description
Technical field
What the present invention relates to is foam material of a kind of polyurethane material technical field and preparation method thereof, particularly a kind of hard polyurethane adiabatic heat-insulation foam material and preparation method thereof.
Background technology
Rigid polyurethane foam relies on its lower thermal conductivity, has become irreplaceable now heat-insulation material, is widely used in fields such as building, space flight and aviation, communications and transportation.Along with banning use of of fluorochlorohydrocarbon (CFCs) whipping agent, the restriction of hydrogen fluorochlorohydrocarbon (HCFCs) whipping agent is used, and the whipping agent of zero odp (Ozone Depression Potential ozone depletion potential) has become the research focus, as water, supercritical CO
2, pentane class, hydrogen fluorohydrocarbon (HFCs) etc.But wherein the shortcoming of pentane foaming agent is inflammable, can produce blast under certain condition with AIR MIXTURES, so must increase some safety features, equipment cost is than higher.In addition, pentane gas phase thermal conductivity has certain swelling action than the HCFC-141b height to polyurethane foam, and in order to reach required intensity and insulativity, foamy density is higher by about 10% than CFC-11 system usually, and poorly soluble in polyethers.Water and supercritical CO
2The polyurethane foam of producing, when low density, foam is crisp, and intensity, dimensional stability, heat-insulating property are relatively poor, and consume more isocyanic ester.And CO
2Gas molecule is little, easily slowly overflows from abscess, causes heat-insulating property to descend.HCFC-141b is high slightly for HFCs class whipping agent gas phase thermal conductivity ratio, and is lower than pentane, and compare with pentane and have better security, hypotoxicity, the zero odp value is more and more paid attention to by people.Wherein, HFC-365mfc has minimum gas phase thermal conductivity, has only 10.6mW/mK in the time of 25 ℃, and it has 40.2 ℃ of higher boiling point, and normal temperature is down for liquid.The HFC-365mfc gasification temperature is higher, usually unites foaming with water, and water is emitted CO with-NCO reaction
2The time, can produce a large amount of heat, help the HFC-365mfc gasification.
In disclosed patent and the document, use the hard polyurethane foams lagging material of HFCs whipping agent, when guaranteeing have than low thermal conductivity, usually all has relatively poor compressive strength, as to authorize publication number be the Chinese patent of CN 100509899C and CN 100509003C, uses HFC-365mfc and HFC-227ea binary blend as whipping agent, do not use reinforcing filler, the foam materials of preparation is when its density is 40Kg/m
3The time, its thermal conductivity is 0.025W/mK, compressive strength has only 0.28MPa.Density reaches 50Kg/m
3The time, its thermal conductivity is 0.027W/mK, compressive strength also has only 0.35MPa.Density reaches 60Kg/m
3The time, its thermal conductivity is 0.025W/mK, compressive strength also has only 0.42MPa.Authorizing publication number is the Chinese patent of CN 1237088C, and HFC-365mfc and HFC-245fa are as main foaming agent, and water does not use reinforcing filler as auxilliary whipping agent, and the foam materials of preparation is when its density is 43Kg/m
3The time, its thermal conductivity is 0.0211W/mK, compressive strength has only 0.29MPa.Density reaches 47Kg/m
3The time, its thermal conductivity is 0.0217W/mK, compressive strength also has only 0.29MPa.When compressive strength reached 0.83MPa, its density need increase to 95Kg/m
3Application publication number is that the Chinese patent of CN 100999566A uses HFC-245fa or HFC-365mfc and HFC-227ea as main foaming agent, and water does not use reinforcing filler as auxilliary whipping agent, and density is 41.5Kg/m
3, 0.0186W/mK, compressive strength has only 0.18MPa.
In disclosed patent and the document, relevant for the report that adds reinforcing filler, but the foam materials that adds filler all has big density, the thermal conductivity of non-constant, some material even have no idea as lagging material.Application publication number is that the Chinese patent of CN 1404503A uses a large amount of hollow microsphere to strengthen polyurethane foam, and the density of this material is 160-480Kg/m
3, this foam can't be as lagging material, and is applicable to " as the reinforcement porous plastics " in " automobile industry ".Application publication number is that the Chinese patent of CN101235128A uses the continuous fibre enhancement polyurethane foam, and the density of this material is 400-800Kg/m
3, compressive strength is 17-62MPa, this foam is suitable for as " bearing structure material ", but not heat-insulation material.Application publication number is that the Chinese patent of CN 101191010A uses the continuous fibre enhancement polyurethane foam, and the density of this material is 690-768Kg/m
3, compressive strength is 48.8-65.1MPa, this foam is suitable for as " technical fields such as warship cabin door, dividing plate, railroad tie, lorry compartment and civil construction material ", but not heat-insulation material.Application publication number is that the Chinese patent of CN 1834130A uses the continuous fibre enhancement polyurethane foam, and the density of this material is 115-135Kg/m
3, compressive strength is 1.4-1.7MPa, but does not provide the thermal conductivity of material in the patent.
People (Kim, Youn Hee such as Youn Hee Kim; Lee, Jae Won; Choi, Seok Jin; Han, Mi Sun; Kim, Ji Mun; Kim, Sang Bum; Kim, Woo Nyon.Properties of rigid polyurethane foams blownby HFC-365mfc and distilled water.Journal of Industrial and Engineering Chemistry (Seoul, Republic of Korea) (2007), 13 (7), 1076-1082.) system that HFC-365mfc and water are made the associating whipping agent done comparatively systematic research, do not use reinforcing filler, just by changing the consumption and the proportioning of whipping agent, they can prepare the rigid polyurethane foam in the different densities scope, when density is 40-80Kg/m
3The time, the material compressive strength has only 0.45-0.55MPa, and thermal conductivity is but up to 0.0244-0.0292W/mK.
Some discuss glass fibre (Li Guozhong both at home and abroad, Yu Yanzhen, glass fibre is to the discussion of rigid urethane foam enhanced mechanism, polymer material science and engineering, 1997,14 (4): 130-133), glass microsphere (Jiang Xin etc., the performance of glass microballon Reinforced Rigid Polyurethane Foam, 2008,24 (11): 62-65), SiO
2(Liu Xinjian, glass/micron SiO
2The preparation of Reinforced Rigid Polyurethane Foam and performance, University On The Mountain Of Swallows's Master's thesis, 2005) etc. strengthen the article of polyurethane foamed material, the more water that makes is as whipping agent, and the emphasis of being studied is to use these materials to increase the mechanical property of polyurethane foamed material, strengthen the thermal conductivity of back material and ignored it, the material after often strengthening like this can't be used as heat-insulation material.And do not report chopped glass fiber powder as reinforcing filler, cooperate HFCs class third generation whipping agent, prepare excellent heat insulating performance, the hard polyurethane foams heat-insulation material of mechanical property excellence.
In sum, there is not a kind of density now between 40～80Kg/m
3, the whipping agent environmental protection of use, the heat-insulating property excellence, the hard polyurethane foams lagging material that has excellent compression performance simultaneously is in the news.
Summary of the invention
The present invention is directed to the prior art above shortcomings, a kind of hard polyurethane adiabatic heat-insulation foam material and preparation method thereof is provided, has heat-insulating property preferably, higher compression performance and modulus of compression, good flame resistance, and the whipping agent environmental protection of using does not have destruction to ozonosphere, is applicable to as heat preserving and insulating material.
The present invention is achieved by the following technical solutions:
The present invention relates to polyurethane adiabatic heat-insulation foam material, its component and content are: polyether glycol 100 weight parts, polymethylene multi-phenenyl isocyanate 150～170 weight parts, chopped glass fiber powder 5～30 weight parts, pneumatogen 10～30 weight parts, water 1 weight part, fire retardant 10～15 weight parts, catalyzer 1～4 weight part, suds-stabilizing agent 1.5～10 weight parts.
Described polyether glycol is to be initiator with sucrose, and hydroxyl value is 450-500mgKOH/g, viscosity 6000～9000mPas in the time of 25 ℃;
The content of isocyano is 30～32%wt in the described polymethylene multi-phenenyl isocyanate, viscosity 350～700mPas in the time of 25 ℃, and functionality is 2.6～3.1.
Described chopped glass fiber powder is diameter 10-20 μ m, the chopped glass fiber powder of long 100-500 μ m;
Described pneumatogen is 1,1,1,3,3-3-pentafluorobutane (HFC-365mfc);
Described fire retardant is not halogen-containing efficient flame-retarding agent, comprising: the mixture of one or both arbitrary proportions in methyl-phosphoric acid dimethyl ester (DMMP) and the ethyl phosphonic acid diethyl ester (DEEP);
Described catalyzer is the mixture of the trolamine of the dibutyl tin laurate (DBTDL) of 50%-100% and 0-50%;
Described suds-stabilizing agent is a kind of tensio-active agent, and it is meant the silicon class tensio-active agent that contains the Si-C structure;
The invention still further relates to the preparation method of aforesaid polyurethane adiabatic heat-insulation foam material, comprise the steps:
The first step is used the surface treatment of silane coupling agent to the chopped glass fiber powder;
Described silane coupling agent is meant: γ-An Bingjisanyiyangjiguiwan (KH-550);
Described surface treatment is meant: the chopped glass fiber powder is immersed in 9: 1 ethanol/water mixing solutions, with acetate pH value is adjusted to 4-6, drip the silane coupling agent of 10% mass fraction, used magnetic agitation 6 hours, with mixture under 30W ultrasonic 30～40 minutes, use the B suction filtration stand-by again.
Second step, polyether glycol polyvalent alcohol, isocyanic ester and surface-treated chopped glass fiber powder for drying are handled, after carry out combination treatment and polymerization foaming successively and handle, obtain building the mould base, after the demoulding, will build the mould base and carry out maturation process, obtain the polyurethane heat-insulation foam material.
Described polyether glycol is meant: be initiator with sucrose, hydroxyl value is 450-500mgKOH/g, the polyether glycol of viscosity 6000～9000mPas in the time of 25 ℃;
Described drying treatment is meant: at 40 ℃ of following vacuum-drying 8h, surface-treated chopped glass fiber powder is at 120 ℃ with polyether glycol and isocyanic ester, following dry 6h;
Described combination treatment is meant: surface-treated chopped glass fiber powder is joined in the polyether glycol after the weighing by prescription, add entry, fire retardant, catalyzer, suds-stabilizing agent by prescription, fully stir with mechanical stirring device, mix, add pneumatogen again, use mechanical stirring device fully to stir, mix;
Described polymerization foaming is handled and is meant: isocyanic ester is joined rapidly in the blending ingredients, fully stir simultaneously, be poured into free foaming in the mould after 30～50 seconds, obtain to build the mould base.
Described maturation process is meant: reacted 40 minutes down at 40 ℃ together with mould, put into baking oven then, more than 100 ℃ of slaking 6h.
The present invention adopts the 3rd class zero odp environment-friendly foaming agent of HFCs class, cooperates the reinforcing filler of chopped glass fiber powder, the Halogen efficient flame-retarding agent, and fire-retardant, the heat-insulating property excellence is prepared density between 40～80Kg/m
3, have the rigid polyurethane foam of excellent compression performance simultaneously, have under the prerequisite of relatively low density, higher compression performance and modulus of compression, and the whipping agent environmental protection of using do not have destruction to ozonosphere, are applicable to as heat preserving and insulating material.
Embodiment
Below embodiments of the invention are elaborated, present embodiment is being to implement under the prerequisite with the technical solution of the present invention, provided detailed embodiment and concrete operating process, but protection scope of the present invention is not limited to following embodiment.
Embodiment
The first step, surface treatment to the chopped glass fiber powder: the chopped glass fiber powder is immersed in 9: 1 ethanol/water mixing solutions, with acetate pH value is adjusted to 4-6, drip the KH-550 silane coupling agent of 10% mass fraction, used magnetic agitation 6 hours, with mixture under 30W ultrasonic 30～40 minutes, use the B suction filtration stand-by again.
In second step, at 40 ℃ of following vacuum-drying 8h, surface-treated chopped glass fiber powder is at 120 ℃ with polyether glycol and isocyanic ester, following dry 6h, and room temperature is placed stand-by.Embodiment 1-9 prescription is as shown in table 1, surface-treated chopped glass fiber powder is joined in the polyether glycol after the weighing by prescription, add entry, fire retardant, catalyzer, suds-stabilizing agent by prescription, fully stir with mechanical stirring device, mix, add pneumatogen HFC-365mfc again, use mechanical stirring device fully to stir, mix; Isocyanic ester is joined rapidly in the blending ingredients, fully stir simultaneously, be poured into free foaming in the mould after 30～50 seconds, obtain to build the mould base.Reacted 40 minutes down at 40 ℃ together with mould, baking oven is put in the demoulding then, more than 100 ℃ of slaking 6h, obtains product.
Two steps with the foregoing description are the implementation step of following example 1-9 and Comparative Examples 1-3, and are as follows with reference to the raw materials quality mark proportioning of table 1:
The raw materials quality mark proportioning of table 1 example 1-9 and Comparative Examples 1-3
It is as follows that the foregoing description prepares the Performance Evaluation of gained composite foam material:
Compression performance: the sample of integral foam material cut growth 50mm, wide 50mm, high 50mm is tested by GB/T 8813-2008, and compression speed is 5mm/min; Combustionproperty: the sample of integral foam material cut growth 250mm, wide 20mm, high 20mm is measured its oxygen index by GB/T 8333-87; Heat-insulating property: the sample of integral foam material cut growth 300mm, wide 300mm, high 10mm is tested by the anti-hot-fluid conductometer HFM436 of company that speeds of use Germany, and the irregularity degree of sample is 0.5mm/m; Density: the sample of integral foam material cut growth 50mm, wide 50mm, high 50mm is tested by GB/T 6343-2009;
Example 1-9 and Comparative Examples 1-3 Performance Evaluation as follows:
The Performance Evaluation of table 2. example 1-9 and Comparative Examples 1-3
Claims (4)
1. the preparation method of a hard polyurethane adiabatic heat-insulation foam material, its component and content are: polyether glycol 100 weight parts, polymethylene multi-phenenyl isocyanate 150～170 weight parts, diameter 10-20 μ m, chopped glass fiber powder 5～30 weight parts of long 100-500 μ m, as 1 of pneumatogen, 1,1,3,3-3-pentafluorobutane 10～30 weight parts, water 1 weight part, fire retardant 10～15 weight parts, catalyzer 1～4 weight part of the mixture of the dibutyl tin laurate of 50%-100% and the trolamine of 0-50%, suds-stabilizing agent 1.5～10 weight parts that contain the Si--C structure, it is characterized in that described preparation method comprises the steps:
The first step is used the surface treatment of γ-An Bingjisanyiyangjiguiwan coupling agent to the chopped glass fiber powder;
Second step, polyether glycol, isocyanic ester and surface-treated chopped glass fiber powder for drying are handled, after carry out combination treatment and polymerization foaming successively and handle, obtain building the mould base, after the demoulding, will build the mould base and carry out maturation process, obtain the polyurethane heat-insulation foam material;
Described surface treatment is meant: the chopped glass fiber powder is immersed in 9: 1 ethanol/water mixing solutions, with acetate the pH value is adjusted to 4-6, drip the silane coupling agent of 10% mass fraction, used magnetic agitation 6 hours, with mixture under 30W ultrasonic 30～40 minutes, use the B suction filtration stand-by again;
Described drying treatment is meant: at 40 ℃ of following vacuum-drying 8h, surface-treated chopped glass fiber powder is at 120 ℃ of dry 6h down with polyether glycol and isocyanic ester;
Described combination treatment is meant: surface-treated chopped glass fiber powder is joined in the polyether glycol after the weighing by prescription, add entry, fire retardant, catalyzer, suds-stabilizing agent by prescription, fully stir with mechanical stirring device, mix, add pneumatogen again, use mechanical stirring device fully to stir, mix;
Described polymerization foaming is handled and is meant: isocyanic ester is joined rapidly in the blending ingredients, fully stir simultaneously, be poured into free foaming in the mould after 30～50 seconds, obtain to build the mould base;
Described maturation process is meant: reacted 40 minutes down at 40 ℃ together with mould, put into baking oven then, more than 100 ℃ of slaking 6h.
2. the preparation method of hard polyurethane adiabatic heat-insulation foam material according to claim 1 is characterized in that, described polyether glycol is to be initiator with sucrose, and hydroxyl value is 450-500mgKOH/g, viscosity 6000～9000mPas in the time of 25 ℃.
3. the preparation method of hard polyurethane adiabatic heat-insulation foam material according to claim 1, it is characterized in that, the content of isocyano is 30～32%wt in the described polymethylene multi-phenenyl isocyanate, viscosity 350～700mPas in the time of 25 ℃, and functionality is 2.6～3.1.
4. the preparation method of hard polyurethane adiabatic heat-insulation foam material according to claim 1, it is characterized in that, described fire retardant is not halogen-containing efficient flame-retarding agent, comprising: the mixture of one or both arbitrary proportions in methyl-phosphoric acid dimethyl ester (DMMP) and the ethyl phosphonic acid diethyl ester.
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| FR2882756B1 (en) * | 2005-03-04 | 2007-04-27 | Gaz Transp Et Technigaz Soc Pa | FOAM OF POLYURETHAN-POLYISOCYANURATE REINFORCED WITH GLASS FIBERS |
| US20060258762A1 (en) * | 2005-05-13 | 2006-11-16 | Dobransky Michael A | Hydrocarbon or hydrofluorocarbon blown ASTM E-84 class I rigid polyurethane foams |
| JP5333981B2 (en) * | 2008-01-31 | 2013-11-06 | 日本ポリウレタン工業株式会社 | Method for producing rigid polyurethane foam |
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