CN108137768A - 阻燃性硬质聚氨酯发泡体 - Google Patents
阻燃性硬质聚氨酯发泡体 Download PDFInfo
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- CN108137768A CN108137768A CN201680058401.XA CN201680058401A CN108137768A CN 108137768 A CN108137768 A CN 108137768A CN 201680058401 A CN201680058401 A CN 201680058401A CN 108137768 A CN108137768 A CN 108137768A
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- foaming body
- trimerization
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- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 title claims abstract description 31
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- 238000002474 experimental method Methods 0.000 description 8
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 8
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- 238000012360 testing method Methods 0.000 description 8
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- 229940106691 bisphenol a Drugs 0.000 description 7
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- 229910052744 lithium Inorganic materials 0.000 description 6
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- 229910052751 metal Inorganic materials 0.000 description 5
- 239000002184 metal Substances 0.000 description 5
- MSSNHSVIGIHOJA-UHFFFAOYSA-N pentafluoropropane Chemical compound FC(F)CC(F)(F)F MSSNHSVIGIHOJA-UHFFFAOYSA-N 0.000 description 5
- 239000000047 product Substances 0.000 description 5
- WZLFPVPRZGTCKP-UHFFFAOYSA-N 1,1,1,3,3-pentafluorobutane Chemical compound CC(F)(F)CC(F)(F)F WZLFPVPRZGTCKP-UHFFFAOYSA-N 0.000 description 4
- SVTBMSDMJJWYQN-UHFFFAOYSA-N 2-methylpentane-2,4-diol Chemical compound CC(O)CC(C)(C)O SVTBMSDMJJWYQN-UHFFFAOYSA-N 0.000 description 4
- JOYRKODLDBILNP-UHFFFAOYSA-N Ethyl urethane Chemical compound CCOC(N)=O JOYRKODLDBILNP-UHFFFAOYSA-N 0.000 description 4
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 4
- QIGBRXMKCJKVMJ-UHFFFAOYSA-N Hydroquinone Chemical compound OC1=CC=C(O)C=C1 QIGBRXMKCJKVMJ-UHFFFAOYSA-N 0.000 description 4
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- 239000004793 Polystyrene Substances 0.000 description 4
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 description 4
- 239000002253 acid Substances 0.000 description 4
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- 125000003006 2-dimethylaminoethyl group Chemical group [H]C([H])([H])N(C([H])([H])[H])C([H])([H])C([H])([H])* 0.000 description 3
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- 125000000217 alkyl group Chemical group 0.000 description 2
- 239000004411 aluminium Substances 0.000 description 2
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- LFVGISIMTYGQHF-UHFFFAOYSA-N ammonium dihydrogen phosphate Chemical compound [NH4+].OP(O)([O-])=O LFVGISIMTYGQHF-UHFFFAOYSA-N 0.000 description 2
- 229910000387 ammonium dihydrogen phosphate Inorganic materials 0.000 description 2
- 235000019826 ammonium polyphosphate Nutrition 0.000 description 2
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- 125000004429 atom Chemical group 0.000 description 1
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- KCIDZIIHRGYJAE-YGFYJFDDSA-L dipotassium;[(2r,3r,4s,5r,6r)-3,4,5-trihydroxy-6-(hydroxymethyl)oxan-2-yl] phosphate Chemical compound [K+].[K+].OC[C@H]1O[C@H](OP([O-])([O-])=O)[C@H](O)[C@@H](O)[C@H]1O KCIDZIIHRGYJAE-YGFYJFDDSA-L 0.000 description 1
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- HFGPZNIAWCZYJU-UHFFFAOYSA-N lead zirconate titanate Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Ti+4].[Zr+4].[Pb+2] HFGPZNIAWCZYJU-UHFFFAOYSA-N 0.000 description 1
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- CMVOJSWILFNLFI-UHFFFAOYSA-L magnesium;dibromate;hexahydrate Chemical compound O.O.O.O.O.O.[Mg+2].[O-]Br(=O)=O.[O-]Br(=O)=O CMVOJSWILFNLFI-UHFFFAOYSA-L 0.000 description 1
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- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- GYNNXHKOJHMOHS-UHFFFAOYSA-N methyl-cycloheptane Natural products CC1CCCCCC1 GYNNXHKOJHMOHS-UHFFFAOYSA-N 0.000 description 1
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- 230000004048 modification Effects 0.000 description 1
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- 239000000178 monomer Substances 0.000 description 1
- 229910000402 monopotassium phosphate Inorganic materials 0.000 description 1
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- 229910000403 monosodium phosphate Inorganic materials 0.000 description 1
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- 229910052901 montmorillonite Inorganic materials 0.000 description 1
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- SNMVRZFUUCLYTO-UHFFFAOYSA-N n-propyl chloride Chemical compound CCCCl SNMVRZFUUCLYTO-UHFFFAOYSA-N 0.000 description 1
- SLCVBVWXLSEKPL-UHFFFAOYSA-N neopentyl glycol Chemical compound OCC(C)(C)CO SLCVBVWXLSEKPL-UHFFFAOYSA-N 0.000 description 1
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- AHHWIHXENZJRFG-UHFFFAOYSA-N oxetane Chemical compound C1COC1 AHHWIHXENZJRFG-UHFFFAOYSA-N 0.000 description 1
- 125000004430 oxygen atom Chemical group O* 0.000 description 1
- 238000005192 partition Methods 0.000 description 1
- QCDYQQDYXPDABM-UHFFFAOYSA-N phloroglucinol Chemical compound OC1=CC(O)=CC(O)=C1 QCDYQQDYXPDABM-UHFFFAOYSA-N 0.000 description 1
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- GNSKLFRGEWLPPA-UHFFFAOYSA-M potassium dihydrogen phosphate Chemical compound [K+].OP(O)([O-])=O GNSKLFRGEWLPPA-UHFFFAOYSA-M 0.000 description 1
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- 239000010458 rotten stone Substances 0.000 description 1
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- CNALVHVMBXLLIY-IUCAKERBSA-N tert-butyl n-[(3s,5s)-5-methylpiperidin-3-yl]carbamate Chemical compound C[C@@H]1CNC[C@@H](NC(=O)OC(C)(C)C)C1 CNALVHVMBXLLIY-IUCAKERBSA-N 0.000 description 1
- CBXCPBUEXACCNR-UHFFFAOYSA-N tetraethylammonium Chemical class CC[N+](CC)(CC)CC CBXCPBUEXACCNR-UHFFFAOYSA-N 0.000 description 1
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- CZMILNXHOAKSBR-UHFFFAOYSA-N tetraphenylazanium Chemical class C1=CC=CC=C1[N+](C=1C=CC=CC=1)(C=1C=CC=CC=1)C1=CC=CC=C1 CZMILNXHOAKSBR-UHFFFAOYSA-N 0.000 description 1
- CIWAOCMKRKRDME-UHFFFAOYSA-N tetrasodium dioxido-oxo-stibonatooxy-lambda5-stibane Chemical compound [Na+].[Na+].[Na+].[Na+].[O-][Sb]([O-])(=O)O[Sb]([O-])([O-])=O CIWAOCMKRKRDME-UHFFFAOYSA-N 0.000 description 1
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 1
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- LLZRNZOLAXHGLL-UHFFFAOYSA-J titanic acid Chemical compound O[Ti](O)(O)O LLZRNZOLAXHGLL-UHFFFAOYSA-J 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 238000011282 treatment Methods 0.000 description 1
- STCOOQWBFONSKY-UHFFFAOYSA-N tributyl phosphate Chemical compound CCCCOP(=O)(OCCCC)OCCCC STCOOQWBFONSKY-UHFFFAOYSA-N 0.000 description 1
- CYRMSUTZVYGINF-UHFFFAOYSA-N trichlorofluoromethane Chemical compound FC(Cl)(Cl)Cl CYRMSUTZVYGINF-UHFFFAOYSA-N 0.000 description 1
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- RIUWBIIVUYSTCN-UHFFFAOYSA-N trilithium borate Chemical compound [Li+].[Li+].[Li+].[O-]B([O-])[O-] RIUWBIIVUYSTCN-UHFFFAOYSA-N 0.000 description 1
- WVLBCYQITXONBZ-UHFFFAOYSA-N trimethyl phosphate Chemical compound COP(=O)(OC)OC WVLBCYQITXONBZ-UHFFFAOYSA-N 0.000 description 1
- 150000004072 triols Chemical class 0.000 description 1
- XZZNDPSIHUTMOC-UHFFFAOYSA-N triphenyl phosphate Chemical compound C=1C=CC=CC=1OP(OC=1C=CC=CC=1)(=O)OC1=CC=CC=C1 XZZNDPSIHUTMOC-UHFFFAOYSA-N 0.000 description 1
- FIQMHBFVRAXMOP-UHFFFAOYSA-N triphenylphosphane oxide Chemical compound C=1C=CC=CC=1P(C=1C=CC=CC=1)(=O)C1=CC=CC=C1 FIQMHBFVRAXMOP-UHFFFAOYSA-N 0.000 description 1
- WUUHFRRPHJEEKV-UHFFFAOYSA-N tripotassium borate Chemical compound [K+].[K+].[K+].[O-]B([O-])[O-] WUUHFRRPHJEEKV-UHFFFAOYSA-N 0.000 description 1
- 229910000404 tripotassium phosphate Inorganic materials 0.000 description 1
- 235000019798 tripotassium phosphate Nutrition 0.000 description 1
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 description 1
- NSBGJRFJIJFMGW-UHFFFAOYSA-N trisodium;stiborate Chemical compound [Na+].[Na+].[Na+].[O-][Sb]([O-])([O-])=O NSBGJRFJIJFMGW-UHFFFAOYSA-N 0.000 description 1
- AUTOISGCBLBLBA-UHFFFAOYSA-N trizinc;diphosphite Chemical compound [Zn+2].[Zn+2].[Zn+2].[O-]P([O-])[O-].[O-]P([O-])[O-] AUTOISGCBLBLBA-UHFFFAOYSA-N 0.000 description 1
- 230000010148 water-pollination Effects 0.000 description 1
- 150000003751 zinc Chemical class 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- 239000011667 zinc carbonate Substances 0.000 description 1
- 235000004416 zinc carbonate Nutrition 0.000 description 1
- 229910000010 zinc carbonate Inorganic materials 0.000 description 1
- UGZADUVQMDAIAO-UHFFFAOYSA-L zinc hydroxide Chemical compound [OH-].[OH-].[Zn+2] UGZADUVQMDAIAO-UHFFFAOYSA-L 0.000 description 1
- 229910021511 zinc hydroxide Inorganic materials 0.000 description 1
- 229940007718 zinc hydroxide Drugs 0.000 description 1
- LRXTYHSAJDENHV-UHFFFAOYSA-H zinc phosphate Chemical compound [Zn+2].[Zn+2].[Zn+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O LRXTYHSAJDENHV-UHFFFAOYSA-H 0.000 description 1
- 229910000165 zinc phosphate Inorganic materials 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
- 229910000859 α-Fe Inorganic materials 0.000 description 1
- PAPBSGBWRJIAAV-UHFFFAOYSA-N ε-Caprolactone Chemical compound O=C1CCCCCO1 PAPBSGBWRJIAAV-UHFFFAOYSA-N 0.000 description 1
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Abstract
一种阻燃性硬质聚氨酯发泡体,其含有阻燃剂,其中,将所述发泡体在温度80℃、湿度85%的条件下进行一星期的湿热处理后的最大峰强度比(P1)与所述湿热处理前所述发泡体的最大峰强度比(P2)的比例(P1/P2×100)为85%以上。其中,所述P1和P2是指:对从所述发泡体的表层向内5mm~10mm的位置处的红外线吸收光谱进行测定,将1900~2000cm‑1的平均强度设为0时,1390~1430cm‑1的最大峰强度与1500~1520cm‑1的最大峰强度之比。
Description
技术领域
(与相关专利申请相互参照)
本申请主张2015年9月30日提出申请的日本特愿2015-194241号说明书的优先权的权利,本说明书参照该说明书全体并加以引用。
(技术领域)
本发明是关于一种阻燃性硬质聚氨酯发泡体。
背景技术
作为公寓等集合住宅、独栋住宅、学校的各种设施、商业大厦等建筑物的隔热材料,经常使用发泡聚氨酯树脂。但是,已知聚氨酯树脂的阻燃性较低,赋予隔热氨基甲酸酯材料阻燃性已经成为技术问题。而且,为长期保证其效果,要求阻燃性的耐湿热性,即要求其有能够在较高的湿度与较高的温度下维持阻燃性的性质。
作为致力于改善阻燃性聚氨酯树脂组合物的耐湿性的例子,例如专利文献1中含有聚氨酯的阻燃性聚氨酯树脂组合物的相关记载如下;该聚氨酯是通过以下方式获得:氧原子的平均含量为20重量%以下的由1种或2种以上的成分所构成的多元醇、以及相对于该多元醇由异氰酸酯基的数与上述多元醇的羟基的数的比例所求出的NCO/OH指数为200以上2,000以下的范围的重量的多异氰酸酯,使用相对于多元醇的100重量份为0.5重量份以上且20重量份以下的比例的金属系异氰尿酸酯化催化剂使上述两者进行反应。
专利文献2中对硬质聚氨酯发泡体的相关记载如下,该硬质聚氨酯发泡体的特征在于:将多异氰酸酯成分与混合有多元醇成分、发泡剂、催化剂及其他助剂的混合溶液混合并使其发泡而获得硬质聚氨酯发泡体,并且使用水作为发泡剂,含有咪唑系化合物的硬质聚氨酯发泡体作为催化剂,咪唑系化合物的含量相对于该混合溶液中的水分量的重量比例为0.05~5.0。
专利文献3中聚氨酯树脂组合物的相关记载如下,该聚氨酯树脂组合物系含有含羟基的化合物、含异氰酸酯基的化合物及金属氢氧化物(C)的聚氨酯树脂组合物(X),并且上述含羟基的化合物含有聚丁二烯多元醇(A)及蓖麻油系多元醇(B),上述金属氢氧化物(C)相对于聚氨酯树脂组合物(X)100质量份而含有55质量份~80质量份,上述蓖麻油系多元醇(B)与上述金属氢氧化物(C)的质量比为(B):(C)=1:5~1:10。
现有技术文献
专利文献
专利文献1:日本特开2000-169542
专利文献2:日本特开2004-059900
专利文献3:日本特开2015-131883
发明内容
本发明所要解决的技术问题
专利文献1中,通过使用氧原子的平均含量为20重量%以下的由1种或2种以上的成分所构成的多元醇,得到的聚氨酯树脂组合物的亲水性降低,耐湿性得到改善。
专利文献2中,通过使用规定量的咪唑系化合物作为催化剂,可以抑制使用水作为发泡剂时聚酯多醇的水解,提高混合液的储存稳定性。
专利文献3中,含异氰酸酯基的化合物由于含有异氰尿酸酯改性体,可以提高热耐久性。
但是,专利文献1~3任一者都没有记载:聚氨酯发泡体不仅满足建筑基准法所规定阻燃剂,还要改善耐湿性。
另外,专利文献1中通过使用特定多元醇,专利文献2中通过规定量的咪唑系化合物作为催化剂,专利文献3中通过使用含有异氰尿酸酯改性体的异氰酸酯来改善耐湿性,三者用以改善耐湿性的成分各不相同,并未通过共同的指标评价聚氨酯发泡体的耐湿热性。
本发明的目的在于提供一种阻燃性的耐湿热性得以提高的阻燃性硬质聚氨酯发泡体。
解决课题的技术方案
本发明的发明人为了实现上述目的进行了研究,发现由湿热导致阻燃性降低的原因在于水分导致的异氰尿酸酯基的分解,由此完成本发明。
即,根据本发明的一个实施方式,提供一种阻燃性硬质聚氨酯发泡体,其含有阻燃剂,其中,将所述发泡体在温度80℃、湿度85%的条件下进行一星期的湿热处理后的最大峰强度比(P1)与所述湿热处理前所述发泡体的最大峰强度比(P2)的比例(P1/P2×100)为85%以上。
其中,所述P1和P2是指:对从所述发泡体的表层向内5mm~10mm的位置处的红外线吸收光谱进行测定,将1900~2000cm-1的平均强度设为0时,1390~1430cm-1的最大峰强度与1500~1520cm-1的最大峰强度之比。
发明效果
本发明的阻燃性硬质聚氨酯发泡体具备能够耐受较高的湿度和较高的温度并维持阻燃性的性质。
具体实施方式
本发明包括一种阻燃性硬质聚氨酯发泡体,其为含有阻燃剂的阻燃性硬质聚氨酯发泡体,其特征在于,将发泡体在温度80℃、湿度85%的条件下进行一星期的湿热处理后的最大峰强度比(P1)与所述湿热处理前所述发泡体的最大峰强度比(P2)的比例(P1/P2×100)为85%以上。
其中,所述P1和P2是指:对从所述发泡体的表层向内5mm~10mm的位置处的红外线吸收光谱进行测定,将1900~2000cm-1的平均强度设为0时,1390~1430cm-1的最大峰强度与1500~1520cm-1的最大峰强度之比。
上述比例是将1900~2000cm-1的平均强度设为0时,且将1500~1520cm-1的最大峰强度设为1时,用百分率表示的在1390~1430cm-1下在温度80℃、湿度85%下进行一星期的湿热处理后的最大峰强度与湿热处理前的最大峰强度的比例。
本发明的阻燃性硬质聚氨酯发泡体是通过使发泡性聚氨酯树脂组合物发泡及固化而获得。以下,对发泡性聚氨酯树脂组合物的成分进行说明。
发泡性聚氨酯树脂组合物含有多元醇、芳香族多异氰酸酯、泡沫稳定剂、催化剂、发泡剂、阻燃剂及任意选择的其他成分。作为聚氨酯树脂的主剂的芳香族多异氰酸酯与作为聚氨酯树脂的固化剂的多元醇通过化学反应而进行固化,而形成聚氨酯树脂。以下,对各成分进行说明。
1.芳香族多异氰酸酯
作为聚氨酯树脂主剂的芳香族多异氰酸酯,可列举:苯二异氰酸酯、甲苯二异氰酸酯、苯二甲基二异氰酸酯、二苯基甲烷二异氰酸酯、二甲基二苯基甲烷二异氰酸酯、三苯甲烷三异氰酸酯、萘二异氰酸酯、聚亚甲基聚苯基多异氰酸酯等。
芳香族多异氰酸酯可使用一种或两种以上。出于易使用,易获得等原因,聚氨酯树脂的主剂优选为二苯基甲烷二异氰酸酯。
2.多元醇
作为聚氨酯树脂固化剂的多元醇,可列举:聚内酯多元醇、聚碳酸酯多元醇、芳香族多元醇、脂环族多元醇、脂肪族多元醇、聚酯多元醇、聚合物多元醇、聚醚多元醇等。
作为聚内酯多元醇,可列举:聚丙内酯二醇、聚己内酯二醇、聚戊内酯二醇等。
作为聚碳酸酯多元醇,可列举:通过乙二醇、丙二醇、丁二醇、戊二醇、己二醇、辛二醇、壬二醇等含羟基的化合物与碳酸二亚乙酯、碳酸二亚丙酯等碳酸二亚烷基酯的脱醇反应所获得的多元醇等。
作为芳香族多元醇,可列举:双酚A、双酚F、苯酚酚醛清漆、甲酚酚醛清漆等。
作为脂环族多元醇,可列举:环己二醇、甲基环己二醇、异佛尔酮二醇、二环己基甲烷二醇、二甲基二环己基甲烷二醇等。
作为脂肪族多元醇,可列举:乙二醇、丙二醇、丁二醇、戊二醇、己二醇等。
作为聚酯多元醇,可列举:使多元酸与多元醇进行脱水缩合所获得的聚合物、使ε-己内酯、α-甲基-ε-己内酯等内酯进行开环聚合所获得的聚合物、羟基羧酸与上述多元醇等形成的缩合物。
此处,作为多元酸,具体而言,可列举:己二酸、壬二酸、癸二酸、对苯二甲酸、间苯二甲酸、琥珀酸等。另外,作为多元醇,具体而言,可列举:双酚A、乙二醇、1,2-丙二醇、1,4-丁二醇、二乙二醇、1,6-己烷二醇、新戊二醇等。
另外,作为羟基羧酸,具体而言,可列举:蓖麻油、蓖麻油与乙二醇的反应生成物等。
作为聚合物多元醇,可列举:使丙烯腈、苯乙烯、丙烯酸甲酯、甲基丙烯酸酯等乙烯性不饱和化合物对芳香族多元醇、脂环族多元醇、脂肪族多元醇、聚酯多元醇等进行接枝聚合而获得的聚合物、聚丁二烯多元醇、多元醇的改性多元醇、或上述化合物的氢化物等。
作为多元醇的改性多元醇,可列举:使环氧烷烃与原料多元醇反应进行改性而得到的改性多元醇等。
作为多元醇,可列举:甘油及三羟甲基丙烷等三元醇;季戊四醇、山梨醇、甘露醇、山梨醇酐、双甘油、二季戊四醇等、蔗糖、葡萄糖、甘露糖、果糖、甲基葡糖苷及其衍生物等四~八元醇;苯酚、间苯三酚、甲酚、邻苯三酚、邻苯二酚、对苯二酚、双酚A、双酚F、双酚S、1-羟基萘、1,3,6,8-四羟基萘、蒽酚、1,4,5,8-四羟基蒽、1-羟基芘等酚聚丁二烯多元醇;蓖麻油多元醇;(甲基)丙烯酸羟基烷基酯的(共)聚合物及聚乙烯醇等多官能(例如官能团数2~100)多元醇、苯酚与甲醛的缩合物(酚醛清漆)。
多元醇的改性方法并无特别限定。作为改性方法,适宜使用对多元醇加成环氧烷烃(以下简称为AO)的方法。
作为AO,可列举碳原子数2~6的AO,例如环氧乙烷(以下,简称为EO)、1,2-环氧丙烷(以下,简称为PO)、1,3-环氧丙烷、1,2-环氧丁烷、1,4-环氧丁烷等。
上述化合物中,就性状或反应性的观点而言,优选为PO、EO及1,2-环氧丁烷,更加优选为PO及EO。作为使用两种以上的AO时(例如PO及EO)的加成方法,可为嵌段加成也可为无规加成,也可将并用两者。
作为聚醚多元醇,可列举在具有2个以上的活性氢的低分子量活性氢化合物等中的至少一种的存在下,使环氧乙烷、环氧丙烷、四氢呋喃等环氧烷烃的至少1种进行开环聚合所获得的聚合物。
作为具有2个以上的活性氢的低分子量活性氢化合物,可列举:双酚A、乙二醇、丙二醇、丁二醇、1,6-己二醇等二醇;甘油、三羟甲基丙烷等三醇;乙二胺、丁二胺等胺等。
本发明中使用的多元醇就降低燃烧时的总发热量的效果而言,优选使用聚酯多元醇、或聚醚多元醇。
其中,更加优选使用分子量200~800的聚酯多元醇,进一步优选使用分子量300~500的聚酯多元醇。
另外,异氰酸酯指数是以百分率表示多异氰酸酯的异氰酸酯基相对于多元醇的羟基的当量比,其值超过100时,意味着相比于羟基,异氰酸酯基过量。
本发明中使用的聚氨酯树脂的异氰酸酯指数的范围并无特别限定,优选为150~1000的范围,更加优选为200~800的范围,进一步优选为250~700的范围。异氰酸酯指数(INDEX)是通过以下的方法而算出的。
INDEX=异氰酸酯的当量数÷(多元醇的当量数+水的当量数)×100
此处,异氰酸酯的当量数=NCO的分子量÷NCO含量(%)×100,
多元醇的当量数=OHV×使用份数÷KOH的分子量,
OHV为多元醇的羟值(mg KOH/g),
水的当量数=使用份数/水的分子量×水的OH基数。
需要说明的是,在上述式中,NCO的分子量设为42,KOH的分子量设为56100,水的分子量设为18,水的OH基的数设为2。
3.泡沫稳定剂
作为泡沫稳定剂,可列举:聚氧亚烷基烷基醚等聚氧亚烷基泡沫稳定剂、有机聚硅氧烷等聚硅氧烷泡沫稳定剂等表面活性剂等。
泡沫稳定剂的添加量根据聚氨酯树脂而适当设定,如果列举一例的话,例如,相对于聚氨酯树脂100重量份,优选为0.1重量份~10重量份的范围。
泡沫稳定剂可使用一种或两种以上。
4.催化剂
作为催化剂,可列举三聚催化剂。
三聚催化剂使作为聚氨酯树脂主剂的芳香族多异氰酸酯中所含的异氰酸酯基进行反应而使之三聚化,从而促进异氰尿酸酯环的生成。
为了促进异氰尿酸酯环的生成,例如,作为三聚催化剂,可使用:三(二甲氨基甲基)苯酚、2,4-双(二甲氨基甲基)苯酚、2,4,6-三(二烷基氨基烷基)六氢均三嗪等含氮芳香族化合物;乙酸钾、2-乙基己酸钾、辛酸钾等羧酸碱金属盐;三甲基铵盐、三乙基铵盐、三苯基铵盐等叔铵盐;四甲基铵盐、四乙基铵盐、四苯基铵盐等季铵盐。
三聚催化剂的量相对于聚氨酯树脂100重量份,优选为0.6重量份~10重量份的范围,更加优选为0.6重量份~8重量份的范围,进一步优选为0.6重量份~6重量份的范围,最为优选0.6重量份~3重量份的范围。其为0.6重量份以上时,不会发生芳香族多异氰酸酯的三聚化受到抑制的不良状况,其为10重量份以下时,能够维持适当的发泡速度,易于操作。
另外,作为催化剂,除三聚催化剂以外,也可列举下述树脂化或泡化催化剂:烷基化聚亚烷基多胺、三乙基胺、三乙二胺、N,N,N',N'-四甲基六亚甲基二胺、N",N"-五甲基二乙三胺、N,N,N'-三甲基氨基乙基-乙醇胺、三乙二胺双(2-二甲氨基乙基)醚、氨基甲酸酯催化剂等胺;N-甲基吗啉双(2-二甲氨基乙基)醚、N,N,N'-双(2-二甲氨基乙基)醚、N-甲基-N'-二甲氨基乙基哌啶、咪唑环中的叔胺官能团被氰乙基取代而成的咪唑化合物等含氮原子的催化剂等。
在该三聚催化剂以外的催化剂包含于发泡性聚氨酯树脂组合物中时,该三聚催化剂以外的催化剂的添加量以三聚催化剂与三聚催化剂以外的催化剂的合计量计算,相对于聚氨酯树脂100重量份,优选为0.6重量份~10重量份的范围,更加优选为0.6重量份~8重量份的范围,进一步优选为0.6重量份~6重量份的范围,最为优选为0.6重量份~3重量份的范围。
其为0.6重量份以上时,不会发生尿烷键的形成受到抑制的不良状况,其为10重量份以下时,能够维持适当的发泡速度,易于操作。
虽然不希望被理论束缚,但本发明人员发现:使用胺作为催化剂时,容易发生水分所引起的异氰尿酸酯基的分解。因此,在本发明中,优选三聚催化剂以外的催化剂中胺的添加量较少,尤其优选为叔胺的添加量较少。需要说明的是,咪唑环中的仲胺官能团被氰乙基等经取代或未经取代的烃基取代而成的咪唑化合物也包括在叔胺中。
作为三聚催化剂以外的催化剂的叔胺的添加量相对于聚氨酯树脂100重量份,优选为3重量份以下,更加优选为2.9重量份以下。作为三聚催化剂以外的催化剂的叔胺的添加量的下限并无特别限定,相对于聚氨酯树脂100重量份,优选为0重量份以上,更加优选为0.1重量份以上,进一步优选为0.2重量份以上。
作为三聚催化剂以外的优选的其他催化剂,可例示1,2-二甲基咪唑等。
在一个实施方式中,发泡性聚氨酯树脂组合物不包含作为催化剂的胺。在另一个实施方式中,发泡性聚氨酯树脂组合物不包含作为催化剂的叔胺。在另一个实施方式中,发泡性聚氨酯树脂组合物不包含作为催化剂的烷基化聚亚烷基多胺、三乙基胺、N",N"-五甲基二乙三胺、N,N,N'-三甲基氨基乙基-乙醇胺、以及氨基甲酸酯催化剂中的至少一种。
另外,在本发明的一个实施方式中,发泡性聚氨酯树脂组合物含有具有两亲性的催化剂作为三聚催化剂以外的催化剂。具有两亲性的催化剂的含量相对于聚氨酯树脂100重量份为1.5重量份以下,优选为1.0重量份以下,更加优选为0.5重量以下。具有两亲性的催化剂的含量的下限并无特别限定,相对于聚氨酯树脂100重量份,优选为0重量份以上。
可以认为具有两亲性的催化剂通过使水与聚氨酯树脂亲和而促进异氰尿酸酯的水解。
再者,在本发明中,具有“两亲性的催化剂”是指通过以下的试验所获得的水分量为4.0%以上的催化剂。
水分量是采用如下值:将10g的磷酸三(β-氯丙基)酯(TMCPP)、1g的水及1g的催化剂混合后,充分静置,然后,通过卡尔费歇法测定TMCPP层的水分量而得到的值。
催化剂可使用一种或两种以上。
5.发泡剂
发泡剂促进聚氨酯树脂的发泡。作为发泡剂,可列举:水;丙烷、丁烷、戊烷、己烷、庚烷、环丙烷、环丁烷、环戊烷、环己烷、环庚烷等低沸点的烃;二氯乙烷、氯丙烷、氯异丙烷、氯丁烷、氯异丁烷、氯戊烷、氯异戊烷等氯化脂肪族烃化合物;CHF3、CH2F2、CH3F等氟化合物;三氯单氟甲烷、三氯三氟乙烷、二氯单氟乙烷、(例如,HCFC141b(1,1-二氯-1-氟乙烷)、HCFC22(氯二氟甲烷)、HCFC142b(1-氯-1,1-二氟乙烷))等氯氟碳氢化合物;HFC-245fa(1,1,1,3,3-五氟丙烷)、HFC-365mfc(1,1,1,3,3-五氟丁烷)等氢氟碳;二异丙基醚等醚化合物、或上述化合物的混合物等有机类物理发泡剂、氮气、氧气、氩气、二氧化碳气体等无机类物理发泡剂等。
发泡剂的配比量并无特别限定,相对于聚氨酯树脂100重量份,优选为0.1重量份~30重量份的范围。发泡剂的配比量相对于聚氨酯树脂100重量份,更加优选为0.1重量份~18重量份的范围,进一步优选为0.5重量份~18重量份的范围,最优选为1重量份~10重量份的范围。
水的范围为0.1重量份以上时,能够促进发泡,降低得到的成形体的密度,其为30重量份以下时,能够防止发泡体不发泡而未形成发泡体的情况。
发泡剂可使用一种或两种以上。
6.阻燃剂
阻燃剂含有选自红磷、磷酸酯、含磷酸盐的阻燃剂、含溴的阻燃剂、含硼的阻燃剂、含锑的阻燃剂、以及金属氢氧化物中的至少一种。优选为阻燃剂含有红磷,并且含有选自磷酸酯、含磷酸盐的阻燃剂、含溴的阻燃剂、含硼的阻燃剂、含锑的阻燃剂以及金属氢氧化物中的至少一种。
阻燃剂可适当选择使用市售品。
对于本发明中使用的红磷并无限定,可适当选择使用市售品。
红磷的添加量相对于聚氨酯树脂100重量份,优选为2重量份~30重量份的范围,更加优选为3.5~20重量份的范围,更加优选为6.0重量份~18重量份的范围。
红磷的范围为3.5重量份以上时,会保持阻燃性聚氨酯树脂组合物的自熄性,另外,其为20重量份以下时,不会抑制阻燃性聚氨酯树脂组合物的发泡。
另外,本发明中使用的磷酸酯并无特别限定,优选为使用单磷酸酯、缩合磷酸酯等。
作为单磷酸酯,并无特别限定,可列举:磷酸三甲酯、磷酸三乙酯、磷酸三丁酯、磷酸三(2-乙基己基)酯、磷酸三(丁氧基乙基)酯、磷酸三苯酯、磷酸三甲酚酯、磷酸三(二甲苯基)酯、磷酸三(异丙基苯基)酯、磷酸三(苯基苯基)酯、磷酸三萘酯、磷酸甲酚酯二苯酯、磷酸二甲基苯酯二苯酯、磷酸二苯酯2-乙基己酯、磷酸二(异丙基苯基)酯苯酯、磷酸单异癸酯、酸式磷酸2-丙烯酰氧基乙酯、酸式磷酸2-甲基丙烯酰氧基乙酯、磷酸二苯酯2-丙烯酰氧基乙酯、磷酸二苯酯2-甲基丙烯酰氧基乙酯、磷酸三聚氰胺、磷酸二(三聚氰胺)、焦磷酸三聚氰胺、三苯基氧化膦、三甲酚氧化膦、甲基膦酸二苯酯、苯基膦酸二乙酯、间苯二酚双(磷酸二苯酯)、双酚A双(磷酸二苯酯)、磷杂菲、磷酸三(β-氯丙基)酯等。
作为缩合磷酸酯,并无特别限定,可列举:三烷基聚磷酸酯、间苯二酚聚苯基磷酸酯(resorcinol polyphenyl phosphate)、间苯二酚聚(二-2,6-二甲苯基)磷酸酯(大八化学工业公司制造,商品名PX-200)、对苯二酚聚(2,6-二甲苯基)磷酸酯以及上述缩合物等缩合磷酸酯。
作为市售的缩合磷酸酯,可列举:间苯二酚聚苯基磷酸酯(商品名CR-733S)、双酚A聚甲酚磷酸酯(商品名CR-741)、芳香族缩合磷酸酯(商品名CR747)、间苯二酚聚苯基磷酸酯(ADEKA公司制造,商品名Adekastab PFR)、双酚A聚甲酚磷酸酯(商品名FP-600、FP-700)等。
上述化合物中,为使固化前的组合物中的粘度下降的效果及使初始的发热量降低的效果较高,优选使用单磷酸酯,更加优选使用磷酸三(β-氯丙基)酯。
磷酸酯可使用一种或两种以上。
磷酸酯的添加量相对于聚氨酯树脂100重量份,优选为1.5重量份~52重量份的范围,更加优选为1.5重量份~20重量份的范围,进一步优选为2.0重量份~15重量份的范围,最为优选为2.0重量份~10重量份的范围。
磷酸酯的范围为1.5重量份以上时,能够防止由发泡性聚氨酯树脂组合物形成的成形品因火灾的热而形成的致密残渣发生破碎的情况,磷酸酯的范围为52重量份以下时,不会抑制发泡性聚氨酯树脂组合物的发泡。
另外,本发明中使用的含磷酸盐的阻燃剂包括磷酸。含磷酸盐的阻燃剂所使用的磷酸并无特别限定,可列举:单磷酸、焦磷酸、聚磷酸及它们的组合等各种磷酸。
作为含磷酸盐的阻燃剂,可列举:由各种磷酸与选自周期表IA族~IVB族的金属、氨、脂肪族胺、芳香族胺中的至少一种金属或化合物的盐所形成的磷酸盐。作为周期表IA族~IVB族的金属,可列举:锂、钠、钙、钡、铁(II)、铁(III)、铝等。
另外,作为脂肪族胺,可列举:甲基胺、乙基胺、二乙基胺、三乙基胺、乙二胺、哌啶等。
另外,作为芳香族胺,可列举:吡啶、三嗪、三聚氰胺、铵等。
再者,上述含磷酸盐的阻燃剂可通过施加硅烷偶合剂处理、以三聚氰胺树脂进行被覆等公知的耐水性提高处理,也可添加三聚氰胺、季戊四醇等公知的发泡助剂。
作为含磷酸盐的阻燃剂的具体例,可列举:单磷酸盐、焦磷酸盐、聚磷酸盐等。
作为单磷酸盐,并无特别限定,可列举:磷酸铵、磷酸二氢铵、磷酸氢二铵等铵盐;磷酸一钠、磷酸二钠、磷酸三钠、亚磷酸一钠、亚磷酸二钠、次磷酸钠等钠盐;磷酸一钾、磷酸二钾、磷酸三钾、亚磷酸一钾、亚磷酸二钾、次磷酸钾等钾盐;磷酸一锂、磷酸酸二锂、磷酸三锂、亚磷酸一锂、亚磷酸二锂、次磷酸锂等锂盐;磷酸二氢钡、磷酸氢钡、磷酸三钡、次磷酸钡等钡盐;磷酸一氢镁、磷酸氢镁、磷酸三镁、次磷酸镁等镁盐;磷酸二氢钙、磷酸氢钙、磷酸三钙、次磷酸钙等钙盐;磷酸锌、亚磷酸锌、次磷酸锌等锌盐等。
另外,作为聚磷酸盐,并无特别限定,可列举:聚磷酸铵、聚磷酸哌啶、聚磷酸三聚氰胺、聚磷酸铵酰胺、聚磷酸铝等。
上述化合物中,为了提高含磷酸盐的阻燃剂的自熄性。优选使用单磷酸盐,更加优选使用磷酸二氢铵。
含磷酸盐的阻燃剂可使用一种或两种以上。
本发明中使用的含磷酸盐的阻燃剂的添加量相对于聚氨酯树脂100重量份,优选为1.5重量份~52重量份的范围,更加优选为1.5重量份~20重量份的范围,进一步优选为2.0重量份~15重量份的范围,最优选为2.0重量份~10重量份的范围。
另外,作为本发明中使用的含溴的阻燃剂,只要是分子结构中含有溴的化合物,则无特别限定,可列举芳香族溴化合物等。
作为芳香族溴化合物的具体例子,可列举:六溴苯、五溴甲苯、六溴联苯、十溴联苯、六溴环癸烷、十溴二苯醚、八溴二苯醚、六溴二苯醚、双(五溴苯氧基)乙烷、亚乙基双(四溴邻苯二甲酰亚胺)、四溴双酚A等单体有机溴化合物;以溴化双酚A为原料所制造的聚碳酸酯低聚物、聚碳酸酯低聚物与双酚A的共聚物等溴化聚碳酸酯;通过溴化双酚A与表氯醇的反应所制造的二环氧化合物、通过溴化酚类与表氯醇的反应所获得的单环氧化合物等溴化环氧化合物;聚(丙烯酸溴苄酯);溴化聚苯醚;溴化双酚A、三聚氯化氰及溴化苯酚的缩合物;溴化(聚苯乙烯)、聚(溴化苯乙烯)、交联溴化聚苯乙烯等溴化聚苯乙烯;交联或非交联溴化聚(甲基苯乙烯)等经卤化的溴化合物聚合物。
就控制燃烧初期的发热量的观点而言,优选为溴化聚苯乙烯、六溴苯等,更加优选为六溴苯。
含溴的阻燃剂可使用一种或两种以上。
本发明中使用的含溴的阻燃剂的添加量相对于聚氨酯树脂100重量份,优选为1.5重量份~52重量份的范围,更加优选为1.5重量份~20重量份的范围,进一步优选为2.0重量份~15重量份的范围,最为优选为2.0重量份~10重量份的范围。
另外,作为本发明中使用的含硼的阻燃剂,可列举:硼砂、氧化硼、硼酸、硼酸盐等。
作为氧化硼,可列举:三氧化二硼、三氧化硼、二氧化二硼、三氧化四硼、五氧化四硼等。
作为硼酸盐,可列举:碱金属、碱土金属、周期表第4族、第12族、第13族的元素及铵的硼酸盐等。
具体而言,可列举:硼酸锂、硼酸钠、硼酸钾、硼酸铯等硼酸碱金属盐、硼酸镁、硼酸钙、硼酸钡等硼酸碱土金属盐、硼酸锆、硼酸锌、硼酸铝、硼酸铵等。
本发明中使用的含硼的阻燃剂优选为硼酸盐,更加优选为硼酸锌。
含硼的阻燃剂可使用一种或两种以上。
本发明中使用的含硼的阻燃剂的添加量相对于聚氨酯树脂100重量份,优选为1.5重量份~52重量份的范围,更加优选为1.5重量份~20重量份的范围,进一步优选为2.0重量份~15重量份的范围,最优选为2.0重量份~10重量份的范围。
另外,作为本发明中使用的含锑的阻燃剂,可列举:氧化锑、锑酸盐、焦锑酸盐等。
作为氧化锑,可列举:三氧化锑、五氧化锑等。
作为锑酸盐,可列举:锑酸钠、锑酸钾等。
作为焦锑酸盐,可列举:焦锑酸钠、焦锑酸钾等。
本发明中使用的含锑的阻燃剂优选为氧化锑。
含锑的阻燃剂可使用一种或两种以上。
含锑的阻燃剂的添加量相对于聚氨酯树脂100重量份,优选为1.5重量份~52重量份的范围,更加优选为1.5重量份~20重量份的范围,进一步优选为2.0重量份~15重量份的范围,最为优选为2.0重量份~10重量份的范围。
另外,作为本发明中使用的金属氢氧化物,可列举:氢氧化镁、氢氧化钙、氢氧化铝、氢氧化铁、氢氧化镍、氢氧化锆、氢氧化钛、氢氧化锌、氢氧化铜、氢氧化钒、氢氧化锡等。
金属氢氧化物可使用一种或两种以上。
金属氢氧化物的添加量相对于聚氨酯树脂100重量份,优选为1.5重量份~52重量份的范围,更加优选为1.5重量份~20重量份的范围,进一步优选为2.0重量份~15重量份的范围,最为优选为2.0重量份~10重量份的范围。
本发明中使用的阻燃剂的合计量相对于聚氨酯树脂100重量份,优选为4.5重量份~70重量份的范围,更加优选为4.5重量份~40重量份的范围,进一步优选为4.5重量份~30重量份的范围。
阻燃剂的范围为4.5重量份以上时,能够防止由发泡性聚氨酯树脂组合物所构成的成形品在火灾中因热而形成的致密残渣发生破碎,其为70重量份以下时,不会抑制发泡性聚氨酯树脂组合物的发泡。
在优选的实施方式中,发泡性聚氨酯树脂组合物中,以由芳香族多异氰酸酯与多元醇所构成的聚氨酯树脂100重量份为基准,其中的芳香族多异氰酸酯为50~85重量份,且含有0.1重量份~10重量份的泡沫稳定剂,0.6~10重量份的催化剂,0.1~30重量份的发泡剂,4.5重量份~70重量份的阻燃剂,阻燃剂中的红磷为3重量份~18重量份的范围,选自磷酸酯、含磷酸盐的阻燃剂、含溴的阻燃剂、含硼的阻燃剂、含锑的阻燃剂、及金属氢氧化物中的至少1种为1.5重量份~52重量份。在该情形时,催化剂优选为3.5~10重量份。阻燃剂优选为4.5重量份~52重量份,更加优选为4.5重量份~30重量份,优选的范围为1.5重量份~9重量份的范围。选自磷酸酯、含磷酸盐的阻燃剂、含溴的阻燃剂、含硼的阻燃剂、含锑的阻燃剂、及金属氢氧化物中的至少1种优选为含硼的阻燃剂。
7.其他成分
发泡性聚氨酯树脂组合物也可进一步含有无机填充材。作为无机填充材,并无特别限定,可列举:氧化硅、硅藻土、氧化铝、氧化钛、氧化钙、氧化镁、氧化铁、氧化锡、氧化锑、铁氧体类、碱性碳酸镁、碳酸钙、碳酸镁、碳酸锌、碳酸钡、碳钠铝石、铝碳酸镁、硫酸钙、硫酸钡、石膏纤维、硅酸钙等钾盐、滑石、粘土、云母、硅灰石、蒙脱石、膨润土、活性白土、海泡石、丝状铝英石、绢云母、玻璃纤维、玻璃珠、硅土中空球、氮化铝、氮化硼、氮化硅、碳黑、石墨、碳纤维、碳中空球、木炭粉末、各种金属粉、钛酸钾、硫酸镁、钛酸锆酸铅、硼酸铝、硫化钼、碳化硅、不锈钢纤维、各种磁性粉、矿渣纤维、飞灰、硅铝纤维、氧化铝纤维、氧化硅纤维、氧化锆纤维等。
无机填充材可使用一种或两种以上。
发泡性聚氨酯树脂组合物在各自不损害本发明的目的的范围内,视需要可含有:酚系、胺类、硫类等抗氧化剂;热稳定剂、金属毒害抑制剂、抗静电剂、稳定剂、交联剂、润滑剂、软化剂、颜料、增粘树脂等辅助成分;聚丁烯、石油树脂等增粘剂。
由于上述1.~7.的成分混合,发泡性聚氨酯树脂组合物发生反应而固化,故而其粘度随着时间经过而发生变化。因此,使用发泡性聚氨酯树脂组合物之前,将发泡性聚氨酯树脂组合物分割为两部分以上,从而防止发泡性聚氨酯树脂组合物发生反应而固化。并且,使用发泡性聚氨酯树脂组合物时,通过将分割为两部分以上的发泡性聚氨酯树脂组合物合而为一,而获得发泡性聚氨酯树脂组合物。
需要说明的是,通过如下方式将各成分分割即可,即,将发泡性聚氨酯树脂组合物分割为两部分以上时,分割为两部分以上的发泡性聚氨酯树脂组合物的各成分不会单独开始固化,将发泡性聚氨酯树脂组合物的各成分混合后,开始固化反应。
发泡性聚氨酯树脂组合物的固化可于混合及常温下进行,也可预先将各成分加热。
上述泡沫稳定剂、催化剂、发泡剂及阻燃剂可与多元醇或芳香族多异氰酸酯的任一者混合,也可与多元醇及芳香族多异氰酸酯分别地提供,优选为多元醇、泡沫稳定剂、催化剂、发泡剂、及阻燃剂以含有多元醇及这些成分的多元醇预混物的形式提供。另外,上述7.的其他成分可与多元醇或芳香族多异氰酸酯的任一者混合,也可与多元醇及芳香族多异氰酸酯分别地提供,优选为包含于多元醇预混物中。
将多元醇、芳香族多异氰酸酯、泡沫稳定剂、催化剂、发泡剂及阻燃剂异氰酸酯、优选为芳香族多异氰酸酯,与含有多元醇、泡沫稳定剂、催化剂、发泡剂、及阻燃剂的多元醇预混物进行混合,所产生的发泡性聚氨酯树脂组合物进行发泡及固化而成为聚氨酯发泡体。
关于本发明的聚氨酯发泡体,在温度80℃、湿度85%的条件下将上述发泡体进行一星期的湿热处理后的最大峰强度比(P1)与进行湿热处理前的上述发泡体的最大峰强度比(P2)的比例(P1/P2×100)为85%以上。比例优选为89%以上,更加优选为90%以上。
上述比例(P1/P2×100)可作为阻燃性硬质聚氨酯发泡体的阻燃性及耐湿热性的指标使用。
温度80℃、湿度85%的湿热处理是在建筑领域经常使用的热湿处理的加速试验,温度80℃、湿度85%、两星期的湿热处理相当于在通常的温度及湿度下进行一年的试验。
对从聚氨酯发泡体的表层向内5mm~10mm的位置的IR进行测定是为了避开易放热的表层,对组成稳定的位置进行测定。1390~1430cm-1的范围的波峰的最大值表示异氰尿酸酯,1500~1520cm-1的范围的波峰的最大值表示芳香环。
在本说明书中,将1900~2000cm-1的平均强度设为0时的1390~1430cm-1的范围的波峰的最大值与1500~1520cm-1的范围的波峰的最大值之比(1390~1430cm-1的范围的波峰的最大值/1500~1520cm-1的范围的波峰的最大值)称为异氰尿酸酯比(或简称为尿酸酯比)。意外地,该异氰尿酸酯比可作为评价阻燃性硬质聚氨酯发泡体的阻燃性的耐湿热性的指标。在温度80℃、湿度85%进行一星期的湿热处理后的异氰尿酸酯比相对于湿热处理前的异氰尿酸酯比为85%以上时,阻燃性硬质聚氨酯发泡体具备优异的阻燃性的耐湿热性。
若在温度80℃、湿度85%进行一星期的湿热处理后的异氰尿酸酯比相对于湿热处理前的异氰尿酸酯比未达85%时,则湿热后的阻燃性变得不良。
本发明的阻燃性硬质聚氨酯发泡体的耐火性可通过依据ISO-5660的试验方法的锥形卡路里计试验进行评价。具体而言,在该耐火试验中,将由发泡性聚氨酯树脂组合物形成的聚氨酯发泡体切割为长度10cm、宽度10cm及厚度5cm,准备锥形卡路里计试验用样品。接着,使用锥形卡路里计试验用样品,依据ISO-5660的试验方法,利用锥形卡路里计测定以50kW/m2的放射热强度加热20分钟时的总发热量。
在本说明书中,所谓“不燃性”是指具备以下(1)~(3)的全部条件:(1)以50kW/m2的放射热强度开始加热后20分钟的总发热量为8MJ/m2以下;(2)开始加热后20分钟超过200kW/m2的发热速度不连续超过10秒;(3)开始加热后20分钟不产生有碍于防火的龟裂或孔等变形。
本发明的阻燃性硬质聚氨酯发泡体的用途并无特别限定,通常用以填充建筑物的开口部或间隙。此处“建筑物”包括构成建筑物的任意结构,不仅包括墙壁、天花板、屋脊、地板等建筑物的结构材料,也包括窗(包括推拉窗、平开窗、上下推拉窗等)、拉门、房门(即门)、大门、隔扇、格窗等建筑构件。需要说明的是,“开口部”包括产生于建筑物的结构材料之间的接缝、或产生于一个结构材料中的孔,是指建筑物中所产生的任意的开口部,“间隙”也包括在开口部之中,在结构材料与结构材料之间、结构材料与建筑构件之间、建筑构件与建筑构件之间、结构材料或建筑构件与家具(厨房的水槽等)之间相对的2个部件或部分间所产生的开口部。
本发明的阻燃性硬质聚氨酯发泡体优选为直接对建筑物的开口部或间隙等对象物吹送发泡性聚氨酯树脂组合物,在该对象物中使其发泡而成的发泡体。
另外,阻燃性硬质聚氨酯发泡体不仅是使发泡性聚氨酯树脂组合物直接填充至建筑物的开口部或间隙,而且也可流入模具等成形为适合建筑物的开口部或间隙的尺寸(长度、宽度及厚度),或者从混合容器喷出至其他位置制成聚氨酯发泡体并切割成特定的尺寸(长度、宽度及厚度)后,安装至建筑物的开口部或间隙。
使发泡性聚氨酯树脂组合物发泡固化而获得的阻燃性硬质聚氨酯发泡体由于防水性、气密性及防火性优异,故而能够有效地阻断来自建筑物的开口部或间隙的水、烟或火焰、因燃烧所产生的气体等的侵入。以下,列举实施例对本发明更具体地进行说明,但本发明并不限定于下述实施例。
实施例
制造例1发泡性聚氨酯树脂组合物及阻燃性硬质聚氨酯发泡体的制造
根据表1所示的配比组成,将实施例1~7及比较例1~2的发泡性聚氨酯树脂组合物分为(1)多元醇预混物及(2)芳香族多异氰酸酯的两者而准备。再者,表中的各成分的详细情况如下所述。
(1)多元醇预混物
多元醇
对苯二甲酸聚酯多元醇(川崎化成工业公司制造,产品名:MAXIMOL RLK-087,羟值=200mgKOH/g)
泡沫稳定剂
聚亚烷基二醇类泡沫稳定剂(Dow Corning Toray公司制造,产品名:SH-193)
催化剂
三聚催化剂(Tosoh公司制造,产品名:TOYOCAT(注册商标)-TRX)
三聚催化剂(AIR PRODUCTS公司制造,产品名:DABCO(注册商标)K-15)
三聚催化剂(San-Apro株式会社制造,产品名:U-CAT 18X)
叔胺(烷基化聚亚烷基多胺)(Tosoh公司制造,产品名:TOYOCAT(注册商标)-TT)
叔胺的氨基甲酸酯催化剂(咪唑类化合物)(San-Apro株式会社制造,产品名:U-CAT 202)
叔胺(1,2-二甲基咪唑与乙二醇的混合物)(Tosoh公司制造,产品名:TOYOCAT(注册商标)-DM70)
叔胺(三乙二胺)(Tosoh公司制造,产品名:TEDA-L33)
发泡剂
水
HFC HFC-365mfc(1,1,1,3,3-五氟丁烷,Central硝子公司制造)以及HFC-245fa(1,1,1,3,3-五氟丙烷,日本Solvay公司制造),混合比例HFC-365mfc:HFC-245fa=7:3,以下称为“HFC”)
阻燃剂
磷酸三(β-氯丙基)酯(大八化学公司制造,产品名:TMCPP,称为“TMCPP”)。
红磷(磷化学工业公司制造,产品名:Nova Excel 140)
硼酸锌(早川商事株式会社制造,产品名:FIRebrake ZB)
无机填充材
硅灰石(SiO2CaO)(Kinseimatec公司制造,产品名:SH-1250)
气相二氧化硅(日本Aerosil公司制造,产品名:Aerosil R976S)
(2)芳香族多异氰酸酯
4,4'-二苯基甲烷二异氰酸酯(4,4'-MDI)(日本万华化学株式会社制造,产品名:PM200)
根据下述表1的配比组成,称取(1)多元醇预混物的成分置于1000mL聚丙烯烧杯中,在25℃下手动混合搅拌1分钟。对搅拌后的(1)多元醇预混物的成分的混练物添加(2)芳香族多异氰酸酯,使用手动搅拌器搅拌约10秒而制成发泡性聚氨酯树脂组合物。得到的发泡性聚氨酯树脂组合物随着时间经过而失去流动性,从而获得阻燃性硬质聚氨酯发泡体。根据下述基准对上述发泡体进行评价,并将结果示于表1(以相对于聚氨酯树脂100重量份的重量份表示各成分的比例)。
试验例1IR测定
削去实施例1~7及比较例1~2的阻燃性硬质聚氨酯发泡体的从表层向内5mm~10mm的部位,将经削去后的各样品放入至烘箱中,在温度80℃、湿度85%进行湿热处理。
使用IR测定计(Varian公司制造的FT-IR Microscope 600UMA),通过全反射(ATR)法对湿热处理前及湿热处理1星期之后的强度波峰值进行测定。
如表1及表2所示,实施例1的异氰尿酸酯比在湿热处理前为1.62,湿热处理后为1.61,实施例2的异氰尿酸酯比在湿热处理前为1.60,湿热处理后为1.40,进行一星期的湿热处理后的异氰尿酸酯比的值与湿热处理前的异氰尿酸酯比的值的比例在实施例1及实施例2中分别为99%及89%。
另外,实施例3~7的异氰尿酸酯比、以及进行一星期的湿热处理后的异氰尿酸酯比的值相对于湿热处理前的异氰尿酸酯比的值的比例为如表1所示的结果。
与此相对,比较例1的异氰尿酸酯比在湿热处理前为1.72,湿热处理后为1.44,比较例2的异氰尿酸酯比在湿热处理前为1.71,湿热处理后为1.42,进行一星期的湿热处理后的异氰尿酸酯比的值与湿热处理前的异氰尿酸酯比的值的比例在比较例1以及比较例2中分别为84%和83%。
试验例2耐火性试验
在温度80℃、湿度85%对实施例1~7的阻燃性硬质聚氨酯发泡体进行进行一星期以及两星期的湿热处理后的样品以及在温度80℃、湿度85%对比较例1~2的阻燃性硬质聚氨酯发泡体进行一星期的湿热处理后的样品,从上述样品切取10cm×10cm×5cm的锥形卡路里计试验用样品,依据ISO-5660对以放射热强度50kW/m2加热20分钟时的最大发热速度、总发热量进行测定。
该测定方法是在建筑基准法施行令第108条的2中所规定的公共机关即建筑综合试验所中被规定为与锥形卡路里计法的基准对应的试验法,并且是依据ISO-5660的试验方法。
在加热20分钟过程中锥形卡路里计的总发热量为8MJ/m2以下为合格,将加热20分钟过程中超过8MJ/m2者设为不合格(FAIL),将加热20分钟过程中为8MJ/m2以下者设为合格(PASS)。
作为耐火性试验的综合判定,将通过锥形卡路里计法所获得的试验结果仅进行一星期的湿热处理后合格者设为B,将进行一星期是热处理以及进行两星期湿热处理这两者后都合格者设为A。将进行一星期的湿热处理后不合格者设为C。如表1所示,综合判定中实施例1、3、5及6为A,实施例2、4及7为B,比较例1及2为C。
试验例3水分量的测定
通过以下的方法,对上述各成分中的烷基化聚亚烷基多胺(叔胺)(Tosoh公司制造,产品名:TOYOCAT(注册商标)-TT)、叔胺的氨基甲酸酯催化剂(咪唑类化合物,San-Apro股份有限公司制造,产品名:U-CAT 202)、叔胺(1,2-二甲基咪唑与乙二醇的混合物,Tosoh公司制造,产品名:TOYOCAT(注册商标)-DM70)、叔胺(三乙二胺、Tosoh公司制造,产品名:TEDA-L33)进行水分量的测定。
首先,将1g各催化剂、10g TMCPP及1g水混合后,充分静置。其后,通过卡尔费歇法测定TMCPP层的水分量。
其结果为,TOYOCAT(注册商标)-TT为4.3%,U-CAT 202为4.5%,TOYOCAT(注册商标)-DM70为3.7%,TEDA-L33为3.6%。
以上,对本发明的实施方式及实施例进行了具体说明,但本发明不限定于上述实施方式,可基于本发明的技术思想进行各种变形。
另外,本发明也可采用以下的技术方案。
[1]一种阻燃性硬质聚氨酯发泡体,其含有阻燃剂,其特征在于:在温度80℃、湿度85%的条件下对所述发泡体进行一星期的湿热处理后的最大峰强度比(P1)与进行上述湿热处理前的所述发泡体的最大峰强度比(P2)的比例(P1/P2×100)为85%以上。
(其中,所述P1和P2是指:对从所述发泡体的表层向内5mm~10mm的位置处的红外线吸收光谱进行测定,将1900~2000cm-1的平均强度设为0时,1390~1430cm-1的最大峰强度与1500~1520cm-1的最大峰强度之比)。
[2]根据[1]中所记载的阻燃性硬质聚氨酯发泡体,其含有选自红磷、磷酸酯、含磷酸盐的阻燃剂、含溴的阻燃剂、含硼的阻燃剂、含锑的阻燃剂及金属氢氧化物中的一种以上作为阻燃剂。
[3]根据[1]或[2]中所记载的阻燃性硬质聚氨酯发泡体,其含有三聚催化剂以及三聚催化剂以外的催化剂,相对于聚氨酯树脂100重量份,含有0.6~10重量份的三聚催化剂,相对于聚氨酯树脂100重量份,以3重量份以下的比例含有三聚催化剂以外的催化剂。
[4]根据[1]至[3]中任一项中所记载的阻燃性硬质聚氨酯发泡体,其中,相对于聚氨酯树脂100重量份,作为三聚催化剂以外的催化剂的叔胺的含量为3重量份以下。
[5]一种发泡性聚氨酯树脂组合物,其含有多元醇、多异氰酸酯、泡沫稳定剂、催化剂、发泡剂及阻燃剂,该组合物还含有三聚催化剂以及三聚催化剂以外的催化剂作为催化剂,相对于聚氨酯树脂100重量份,以0.6~10重量份的比例含有上述三聚催化剂,相对于聚氨酯树脂100重量份,以3重量份以下的比例含有作为上述三聚催化剂以外的催化剂的叔胺。
[6]根据[5]中所记载的发泡性聚氨酯树脂组合物,其含有选自红磷、磷酸酯、含磷酸盐的阻燃剂、含溴的阻燃剂、含硼的阻燃剂、含锑的阻燃剂及金属氢氧化物中的一种以上作为阻燃剂。
Claims (5)
1.一种阻燃性硬质聚氨酯发泡体,其含有阻燃剂,其中,
将所述发泡体在温度80℃、湿度85%的条件下进行一星期的湿热处理后的最大峰强度比(P1)与所述湿热处理前所述发泡体的最大峰强度比(P2)的比例(P1/P2×100)为85%以上,
其中,所述P1和P2是指:对从所述发泡体的表层向内5mm~10mm的位置处的红外线吸收光谱进行测定,将1900~2000cm-1的平均强度设为0时,1390~1430cm-1的最大峰强度与1500~1520cm-1的最大峰强度之比。
2.权利要求1所述的阻燃性硬质聚氨酯发泡体,其含有选自红磷、磷酸酯、含磷酸盐的阻燃剂、含溴的阻燃剂、含硼的阻燃剂、含锑的阻燃剂及金属氢氧化物中的一种以上作为阻燃剂。
3.权利要求1或2所述的阻燃性硬质聚氨酯发泡体,其含有三聚催化剂以及三聚催化剂以外的催化剂,其中,
相对于聚氨酯树脂100重量份,含有0.6~10重量份的三聚催化剂,
相对于聚氨酯树脂100重量份,以3重量份以下的比例含有三聚催化剂以外的催化剂。
4.权利要求1~3中任一项所述的阻燃性硬质聚氨酯发泡体,其中,相对于聚氨酯树脂100重量份,作为三聚催化剂以外的催化剂的叔胺的含量为3重量份以下。
5.一种发泡性聚氨酯树脂组合物,其含有多元醇、多异氰酸酯、泡沫稳定剂、催化剂、发泡剂及阻燃剂,
并且含有三聚催化剂以及三聚催化剂以外的催化剂作为催化剂,其中,
相对于聚氨酯树脂100重量份,以0.6~10重量份的比例含有上述三聚催化剂,
相对于聚氨酯树脂100重量份,以3重量份以下的比例含有作为上述三聚催化剂以外的催化剂的叔胺。
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JP2021038409A (ja) | 2021-03-11 |
KR20180063111A (ko) | 2018-06-11 |
EP3357947A1 (en) | 2018-08-08 |
JP6813358B2 (ja) | 2021-01-13 |
JPWO2017057670A1 (ja) | 2018-07-19 |
TW201730228A (zh) | 2017-09-01 |
US11236192B2 (en) | 2022-02-01 |
US20180265620A1 (en) | 2018-09-20 |
EP3357947A4 (en) | 2019-04-17 |
WO2017057670A1 (ja) | 2017-04-06 |
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