CN1179440A - 储存稳定、含阻燃剂的多元醇成分 - Google Patents
储存稳定、含阻燃剂的多元醇成分 Download PDFInfo
- Publication number
- CN1179440A CN1179440A CN97120520A CN97120520A CN1179440A CN 1179440 A CN1179440 A CN 1179440A CN 97120520 A CN97120520 A CN 97120520A CN 97120520 A CN97120520 A CN 97120520A CN 1179440 A CN1179440 A CN 1179440A
- Authority
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- China
- Prior art keywords
- acid
- polyhydroxy reactant
- weight
- alkyl
- mixture
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 239000003063 flame retardant Substances 0.000 title claims abstract description 29
- 229920005862 polyol Polymers 0.000 title abstract description 9
- 150000003077 polyols Chemical class 0.000 title abstract description 8
- 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 abstract description 4
- 239000005056 polyisocyanate Substances 0.000 claims abstract description 28
- 229920001228 polyisocyanate Polymers 0.000 claims abstract description 27
- 150000002460 imidazoles Chemical class 0.000 claims abstract description 15
- 239000000654 additive Substances 0.000 claims abstract description 11
- 239000004970 Chain extender Substances 0.000 claims abstract description 9
- 125000002853 C1-C4 hydroxyalkyl group Chemical group 0.000 claims abstract description 3
- 239000000376 reactant Substances 0.000 claims description 47
- -1 hydrogen atoms compound Chemical class 0.000 claims description 44
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims description 38
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 32
- 239000003795 chemical substances by application Substances 0.000 claims description 27
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 claims description 19
- 235000019253 formic acid Nutrition 0.000 claims description 19
- 239000000463 material Substances 0.000 claims description 16
- 229910052799 carbon Inorganic materials 0.000 claims description 15
- 230000004048 modification Effects 0.000 claims description 14
- 238000012986 modification Methods 0.000 claims description 14
- 150000002148 esters Chemical class 0.000 claims description 11
- 230000000996 additive effect Effects 0.000 claims description 10
- 229910052739 hydrogen Inorganic materials 0.000 claims description 6
- MCTWTZJPVLRJOU-UHFFFAOYSA-N 1-methyl-1H-imidazole Chemical compound CN1C=CN=C1 MCTWTZJPVLRJOU-UHFFFAOYSA-N 0.000 claims description 5
- GIWQSPITLQVMSG-UHFFFAOYSA-N 1,2-dimethylimidazole Chemical compound CC1=NC=CN1C GIWQSPITLQVMSG-UHFFFAOYSA-N 0.000 claims description 3
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- 239000011496 polyurethane foam Substances 0.000 claims description 3
- 239000006260 foam Substances 0.000 abstract description 32
- 239000004814 polyurethane Substances 0.000 abstract description 30
- 125000004435 hydrogen atom Chemical group [H]* 0.000 abstract description 9
- 239000003054 catalyst Substances 0.000 abstract description 7
- 239000004604 Blowing Agent Substances 0.000 abstract description 5
- 239000012774 insulation material Substances 0.000 abstract description 4
- 239000003381 stabilizer Substances 0.000 abstract description 4
- 239000012948 isocyanate Substances 0.000 abstract description 3
- 150000002513 isocyanates Chemical class 0.000 abstract description 3
- 125000004178 (C1-C4) alkyl group Chemical group 0.000 abstract 2
- 239000004971 Cross linker Substances 0.000 abstract 1
- 150000002605 large molecules Chemical class 0.000 abstract 1
- 239000000203 mixture Substances 0.000 description 50
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 46
- 229920002635 polyurethane Polymers 0.000 description 29
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 description 21
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 19
- 239000002253 acid Substances 0.000 description 17
- 239000004721 Polyphenylene oxide Substances 0.000 description 16
- 239000002585 base Substances 0.000 description 16
- 229920000570 polyether Polymers 0.000 description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 16
- XLJMAIOERFSOGZ-UHFFFAOYSA-N anhydrous cyanic acid Natural products OC#N XLJMAIOERFSOGZ-UHFFFAOYSA-N 0.000 description 13
- 150000001875 compounds Chemical class 0.000 description 13
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 12
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 12
- 150000001721 carbon Chemical group 0.000 description 10
- UPMLOUAZCHDJJD-UHFFFAOYSA-N 4,4'-Diphenylmethane Diisocyanate Chemical compound C1=CC(N=C=O)=CC=C1CC1=CC=C(N=C=O)C=C1 UPMLOUAZCHDJJD-UHFFFAOYSA-N 0.000 description 9
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 9
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 9
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 9
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- 229920005906 polyester polyol Polymers 0.000 description 9
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- 238000003860 storage Methods 0.000 description 8
- 125000001931 aliphatic group Chemical group 0.000 description 7
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- XSTXAVWGXDQKEL-UHFFFAOYSA-N Trichloroethylene Chemical compound ClC=C(Cl)Cl XSTXAVWGXDQKEL-UHFFFAOYSA-N 0.000 description 6
- 239000004202 carbamide Substances 0.000 description 6
- 238000006243 chemical reaction Methods 0.000 description 6
- 239000011541 reaction mixture Substances 0.000 description 6
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 description 5
- JOYRKODLDBILNP-UHFFFAOYSA-N Ethyl urethane Chemical compound CCOC(N)=O JOYRKODLDBILNP-UHFFFAOYSA-N 0.000 description 5
- OFOBLEOULBTSOW-UHFFFAOYSA-N Malonic acid Chemical compound OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 description 5
- GOOHAUXETOMSMM-UHFFFAOYSA-N Propylene oxide Chemical compound CC1CO1 GOOHAUXETOMSMM-UHFFFAOYSA-N 0.000 description 5
- XXMIOPMDWAUFGU-UHFFFAOYSA-N hexane-1,6-diol Chemical compound OCCCCCCO XXMIOPMDWAUFGU-UHFFFAOYSA-N 0.000 description 5
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- 238000004519 manufacturing process Methods 0.000 description 5
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 5
- 238000002360 preparation method Methods 0.000 description 5
- 230000006641 stabilisation Effects 0.000 description 5
- 238000011105 stabilization Methods 0.000 description 5
- 150000003512 tertiary amines Chemical class 0.000 description 5
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 5
- UXFQFBNBSPQBJW-UHFFFAOYSA-N 2-amino-2-methylpropane-1,3-diol Chemical compound OCC(N)(C)CO UXFQFBNBSPQBJW-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
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 4
- 239000004215 Carbon black (E152) Substances 0.000 description 4
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 4
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical group [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 4
- OFBQJSOFQDEBGM-UHFFFAOYSA-N Pentane Chemical compound CCCCC OFBQJSOFQDEBGM-UHFFFAOYSA-N 0.000 description 4
- 229930182556 Polyacetal Natural products 0.000 description 4
- ATUOYWHBWRKTHZ-UHFFFAOYSA-N Propane Chemical compound CCC ATUOYWHBWRKTHZ-UHFFFAOYSA-N 0.000 description 4
- WQDUMFSSJAZKTM-UHFFFAOYSA-N Sodium methoxide Chemical compound [Na+].[O-]C WQDUMFSSJAZKTM-UHFFFAOYSA-N 0.000 description 4
- YSMRWXYRXBRSND-UHFFFAOYSA-N TOTP Chemical compound CC1=CC=CC=C1OP(=O)(OC=1C(=CC=CC=1)C)OC1=CC=CC=C1C YSMRWXYRXBRSND-UHFFFAOYSA-N 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
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 4
- 229910052783 alkali metal Inorganic materials 0.000 description 4
- WERYXYBDKMZEQL-UHFFFAOYSA-N butane-1,4-diol Chemical compound OCCCCO WERYXYBDKMZEQL-UHFFFAOYSA-N 0.000 description 4
- 125000005442 diisocyanate group Chemical group 0.000 description 4
- SZXQTJUDPRGNJN-UHFFFAOYSA-N dipropylene glycol Chemical compound OCCCOCCCO SZXQTJUDPRGNJN-UHFFFAOYSA-N 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
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- XNGIFLGASWRNHJ-UHFFFAOYSA-N phthalic acid Chemical compound OC(=O)C1=CC=CC=C1C(O)=O XNGIFLGASWRNHJ-UHFFFAOYSA-N 0.000 description 4
- 229920000768 polyamine Polymers 0.000 description 4
- 238000006068 polycondensation reaction Methods 0.000 description 4
- 238000006116 polymerization reaction Methods 0.000 description 4
- 229920006324 polyoxymethylene Polymers 0.000 description 4
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 description 3
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- 239000005995 Aluminium silicate Substances 0.000 description 3
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- DJOWTWWHMWQATC-KYHIUUMWSA-N Karpoxanthin Natural products CC(=C/C=C/C=C(C)/C=C/C=C(C)/C=C/C1(O)C(C)(C)CC(O)CC1(C)O)C=CC=C(/C)C=CC2=C(C)CC(O)CC2(C)C DJOWTWWHMWQATC-KYHIUUMWSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- SVYKKECYCPFKGB-UHFFFAOYSA-N N,N-dimethylcyclohexylamine Chemical compound CN(C)C1CCCCC1 SVYKKECYCPFKGB-UHFFFAOYSA-N 0.000 description 3
- SJRJJKPEHAURKC-UHFFFAOYSA-N N-Methylmorpholine Chemical compound CN1CCOCC1 SJRJJKPEHAURKC-UHFFFAOYSA-N 0.000 description 3
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Abstract
一种储存稳定、含阻燃剂的多元醇成分,它包括至少一种多元醇,如果需要,还有分子量较高且含至少二个活性氢原子的化合物和,如果需要,低分子量的链增量剂和/或交联剂及发泡剂,催化剂,稳定剂和,如果需要,其它辅料和/或添加剂,所用的稳定剂是下列通式的咪唑和/或甲酸,式中R1=C1-C4-烷基,C1-C4-羟烷基或二甲氨-C1-C4-烷基,和R2,R3,R4=H或C1-C4-烷基。通过将该多元醇成分与有机和/或改性有机聚异氰酸酯反应,可制备异氰酸酯基刚性PUR泡沫体并可用作建筑构件中的绝热材料。
Description
本发明涉及储存稳定、含阻燃剂的多元醇成分,它用于阻燃、刚性、基于异氰酸酯的聚氨基甲酸乙酯(PUR)泡沫体的生产。这些刚性PUR泡沫体优选地用在建筑构件中作为绝热材料。
这种基于异氰酸酯的刚性PUR泡沫体包括作为特殊结构部分的氨基甲酸乙酯和/或异氰脲酸酯和/或缩二脲和/或脲基甲酸酯和/或脲二酮和/或脲和/或碳化二亚胺基团。实际上,已经发现制备多元醇成分是有好处的。它们是包括基于异氰酸酯的刚性PUR泡沫体生产所必须的配料成分的液体组合物,例知,多元醇,阻燃性,和水,如果需要还有辅料和添加剂,如催化剂,缓凝剂,物理发泡剂,泡沫体稳定剂,塑化剂,乳化剂,染料,填料和抗沉淀剂。
例如在塑料手册,卷VIII,“聚氨基甲酸乙酯”第一版1996,由R.Viewed和A.Hchtlen博士编写以及第二版1983,和第3版1993,由G.oertel博士编写(carl Hanser出版社,慕尼黑)中给出了刚性PUR泡沫体生产和所用原料的综述。
用另一种发泡剂(即发泡剂)取代CFC,通过异氰酸酯一水反应产生的CO2被越来越多地用作单一发泡剂或与含氢CFC,含氢的碳氟化合物或烃一起用作辅助发泡剂。其涉及到多元醇成分中较高的含水量。特别是在同时存在阻燃剂的情况下,这将在生产刚性泡沫体之前的储存期间产生一些问题。作为水解过程的结果,多元醇成分中酸的含量稳定增加。这将导致与相关的异氰酸酯成分进行反应的时间越来越长,从而产生较差的加工性并有损最终的刚性PUR泡沫体的性能。其不得不进一步加入催化剂来调整多元醇成分,或大多数不利的情况下,不得不将之废弃。这导致不好的经济效益,并在实际中不可能真正达到人们所希望延长了的数星期或数月的储存时间。
因此寻找储存稳定的多元醇成分是一个重要的工业任务。
文献BE843172,DE-A-3607964,EP-A-401787,EP-A-410467,EP-A-451826,JP1256511,JP2047125,JP3033120,JP3131618,JP4055419,JP4161417,JP4202215,JP4214712,JP5209034,JP58213016,JP60084319,JP61031413,JP61031414,JP42998519,JP5070544,US-A-4165412,US-A-431753,US-A-4481309,US-A-52409+64,WO9315121和WO9316122描述了利用N-取代的咪唑作为生产PUR泡沫体的催化剂。
JP3064312和EP-A-560154描述了将甲酸作为发泡剂的应用。根据JP5031989,所用物质由包括Freon22和甲酸的发泡剂混合物构成,在储存期间,甲酸产生稳定的PH值和胶凝时间。EP322801和JP1104611描述了通过调整甲酸的摩尔量(以催化剂为基)来对胺催化剂进行改性。
本发明的一个目的是发现用于含阻燃剂的多元醇成分的合适配方,该多元醇成分具有满意的储存稳定性并使刚性PUR泡沫体具有良好的力学和热性能。
我们发现通过将咪唑和/或甲酸用作稳定剂可达到该目的。
因此,本发明提供了储存稳定,含阻燃剂的多元醇成分,它包括至少一种多元醇,如果需要还有分子量较高且含至少二个活性氢原子的其它化合物和,如果需要,还有低分子量的链增量剂和/或交联剂和发泡剂,催化剂,稳定剂和,如果需要还有辅料和/或添加剂,其中稳定剂是以下通式的咪唑,和/或甲酸。
式中R1=C1-C4烷基,C1-C4羟烷基,或二甲胺基-C1-C4烷基,R2,R3,R4=H或C1-C4烷基。
本发明进一步提供了基于异氰酸酯的刚性PUR泡沫体,其可通过该多元醇与有机和/或改性有机聚异氰酸酯反应来生产,本发明还提供了将该PUR泡沫体在建筑构件中作为绝热材料的应用。
本发明多元醇成分当含有数量较大的阻燃剂水和阻燃剂时也具有良好的储存稳定性。另一优点是稳定剂并不对阻燃剂的作用产生不良影响,并且稳定剂可以较小的数量使用。
优选使用的咪唑是1-乙基咪唑,1-丙基咪唑,1-丁基咪唑,1,3-二甲基咪唑,1,5-二甲基咪唑,1-乙基-2-甲基咪唑,1-甲基-2-乙基咪唑,1-甲基-2-丙基咪唑,1-正-丁基-2-甲基咪唑,1-异丁基-2-甲基咪唑,1-(3-二甲胺基丙基)咪唑,,1,1’-(氧代二亚乙基)二(咪唑),1,1’-(氧代二亚乙基)二(乙-甲基咪唑),特别优选的为1-甲基咪唑和1,2-二甲基咪唑。
咪唑可单独一种使用或与另一种混合使用。
甲酸同样也适合用作本发明的稳定剂。甲酸可单独一种使用或与上述咪唑混合使用。
特别有利的技术方案是甲酸与1-甲基咪唑或1,2-二甲基咪唑混合使用,因此这些混合物是优选使用的。
作为稳定剂的甲酸通常用量为0.01-0.5%,优选为0.05-0.2%(重量,以多元醇成分为基)。
作为稳定剂的咪唑通常用量为0.1-8%(重量),优选为0.5-4%(重量,以多元醇成分为基)。
如果将咪唑和甲酸二者同时用作稳定剂,所用总量为0.1-8.5%(重量,以多元醇成分为基)。
令人吃惊和无论如何无法预见的是迄今已知作为发泡剂或催化剂改性剂的甲酸和已知作为聚氨基甲酸乙酯催化剂的取代的咪唑在含阻燃剂的多元醇成分中具有稳定作用并因此首次使得解决多元醇成分以前不能完全令人满意的储存稳定性问题变为可能。特别令人吃惊和无法预见的是在许多种叔胺中只有取代的咪唑具有该稳定作用;由于叔胺通常趋向于增加储存稳定性问题,这就更加令人吃惊。在甲酸稳定作用方面,需要强调的是甚至在其含量如此之低以至于观察不到真正的加气作用的情况下,其稳定作用仍能发生。
由此开发出了一种制备储存稳定,含阻燃剂的多元醇成分的经济的方法,该多元醇成分易于处理从而形成适合作为建筑构件中绝热材料的刚性PUR泡沫体。
储存稳定、含阻燃剂的多元醇成分包括至少一种多元醇,如果需要还含有分子量较高且含至少二个活性氢原子的其它化合物和,如果需要,低分子量的链增量剂和/或交联剂及发泡剂,催化剂,稳定剂和,如果需要,还有辅料和/或添加剂。
除了特定的稳定剂外,可以用本身已知成分来制备本发明储存稳定、含阻燃剂的多元醇成分,关于该成分将在下面作详细描述。
当使用多元醇以及其它分子量较高且含至少二个活性氢原子的化合物时,有利地应使用那些官能度为2-8,优选为2-6和分子量300-8000,优选为300-3000的物质。例如,现已发现实用的化合物是聚醚多胺和/或优选地选自于聚醚多元醇,聚酯多元醇,聚硫醚多元醇,聚酯酰胺,含羟基的聚缩醛和含羟基的脂族聚碳酸脂,或至少两种上述多元醇的混合物。使用聚酯多元醇和/或聚醚多元醇是优选的。多羟基化合物的羟基数一般为150-850kg KOH/g,优选为200-600kg KOH/g。
例如,可由具有2-12个碳原子的有机二元羧酸,优选为具有4-6个碳原子的脂族二元羧酸,和具有2-12个碳原子,优选为2-6个碳原子的多元醇,优选为二元醇来制备合适的聚酯多元醇。合适的二元羧酸的实例是琥珀酸,戊二酸,己二酸,辛二酸,壬二酸,癸二酸,癸烷二羧酸,马来酸,富马酸,苯二甲酸,间苯二甲酸和对苯二甲酸。此外二元羧酸可以单独一种也可以与另一种混合使用。除了游离二羧酸以外,也可以用相应的二元羧酸衍生物,如具有1-4个碳原子的醇的二羧酸酯,和二元羧酸酐。优选地以例如重量比为20-35∶35-50∶20-32使用琥珀酸,戊二酸和己二酸的二元羧酸混合物,特别是己二酸是优选的。二元醇或多元醇,特别是二元醇的实例是乙二醇,二乙二醇,1,2-或1,3-丙二醇,二丙二醇,1,4-丁二醇,1,5-戊二醇,1,6-己二醇,1,10-癸二醇,甘油醇和三甲醇丙烷。使用乙二醇,二乙二醇,1,4-丁二醇,1,5-戊二醇,1,6-己二醇或至少二种上述二元醇混合物是优选的,特别是1,4-丁二醇,1,5-戊二醇,和1,6-己二醇的混合物。使用从内酯,如ε-己内酯,或羟羧酸,如ω-羟己酸衍生的聚酯多元醇也是可以的。
为了制备聚酯多元醇,可在缺少催化剂或优选地存在酯化催化剂的条件下将有机物,如芳族,优选为脂族多元羧酸和/或衍生物和多元醇缩聚至所需的酸量,较好地为低于10,优选地低于2,反应有利地在惰性气体,如氮,一氧化碳,氦和氩等气氛中进行,反应在150-250℃,优选为180-220℃熔体中进行,并处于大气压或减压下。酯化混合物在上述温度时缩聚成80-30,优选为40-30的酸量,其处于大气压下并随后处于少于500毫泊,优选地少于50-150毫泊的减压下。例如,合适的酯化催化剂是铁、镉、钴、铅、锌、锑、钛和锡催化剂,其为金属,金属氧化物或金属盐的形式。然而,该缩聚反应也可在液相中在稀释剂和/或共沸剂,如苯,甲苯,二甲苯,或氯苯存在下进行,以共沸蒸馏掉缩合的水。
为了制备聚酯多元醇,有机多元羧酸和/或衍生物和多元醇有利地以1∶1-1∶8,优选为1∶1.05-1.2的摩尔比进行缩聚。
所获聚酯多元醇优选具有2-4,特别是2-3的宫能度以及480-3000,优选600-2000,特别是600-1500的分子量。
然而,特别优选地使用的多元醇是那些用已知方法例如,由一种或多种在烯基上具有2-4个碳原子的氧化烯制备的聚醚多元醇阴离子聚合或阳离子聚合。所说的阴离子聚合使用碱金属氢氧化物,如氢氧化钠或氢氧化钾或碱金属醇盐,如甲醇钠或乙醇钾或异丙醇钾作为催化剂并加入至少一种含2-8,优选为2-6个活性氢原子(键合形式)的引发剂分子,所说的阳离子聚合使用路易斯酸,如五氯化锑,氟化硼***配合物等,或漂白土作为催化剂。
例如,合适的氧化烯是四氢呋喃,1,3-氧化丙烯,1,2-或2,3-氧化丁烯,氧化苯乙烯,以及优选的氧化乙烯和1,2-氧化丙烯。氧化烯可单独一种交替或连续地使用用或作为混合物使用。合适的引发剂分子的实例为水,有机二元羧酸,如琥珀酸,己二酸,苯二甲酸,和对苯二甲酸,脂族和芳香族未烷基化或N-单烷基化,N,N-或N,N’-二烷基化的在烷基上具有1-4个碳原子的二胺,例如,未烷基化的,单烷基化的或二烷基化的乙二胺,二乙三胺,三乙四胺,1,3-丙二胺,1,3-或1,4-丁二胺,1,2-,1,3-,1,4-,1,5-和1,6-六甲二胺。苯胺二胺,2,3-,2,4-和2,6-甲代苯二胺和4,4’-,2,4’-和2,2’二胺二苯甲烷。
其它合适的引发剂分子是链烷醇胺,如乙醇胺,N-甲基乙醇胺,如N-乙基乙醇胺,二链烷醇胺,如二乙醇胺,N-甲基二乙醇胺,二链烷醇胺,如二乙醇胺,N-甲基二乙醇胺,和N-乙基二乙醇胺,和三链烷醇胺,如三乙醇胺,和氨。使用多元醇,特别是二元和/或三元醇是优选的,如乙二醇,1,2-和1,3-丙二醇,二乙二醇,二丙二醇,1,4-丁二醇,1,6-己二醇,丙三醇,三甲醇丙烷,季戊四醇,山梨醇,蔗糖。
聚醚多元醇,优选聚氧化丙烯和聚氧化丙烯-聚氧化乙烯多元醇,优选地具有2-8,特别是2-6个宫能度,并具有300-3000,优选地300-2000,特别是400-2000的分子量,合适的聚氧化四甲二醇具有不大于约3500的分子量。
其它合适的聚醚多元醇是聚合物改性的聚醚多元醇,优选地为接枝聚醚多元醇,特别是那些以苯乙烯和/或丙烯腈为基的多元醇,它们是通过丙烯腈,苯乙烯或优选的重量比例如为90∶10-10∶90,优选为70∶30-30∶70的苯乙烯和丙烯腈的混合物当场聚合来制备,在上述聚醚多元醇中有利地使用在德国专利1111394,1222669(US3304273,3383351,3523093),1152536(GB1040452)和1152537(GB987618)中给出的相似的方法,以及包括数量通常为1-50%(重量),优选为2-25%(重量)的分散相,如聚脲,聚酰肼,含键合的叔胺基的聚氨基甲酸乙酯和/或并且例如在EP-B-011752(US4304708),US-A-4374209和DE-A-3231497中所描述的的聚醚多元醇分散液。
与聚酯多元醇一样,聚醚多元醇可单独一种使用或以混合物形式使用。还有,它们可与接枝的聚醚多元醇或聚酯多元醇或与含羟基的聚酯酰胺,聚缩醛,聚碳酸酯和/或聚醚多胺混合使用。例如,合适的含羟基的聚缩醛是可由醇,如二乙二醇,三乙二醇,4,4’-二羟基乙氧基(二苯二甲基甲烷),己二醇和甲醛制得的化合物。合适的聚缩醛也可通过环缩醛聚合来制备。
合适的含羟基的聚碳酸酯是那些本身已知可通过例如二元醇,如1,3-丙二醇,1,4-丁二醇和/或1,6-己二醇,二乙二醇,三乙二醇,或四乙二醇与二芳基碳酸酯,如碳酸二苯酯,或碳酰氯反应而制得的化合物。
例如,聚酯酰胺包括由多元、饱和、和/或不饱和的羧酸或其酸酐和多官能的饱和和/或不饱和氨基醇或多官能醇和氨基醇的混合物和/或多胺获得的主要为线型的缩合物。
用已知的方法可由上述聚醚多元醇制备合适的聚醚多胺。可列举出的实例是聚氧化烯多元醇的氰烷化和随后形成的腈的氢化(US3267050)或在氢和催化剂存在下用胺或氨对聚氧化烯多元醇进行的部分或全部胺化(DE1215373)。
根据由其生产的刚性PUR泡沫体所期望的性能,储存稳定,含阻燃剂的多元醇成分可在没有使用或使用了链增量剂和/或交联剂的条件下制备。加入链增量剂,交联剂或其混合物(如果需要)证明有利于改进力学性能,如硬度。所用的链增量剂和/或交联剂是二元醇,和/或三元醇,它们具有少于400,优选为60-300的分子量。合适的链增量剂/交联剂的实例是具有2-14,优选为4-10个碳原子的脂族,环脂族和/或芳脂族二元醇,例如己二醇,1,3-丙二醇,1,10-癸二醇,邻,间,对一二羟基环己烷,二乙二醇,二丙二醇,和优选的1,4-丁二醇,1,6-己二醇和二(乙-羟己基)氢醌,三醇,如1,2,4-,1,3,5-三羟基环己烷,丙三醇和三甲醇丙烷,及低分子量含羟基的氧化乙烯或1,2氧化丙烯基聚氧化烯和作为引发剂分子的上述二元醇和/或三元醇。
如果将链增量剂,交联剂或其混合物用于制备刚性聚氨基甲酸乙酯泡沫体,其有利的用量为0-20%,优选为2-8%(重量,以所用的多元醇和其它分子量较高含至少二个活性氢原子的化合物的重量为基)。
如上所述,由于用另一种发泡剂代替CFC,结果,水越来越多地被用作单一或辅助发泡剂,利用由异氰酸酯-水反应所产生的CO2的加气作用。还有可另外使用物理发泡剂。
合适的物理发泡剂是对有机改性或未改性的聚异氰酸酯呈惰性的液体,所说的聚异氰酸酯用在对本发明多元醇成分进行的进一步处理中从而形成刚性PUR泡沫体,该液体在大气压下具有低于100℃,优选低于50℃,特别为-50℃-30℃的沸点,以便在放热加聚反应作用下蒸发。该优选使用的液体的实例是烷烃,如庚烷,己烷,正和异戊烷,优选的为正一和异一戊烷;正和异丁烷和丙烷的工业级混合物,环烷烃,如环戊烷和/或环己烷,醚,如呋喃,二甲基醚,和二乙基醚,酮,如丙酮和甲基乙酮,烷基羧酸酯,如甲酸甲酯,酸二甲酯和乙酸乙酯和卤化烃,如二氯甲烷,二氯一氟甲烷,二氟甲烷,三氟甲烷,二氟乙烷,四氟乙烷,一氯二氟乙烷,1,1-二氯-2,2,2三氟乙烷,2,2-二氯-2-氟乙烷和七氟丙烷。这些低沸点液体与另一种液体和/或其它取代或未取代的烃的混合物也可使用。其合适的例子是有机羧酸,如甲酸,乙酸,草酸,蓖麻油酸和含羧基的化合物。
使用水,一氯二氯甲烷,一氯二氟乙烷,二氯一氟乙烷,戊烷混合物,环己烷和至少二种发泡剂的混合物,例如水和环己烷的混合物,一氯二氟甲烷和1-氯-2,2-二氟己烷和水(如果需要)的混合物。
当用水作发泡剂时,其优选的加入量为0.5-5%(重量)。水的加入可与所述其它发泡剂的加入一块进行。
所用的发泡剂或发泡剂混合物的总量为1-25%(重量),优选为5-15%(重量)。
所说的数量在各种情况下均是以多元醇成分的总重量为基准。
所用的催化剂是通常用于生产刚性PUR泡沫体的化合物,其大大加速含活性氢原子,特别是羟基的多元醇成分的化合物与有机改性,或未改性聚异氰酸酯的反应。
所用物质有利地为碱性PUR催化剂例如叔胺,如三乙胺,三丁胺,二甲基苄胺,二环己基甲胺,二甲基环己胺,二(N,N-二甲基氨乙基)醚-二(二甲基氨丙基)脲,N-甲基吗啉或N-乙基吗啉,N-环己基吗啉,N,N,N’,N’-四甲基乙二胺,N,N,N’,N’-四甲基丁二胺,N,N,N’,N’-四甲基己烷-1,6-二胺,五甲基二亚乙基三胺,二甲基哌嗪,N-甲基氨乙基哌淀,1-偶氮二环[2,2,0]辛烷,1,4-二偶氮二环[2,2,2]辛烷(Dabco)和链烷醇胺化合物,如三乙醇胺,三异丙醇胺,N-甲基二乙醇胺,和N-乙基二乙醇胺,二甲基氨基乙醇,2-(N,N-二甲基氨基乙氧基,乙醇,N,N’,N”-三(二烷基氨烷基)六氢三吖嗪,如N,N’,N”-三(二甲基氨丙基)-5-六氢三吖嗪,和三乙二胺。然而,金属盐,如氯化铁(II),氯铁锌,辛酸铅,辛酸铋,和优选的锡盐,如二辛酸锡,二乙基己酸锡和二月桂酸二丁基锡,特别是叔胺和有机锡盐的混合物也是合适的。
其它合适的催化剂是脒,如2,3-二甲基-3,4,5,6-四氢嘧啶,氢氧化四烷基铵,如氢氧化四甲基铵,碱金属氢氧化物,如氢氧化钠,和碱金属醇盐,如甲醇钠和异丙醇钾,及具有10-20个碳原子、侧向可含有OH基的长链脂肪酸的碱金属盐。使用0.001-5%,特别是0.05-2%(重量)(以多元醇成分的总重量计)的催化剂或催化剂混合物是优选的。
本发明多元醇成分含有阻燃剂。合适的阻燃剂是那些通常在刚性PUR泡沫体中用于该目的的化合物。
可列举的实例是磷酸联苯·甲苯酯,磷酸三甲苯酯,磷酸三乙酯或三丁酯,磷酸三(乙-氯己基)酯,磷酸三(乙-氯丙基)酯,磷酸三(1,3-二氯丙基)酯,二磷酸四(2-氯己基)亚乙酯,甲烷磷酸二乙酯,二乙醇胺甲基磷酸二乙酯。
含溴的阻燃剂也是合适的,如三溴新戊醇,三溴新戊醇的反应产物,二溴新戊二醇及其反应产物,二溴丁烯二醇及其反应产物,2,3-二溴丙醇及其反应产物,四溴苯二甲酸酐及其反应产物,三溴苯酚及其反应产物,四溴双酚A及其反应产物,含溴磷酸酯,和溴化烃。
除了上述化合物外,还可以使用无机或有机阻燃剂使聚异氰酸酯加聚产物具有阻燃性,例如红磷,水合氧化铝,三氧化锑,氧化砷,聚磷酸铵,和硫酸钙,膨胀石墨或三聚氰酸衍生物,如密胺和膨胀石墨和/或芳族或脂族聚酯。
优选的阻燃剂在室温下是液体并具有至少20%(重量)的氯含量或至少30%的溴含量或至少5%(重量)的磷含量。
已发现通常使用10-80%(重量),优选30-60%(重量)的上述阻燃剂(以多元醇成分的总重量为基)是有利的。
如果需要,可进一步将辅料和/或添加剂引入到本发明储存稳定,含阻燃剂的多元醇成分中。可列举的实例是表面活性剂,泡沫体稳定剂,气泡控制剂,填料,染料,颜料,抗水解剂,制霉剂和抑菌剂物质。
例如,合适的表面活性剂物质是有助于原料均化及也可适用于塑料气泡结构控制的化合物,可列举的实例是乳化剂,如蓖麻油硫酸盐或脂肪酸的钠盐,及脂肪酸胺盐,例如,油酸二乙胺,硬脂酸二乙醇胺,蓖麻醇酸二乙醇胺,磺酸盐,如十二烷基苯一或二萘甲烷二磺酸和蓖麻油酸的碱金属盐或铵盐;泡沫体稳定剂,如硅氧烷一氧化烯共聚物和其它有机聚硅氧烷,乙氧化烷基苯酚,乙氧化脂肪醇,石蜡油,蓖麻油,或蓖麻油酸酯,土耳其红油,和花生油;气泡控制剂,如石蜡,脂肪醇,和二甲基聚硅氧烷。还有,上述具有聚氧化烯和氟烷烃基作为侧边基团的低聚丙烯酸酯也适用于改进乳化作用,气泡结构和/或稳定泡沫体。表面活性剂通常用量为0.01-5%(重量,以多元醇成分总重量为基)。
为了达到本发明目的,填料,特别是增强填料是本身已知的常规有机填料和无机填料,增强剂,增重剂,用于改善油漆、涂料组合物耐磨性的助剂。特定的实例为无机填料,如硅质矿物,例如层状硅酸盐,如叶蛇纹石,蛇纹石。角闪石,闪石,纤蛇纹石和滑石,金属氧化物,如高岭土,氧化铝,氧化钛和氧化铁,金属盐,如白垩,重晶石和无机颜料,如硫化镉和硫化锌,以及玻璃等。优选地使用高岭土(瓷土),硅酸铝,以及天然和合成纤维矿物,如硅灰石,金属和,特别是各种长度(可测的)的玻璃纤维。合适的有机填料的实例是碳,蜜胺,松香,环戊二烯基树脂和接枝聚合物以及纤维素纤维,聚酰胺,聚丙烯腈,芳香族和/或脂族二元羧酸酯基聚氨基甲酸乙酯和聚酯纤维,特别是碳纤维。
无机和有机纤维可单独一种、或作为混合物使用,并有利地将它们以0.5-50%,优选为1-40%(重量,以多元醇成分总重量为基)的数量引入到反应混合物中。
在专业文献中可发现与上述常规辅料和添加剂相关的其它细节,如J.H.Sounders和K.C.Frisch,“高聚物”卷XVI,聚氨基甲酸乙酯,第1,2部分,Interscience出版社,1962和1964或塑料手册,聚氨基甲酸乙酯,卷VII,Hanser-出版社,慕尼黑,维也纳,第1、2和3版,1966,1983和1993。
本发明储存稳定、含阻燃剂的多元醇成分原则上适用于用常规方法生产所有类型的刚性PUR泡沫体。
该刚性泡沫体特别是指那些含氨基甲酸乙酯和/或异氰脲酸酯和/或缩二脲和/或脲基甲酸酯和/或脲二酮和/或脲和/或碳化二亚胺基团作为特征性化学结构部分的泡沫体。
它们是通过本发明多元醇成分与有机和/或改性有机聚异氰酸酯反应来制备的。
合适的有机和/或改性有机聚异氰酸酯是本身已知的脂族的、环脂族的、芳脂族的、和优选的芳香多官能的异氰酸酯。
特定的实例是:在亚烷基上具有4-12个碳原子的亚烷基二异氰酸酯,例如,1,2-二异氰酸十二烷酯,1,4-二异氰酸2-乙基甲亚甲酯,1,5-二异氰酸2-甲基五亚甲酯,1,4-二异氰酸四亚甲酯和优选的1,6-二异氰酸六亚甲酯,环脂族二异氰酸酯,如1,3和1,4-二异氰酸环己酯及该异构体的混合物,1-异氰氧基-3,3,5-三甲基-5-异氰氧基甲基环己烷(IPDI);2,4-和2,6-二异氰酸六氢甲代亚苯酯及其相应的异构体混合物,4,4’-,2,2’-和2,4’-二异氰酸二环己基甲酯及其相应的异构体混合物,和优选的芳香族二异氰酸酯和聚异氰酸酯,如2,4和2,6-二异氰酸甲代亚苯酯和相应的异构体混合物,4,4’-,2,2’-和2,4’-二异氰酸二苯甲烷酯和相应的异构体混合物,4,4’-和2,2’-二异氰酸二苯甲烷酯的混合物,聚异氰酸多苯聚亚甲酯,4,4’-,2,2’-和2,4’-二异氰酸二苯甲烷酯和聚异氰酸多苯聚亚甲酯(粗MDI)的混合物以及粗MDI和二异氰酸甲代亚苯酯的混合物。这些有机二异氰酸酯和聚异氰酸酯可以单独一种或以其混合物形式使用。
改性的多官能异氰酸酯,即有机二异氰酸酯和/或聚异氰酸酯的化学的反应产物也经常被采用。可列举的实例是含酯,脲,缩二脲,脲基甲酸酯,碳化二亚胺,异氰脲酸酯,脲二酮和/或氨基甲酸乙酯基团的二异氰酸酯和/或聚异氰酸酯。合适的改性有机二异氰酸酯/聚异氰酸酯的特定实例是:含氨基甲酸乙酯基团并含有33.6-15%,优选为31-21%(重量,以总重量为基)NCO的有机,优选地为芳香聚异氰酸酯,例如用低分子量的二醇、三醇,二亚烷基醇,三亚烷基醇或分子量不大于6000,特别是不大于1500的聚氧化烯醇改性的4,4’-二异氰酸二苯甲烷酯,改性的4,4’-和2,4’-二异氰酸二苯甲烷酯混合物,改性的粗MDI或2,4-和2,6-二异氰酸甲代亚苯酯,可单独一种或以混合物形式使用的二氧化烯基或聚氧化烯醇的实例是二乙二醇和二丙二醇,聚氧乙二醇、三醇和/或四醇,聚氧丙二醇、三醇和/或四醇和聚氧丙二醇、三醇和/或四醇-聚氧乙二醇,三醇和/或四醇。含有NCO基并含有25-3.5%,优选为21-14%(重量,以总重量为基)NCO的预聚物也是合适的,并且其由上述聚酯和/或优选的聚醚多元醇以及4,4’-二异氰酸二苯甲烷酯,2,4’-和4,4’-二异氰酸二苯甲烷酯的混合物,2,4-和/或2,6-二异氰酸甲代亚苯酯或粗MDI制得。其它发现可使用的改性聚异氰酸酯是含有碳化二亚胺基和/或异氰脲酸酯环并含有33.6-15%,优选为31-21%(重量,以总重量为基)NCO的液态聚异氰酸酯,例如以4,4’-,2,4’-和/或2,2’二异氰酸二苯甲烷酯和/或2,4-和/或2,6-二异氰酸甲代亚苯酯为基础的那些聚异氰酸酯。
如果需要,改性聚异氰酸酯可与另一种或与未改性的有机聚异氰酸酯,如2,4’-和/或4,4’-二氰酸二苯甲烷酯,粗MDI,2,4-和/或2,6-二异氰酸甲代亚苯酯混合。
现已发现特别实用的并因此是优选使用的有机聚异氰酸酯是:二异氰酸甲代亚苯酯和粗MDI的混合物或含有氨基甲酸乙酯基团并含有33.6-15%(重量)NCO的改性有机聚异氰酸酯的混合物,特别是以二异氰酸甲代亚苯酯,4,4’-二异氰酸二苯甲烷酯,二异氰酸二苯甲烷酯异构体混合物或粗MDI为基础的;特别是含有30-80%,优选30-60%,特别是30-55%(重量)二异氰酸二苯甲烷酯异构体的粗MDI。
除了本发明多元醇成分和有机和/或改性有机聚异氰酸酯外,还可将上述其它辅料或/和添加剂加入到反应混合物中。
为了生产刚性PUR泡沫体,在其它辅料和/或添加剂的存在下(如果需要)使有机和/或改性有机聚异氰酸酯与本发明多元醇成分反应,它们的数量使聚异氰酸酯中NCO基与多元醇成分中活性氢原子总数的当量比为0.85-1.25∶1,优选0.95-1.15∶1,特别是1-1.05∶1,如果刚性PUR泡沫体含有至少一些键合的异氰脲酸酯基团,刚通常采取1.5-60∶1,优选为1.5-8∶1的聚异氰酸酯中NCO基与多元醇成分中活性氢原子总数之比。
用一次注射法来有利地生产刚性PUR泡沫体,例如在开或闭模,如金属模中使用高压或低压技术。将反应混合物连续地涂在合适的带上以板材也是常用的。
本发明异氰酸酯基刚性PUR泡沫体优选地用浇注或喷射法来生产。特别是使用块体发泡或模制发泡或用双传送带连续生产的方法。
通常在15-90℃,优选20-60℃,特别是20-35℃下混合各原料,并将其引入开模或可处于超大气压的压力下的闭模中,或在连续工作台的情况下,将其涂在与反应混合物相适应的带子上。可用搅拌机或搅拌螺旋进行混合。模具温度有利地为20-110℃,优选为30-60℃,特别是45-50℃。
本发明方法生产的刚性PUR泡沫体具有0.02-0.30克/厘米3,优选为0.025-0.24克/厘米3,特别是0.03-0.1克/厘米3。
它们具有良好的力学和势性能
该产品优选地用作绝势建筑材料。
用以下实施例说明本发明。
实施例1-6和比较实施例1
由下列成分来制备基础混合物:
28份(质量)聚醚醇,其以蔗糖/丙三醇/氧化丙烯为基础(羟基数440),
26份(质量)聚醚醇,其以丙三醇/氧化丙烯为基础(羟基数400),
22份(质量)磷酸三氯丙酯阻燃剂,
4份(重量)四溴苯二甲酸/乙二醇基阻燃剂(羟基数2/5)
15份(质量)二溴丁烯二醇/表氯醇/氧化丙烯基阻燃剂(羟基数330),
1.5份(质量)硅氧烷基泡沫体稳定剂,
3.5份(质量)水。
通过与示于表1中的添加剂混合,由基础混合物来制备最终的多元醇成分。
比较实施例2
在上述基础混合物中,用5份(质量)甲酸(98%纯)代替3.5份(质量)水,并加入1.5份(质量)二甲基环己胺。通过混合原料来制备最终的多元醇成分。此处较大量的甲醇用作发泡剂;其不产生稳定作用。
测定储存稳定性。
通过在45℃下储存二星期来测定储存稳定性。作为储存稳定性的测量手段,按制备多元醇成分后成丝时间的百分数来确定储存后成丝时间(拉丝时间)的变化。用烧杯试验测定成丝时间,其中将42克多元醇成分与58克粗二氰酸二苯甲烷酯(NCO量31.6%)混合。测定可用玻璃棒将反应混合物拉起成丝的最早时间作为成丝时间。
所测定的成丝时间示于表1中。
从实施例中可明显看出含本发明稳定剂的配料与比较实施例相比具有明显改进的储存稳定性。
实施例7-9
在每种情况下,在压力机上以60mm的间隔放置二块厚度0.8mm,尺寸为1000mm×2000mm的钢板。在每种情况下用5.8kg的发泡反应混合物填充钢板之间的空隙。在每种情况下,通过混合2.436kg实施例1,4和6的多元醇化合物和3.364kg的粗MDI(NCO量:31.6%)来制备反应混合物。固化后,从压力机上取下该夹层构件。
该构件可用于绝缘并满足DIN4102规定的建筑B1级要求。
所生产的聚氨基甲酸乙酯泡沫体均具有48kg/m3的松散密度和45kg/m3的核心密度。
表1
实施例1 | 实施例2 | 实施例3 | 实施例4 | 实施例5 | 实施例6 | 比较实施例1 | 比较实施例2 | |
基础混合物(质量份) | 100 | 100 | 100 | 100 | 100 | 100 | 100 | 101.5*) |
添加剂(质量份/化合物) | 1.8IZ-1 | 1.8IZ-10.1FA | 0.9IZ-10.4DMC | 0.9IZ-10.1FA0.6DMC | 3.9IZ-2 | 0.1FA1.0DMC | 1.0DMC | 1.5DMC |
立刻成丝时间(秒) | 84 | 85 | 88 | 76 | 81 | 82 | 82 | 95 |
储存后成丝时间(秒) | 88 | 91 | 103 | 84 | 86 | 93 | 110 | 124 |
成丝时间变化(%) | 5 | 7 | 17 | 11 | 6 | 13 | 34 | 31 |
IZ-1=1-甲基咪唑
IZ-2=1,2-二甲基咪唑
FA=甲酸
DMC=二甲基环己胺
*)=用5份(质量)甲酸(98%纯)代替3.5份(质量)基础混合物中的水
Claims (5)
2.权利要求1的多元醇成分,其中所用咪唑是1-甲基咪唑和/或1,2-二甲基咪唑。
3.权利要求1的多元醇成分,其中所用稳定剂包括数量为0.1-8%(重量)的咪唑,基于多元醇成分计。
4.权利要求1的多元醇成分,其中所用稳定剂是数量为0.01-0.5%(重量)的甲酸,基于多元醇成分计。
5.一种刚性聚氨基甲酸乙酯泡沫体,它基于异氰酸酯并可通过权利要求1的多元醇成分与有机和/或改性有机聚异氰酸酯反应来生产。
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CN110799564A (zh) * | 2017-09-28 | 2020-02-14 | 雅宝公司 | 溴化阻燃剂及其在聚氨酯泡沫中的应用 |
CN111732707A (zh) * | 2020-07-07 | 2020-10-02 | 万华化学集团股份有限公司 | 一种大分子单体稳定剂及其制备方法和应用 |
TWI775882B (zh) * | 2017-09-28 | 2022-09-01 | 美商亞比馬利股份有限公司 | 聚胺基甲酸酯泡沫及其形成方法 |
CN115678413A (zh) * | 2022-09-14 | 2023-02-03 | 徐州卧牛山新型防水材料有限公司 | 一种双组分聚氨酯防水涂料及其制备方法 |
US11897993B2 (en) | 2017-06-27 | 2024-02-13 | Albemarle Corporation | Flame retarded polyurethane foam |
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WO2003091308A1 (en) * | 2002-04-25 | 2003-11-06 | World Properties Inc. | Flame retardant polyurethane composition and method of manufacture thereof |
KR20040035124A (ko) * | 2002-10-18 | 2004-04-29 | 주식회사 두본 | 비할로겐 질소(n)-인(p)계 난연제를 포함하는폴리우레탄용 비할로겐난연제 및 이를 이용한 비할로겐난연 우레탄 발포체와 이들의 제조방법 |
JP5241269B2 (ja) * | 2008-02-26 | 2013-07-17 | 株式会社イノアックコーポレーション | 電磁波シールドガスケット及びそれに用いる軟質ポリウレタンフォーム |
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US11897993B2 (en) | 2017-06-27 | 2024-02-13 | Albemarle Corporation | Flame retarded polyurethane foam |
CN110799564A (zh) * | 2017-09-28 | 2020-02-14 | 雅宝公司 | 溴化阻燃剂及其在聚氨酯泡沫中的应用 |
TWI775882B (zh) * | 2017-09-28 | 2022-09-01 | 美商亞比馬利股份有限公司 | 聚胺基甲酸酯泡沫及其形成方法 |
US11970570B2 (en) | 2017-09-28 | 2024-04-30 | Albemarle Corporation | Brominated flame retardant and its application in polyurethane foams |
CN111732707A (zh) * | 2020-07-07 | 2020-10-02 | 万华化学集团股份有限公司 | 一种大分子单体稳定剂及其制备方法和应用 |
CN111732707B (zh) * | 2020-07-07 | 2022-07-12 | 万华化学集团股份有限公司 | 一种大分子单体稳定剂及其制备方法和应用 |
CN115678413A (zh) * | 2022-09-14 | 2023-02-03 | 徐州卧牛山新型防水材料有限公司 | 一种双组分聚氨酯防水涂料及其制备方法 |
CN115678413B (zh) * | 2022-09-14 | 2023-08-04 | 徐州卧牛山新型防水材料有限公司 | 一种双组分聚氨酯防水涂料及其制备方法 |
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CA2213161A1 (en) | 1998-02-28 |
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