CN116829633A - 包含聚磷酸铵的组合物 - Google Patents
包含聚磷酸铵的组合物 Download PDFInfo
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- CN116829633A CN116829633A CN202280010768.XA CN202280010768A CN116829633A CN 116829633 A CN116829633 A CN 116829633A CN 202280010768 A CN202280010768 A CN 202280010768A CN 116829633 A CN116829633 A CN 116829633A
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- sulfate
- weight
- composition according
- flame retardant
- styrene
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- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 claims description 74
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- 239000003063 flame retardant Substances 0.000 claims description 48
- -1 siloxanes Chemical class 0.000 claims description 47
- 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 claims description 44
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- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 6
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- WXZMFSXDPGVJKK-UHFFFAOYSA-N pentaerythritol Chemical compound OCC(CO)(CO)CO WXZMFSXDPGVJKK-UHFFFAOYSA-N 0.000 claims description 5
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- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 claims description 4
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- 239000004604 Blowing Agent Substances 0.000 claims description 4
- ZRALSGWEFCBTJO-UHFFFAOYSA-N Guanidine Chemical compound NC(N)=N ZRALSGWEFCBTJO-UHFFFAOYSA-N 0.000 claims description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 4
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- 150000001298 alcohols Chemical class 0.000 claims description 4
- TZCXTZWJZNENPQ-UHFFFAOYSA-L barium sulfate Chemical compound [Ba+2].[O-]S([O-])(=O)=O TZCXTZWJZNENPQ-UHFFFAOYSA-L 0.000 claims description 4
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 3
- 229920000084 Gum arabic Polymers 0.000 claims description 3
- 241000978776 Senegalia senegal Species 0.000 claims description 3
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- MOTZDAYCYVMXPC-UHFFFAOYSA-N dodecyl hydrogen sulfate Chemical compound CCCCCCCCCCCCOS(O)(=O)=O MOTZDAYCYVMXPC-UHFFFAOYSA-N 0.000 claims description 3
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- PTJWCLYPVFJWMP-UHFFFAOYSA-N 2-[[3-hydroxy-2-[[3-hydroxy-2,2-bis(hydroxymethyl)propoxy]methyl]-2-(hydroxymethyl)propoxy]methyl]-2-(hydroxymethyl)propane-1,3-diol Chemical compound OCC(CO)(CO)COCC(CO)(CO)COCC(CO)(CO)CO PTJWCLYPVFJWMP-UHFFFAOYSA-N 0.000 claims description 2
- ZNBNBTIDJSKEAM-UHFFFAOYSA-N 4-[7-hydroxy-2-[5-[5-[6-hydroxy-6-(hydroxymethyl)-3,5-dimethyloxan-2-yl]-3-methyloxolan-2-yl]-5-methyloxolan-2-yl]-2,8-dimethyl-1,10-dioxaspiro[4.5]decan-9-yl]-2-methyl-3-propanoyloxypentanoic acid Chemical compound C1C(O)C(C)C(C(C)C(OC(=O)CC)C(C)C(O)=O)OC11OC(C)(C2OC(C)(CC2)C2C(CC(O2)C2C(CC(C)C(O)(CO)O2)C)C)CC1 ZNBNBTIDJSKEAM-UHFFFAOYSA-N 0.000 claims description 2
- FUSNOPLQVRUIIM-UHFFFAOYSA-N 4-amino-2-(4,4-dimethyl-2-oxoimidazolidin-1-yl)-n-[3-(trifluoromethyl)phenyl]pyrimidine-5-carboxamide Chemical compound O=C1NC(C)(C)CN1C(N=C1N)=NC=C1C(=O)NC1=CC=CC(C(F)(F)F)=C1 FUSNOPLQVRUIIM-UHFFFAOYSA-N 0.000 claims description 2
- 239000005995 Aluminium silicate Substances 0.000 claims description 2
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- FBPFZTCFMRRESA-FSIIMWSLSA-N D-Glucitol Natural products OC[C@H](O)[C@H](O)[C@@H](O)[C@H](O)CO FBPFZTCFMRRESA-FSIIMWSLSA-N 0.000 claims description 2
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- CHJJGSNFBQVOTG-UHFFFAOYSA-N N-methyl-guanidine Natural products CNC(N)=N CHJJGSNFBQVOTG-UHFFFAOYSA-N 0.000 claims description 2
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- RJFAYQIBOAGBLC-BYPYZUCNSA-N Selenium-L-methionine Chemical compound C[Se]CC[C@H](N)C(O)=O RJFAYQIBOAGBLC-BYPYZUCNSA-N 0.000 claims description 2
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- SSBRSHIQIANGKS-UHFFFAOYSA-N [amino(hydroxy)methylidene]azanium;hydrogen sulfate Chemical compound NC(N)=O.OS(O)(=O)=O SSBRSHIQIANGKS-UHFFFAOYSA-N 0.000 claims description 2
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- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 claims description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 2
- 235000012211 aluminium silicate Nutrition 0.000 claims description 2
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 claims description 2
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- JXRVKYBCWUJJBP-UHFFFAOYSA-L calcium;hydrogen sulfate Chemical compound [Ca+2].OS([O-])(=O)=O.OS([O-])(=O)=O JXRVKYBCWUJJBP-UHFFFAOYSA-L 0.000 claims description 2
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- OZECDDHOAMNMQI-UHFFFAOYSA-H cerium(3+);trisulfate Chemical compound [Ce+3].[Ce+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O OZECDDHOAMNMQI-UHFFFAOYSA-H 0.000 claims description 2
- 229910000361 cobalt sulfate Inorganic materials 0.000 claims description 2
- 229940044175 cobalt sulfate Drugs 0.000 claims description 2
- KTVIXTQDYHMGHF-UHFFFAOYSA-L cobalt(2+) sulfate Chemical compound [Co+2].[O-]S([O-])(=O)=O KTVIXTQDYHMGHF-UHFFFAOYSA-L 0.000 claims description 2
- 239000007859 condensation product Substances 0.000 claims description 2
- 238000004132 cross linking Methods 0.000 claims description 2
- JBSLOWBPDRZSMB-FPLPWBNLSA-N dibutyl (z)-but-2-enedioate Chemical compound CCCCOC(=O)\C=C/C(=O)OCCCC JBSLOWBPDRZSMB-FPLPWBNLSA-N 0.000 claims description 2
- QGBSISYHAICWAH-UHFFFAOYSA-N dicyandiamide Chemical compound NC(N)=NC#N QGBSISYHAICWAH-UHFFFAOYSA-N 0.000 claims description 2
- DENRZWYUOJLTMF-UHFFFAOYSA-N diethyl sulfate Chemical compound CCOS(=O)(=O)OCC DENRZWYUOJLTMF-UHFFFAOYSA-N 0.000 claims description 2
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- VAYGXNSJCAHWJZ-UHFFFAOYSA-N dimethyl sulfate Chemical compound COS(=O)(=O)OC VAYGXNSJCAHWJZ-UHFFFAOYSA-N 0.000 claims description 2
- SWSQBOPZIKWTGO-UHFFFAOYSA-N dimethylaminoamidine Natural products CN(C)C(N)=N SWSQBOPZIKWTGO-UHFFFAOYSA-N 0.000 claims description 2
- IVJISJACKSSFGE-UHFFFAOYSA-N formaldehyde;1,3,5-triazine-2,4,6-triamine Chemical compound O=C.NC1=NC(N)=NC(N)=N1 IVJISJACKSSFGE-UHFFFAOYSA-N 0.000 claims description 2
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- 229910000377 hydrazine sulfate Inorganic materials 0.000 claims description 2
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- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 claims description 2
- RUTXIHLAWFEWGM-UHFFFAOYSA-H iron(3+) sulfate Chemical compound [Fe+3].[Fe+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O RUTXIHLAWFEWGM-UHFFFAOYSA-H 0.000 claims description 2
- 229910000359 iron(II) sulfate Inorganic materials 0.000 claims description 2
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- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 claims description 2
- 150000002576 ketones Chemical class 0.000 claims description 2
- INHCSSUBVCNVSK-UHFFFAOYSA-L lithium sulfate Inorganic materials [Li+].[Li+].[O-]S([O-])(=O)=O INHCSSUBVCNVSK-UHFFFAOYSA-L 0.000 claims description 2
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 claims description 2
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- ANXKZXRDXAZQJT-UHFFFAOYSA-M methyl sulfate;trimethylsulfanium Chemical compound C[S+](C)C.COS([O-])(=O)=O ANXKZXRDXAZQJT-UHFFFAOYSA-M 0.000 claims description 2
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- NKNFUMKGJYKPCT-UHFFFAOYSA-N n,n-diethylethanamine;sulfuric acid Chemical compound [O-]S([O-])(=O)=O.CC[NH+](CC)CC.CC[NH+](CC)CC NKNFUMKGJYKPCT-UHFFFAOYSA-N 0.000 claims description 2
- GJQIMXVRFNLMTB-UHFFFAOYSA-N nonyl acetic acid ester Natural products CCCCCCCCCOC(C)=O GJQIMXVRFNLMTB-UHFFFAOYSA-N 0.000 claims description 2
- DCKVFVYPWDKYDN-UHFFFAOYSA-L oxygen(2-);titanium(4+);sulfate Chemical compound [O-2].[Ti+4].[O-]S([O-])(=O)=O DCKVFVYPWDKYDN-UHFFFAOYSA-L 0.000 claims description 2
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- GRLPQNLYRHEGIJ-UHFFFAOYSA-J potassium aluminium sulfate Chemical compound [Al+3].[K+].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O GRLPQNLYRHEGIJ-UHFFFAOYSA-J 0.000 claims description 2
- HJWLCRVIBGQPNF-UHFFFAOYSA-N prop-2-enylbenzene Chemical compound C=CCC1=CC=CC=C1 HJWLCRVIBGQPNF-UHFFFAOYSA-N 0.000 claims description 2
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- WBHQBSYUUJJSRZ-UHFFFAOYSA-M sodium bisulfate Chemical compound [Na+].OS([O-])(=O)=O WBHQBSYUUJJSRZ-UHFFFAOYSA-M 0.000 claims description 2
- 229910000342 sodium bisulfate Inorganic materials 0.000 claims description 2
- XZTJQQLJJCXOLP-UHFFFAOYSA-M sodium;decyl sulfate Chemical compound [Na+].CCCCCCCCCCOS([O-])(=O)=O XZTJQQLJJCXOLP-UHFFFAOYSA-M 0.000 claims description 2
- NWZBFJYXRGSRGD-UHFFFAOYSA-M sodium;octadecyl sulfate Chemical compound [Na+].CCCCCCCCCCCCCCCCCCOS([O-])(=O)=O NWZBFJYXRGSRGD-UHFFFAOYSA-M 0.000 claims description 2
- 239000000600 sorbitol Substances 0.000 claims description 2
- LTURHSAEWJPFAA-UHFFFAOYSA-N sulfuric acid;1,3,5-triazine-2,4,6-triamine Chemical compound OS(O)(=O)=O.NC1=NC(N)=NC(N)=N1 LTURHSAEWJPFAA-UHFFFAOYSA-N 0.000 claims description 2
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- MHSKRLJMQQNJNC-UHFFFAOYSA-N terephthalamide Chemical compound NC(=O)C1=CC=C(C(N)=O)C=C1 MHSKRLJMQQNJNC-UHFFFAOYSA-N 0.000 description 1
- KKEYFWRCBNTPAC-UHFFFAOYSA-L terephthalate(2-) Chemical compound [O-]C(=O)C1=CC=C(C([O-])=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-L 0.000 description 1
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Abstract
本发明涉及以下组合物,其包含:作为组分(A)的0.1重量%至99.9重量%的相II聚磷酸铵,和作为组分(B)的0.1重量%至99.9重量%的相I和/或相III、IV、V和/或VI聚磷酸铵,其中所述组分的总和为100重量%,并涉及其在膨胀型涂料中的用途。
Description
技术领域
本发明涉及包含聚磷酸铵的组合物。
背景技术
聚磷酸铵被广泛用作阻燃剂。此外,聚磷酸铵还可以用于防止在含有游离硝酸并用于金属表面处理的(酸)浴中产生亚硝气(EP-A-0004560)。
聚磷酸铵可以以几种晶型(crystalline form)(I至VI)存在,其中晶型I的聚磷酸铵可由缩合剂和磷酸或磷酸盐合成。
晶型II的聚磷酸铵是一种微溶于水的产品,并且已知是用于在合成树脂中使用的阻燃剂成分。它通常由五氧化二磷制备。
制备晶型II的聚磷酸铵的已知方法的特征在于,使晶型I的聚磷酸铵经历特定时间段的热处理(C.Y.Shen等人,Journal of American Chemical Society,第91卷,第62页(1969))。其中同样还提出了制备晶型(crystal form)II和IV的方法。
M.Watanabe,M.Sakurai和M.Takahashi,Phosphorus Research Bulletin 2003,16,第39-46页描述了晶型I和晶型V的聚磷酸铵。
M.Watanabe,N.Narita,M.Sakurai,H.Suzuki,Bulletin of the ChemicalSociety of Japan 2000,73,115-119和R.C.Sheridan,J.F.McCullough,N.E.Stahlheber,C.Y.Shen在Inorganic Syntheses,John Wiley&Sons,Inc,1979,278-280中和K.R.Waerstad,G.H.McClellan,J.Agric.Food Chem.1976,24,412-415描述了制备晶型II的聚磷酸铵的不同方法。
US-A-3,978,195要求保护一种用于制备基本上不溶于水的链状聚磷酸铵的方法,其中使等摩尔量的正磷酸铵和五氧化二磷在存在氨气的情况下,在170至350℃的温度下,在配备有混合工具的反应器中,在持续混合、捏合和粉碎的情况下进行反应。
在EP-A-0537475中描述的另一种方法中,使正磷酸铵、五氧化二磷和气态氨在第一阶段中彼此反应,以便在第二阶段中,在盘式干燥器上,在氨气气氛下进一步冷凝和干燥中间体。
聚磷酸铵通常难以以高纯度和均质形式制备;特别地,它的残留水分含量和吸湿性能在储存和运输中表现出相当大的问题。
如今,已知的聚磷酸铵经常用于膨胀型配制剂,这些配制剂然后又用作阻燃涂料。
尽管常规的阻燃配制剂主要用于保护热敏性较低的基材,例如钢、铝和/或混凝土,但对于绝缘(保护)热稳定性较低的基材的需求日益增长。这些可以是有机和无机材料。这些可具有聚合物和非聚合物特性。
对于所有基材,在低温下的热绝缘是必不可少的,因为不仅发生的热解反应受到抑制;而且在惰性基材(例如钢)的情况下,由于在低温下发生的膨胀,在整个火灾过程中的绝缘效果也会增加。可以实现长得多的阻燃时间,或可以明显减少施加的量。
发明内容
因此,本发明的目的是提供以下聚磷酸铵:它们是稳定且易于处理的,并且导致增加的基材保护,尤其是在膨胀型涂料中使用的情况下。
这个目的通过以下组合物得以实现,所述组合物包含:
作为组分(A)的0.1重量%至99.9重量%的相II聚磷酸铵,和
作为组分(B)的0.1重量%至99.9重量%的相I和/或相III、IV、V和/或VI聚磷酸铵,其中所述组分的总和为100重量%。
所述组合物优选含有60重量%至99.9重量%的组分A和0.1重量%至40重量%的组分B。
所述组合物更优选含有65重量%至92重量%的组分A和8重量%至35重量%的组分B。
优选其中组分A是相II聚磷酸铵并且组分B是相I聚磷酸铵的组合物。
组分A优选是具有式(NH4)n+2PnO3n+1的相II聚磷酸铵,其中n=300至100000。
组分A更优选是具有式(NH4)n+2PnO3n+1的相II聚磷酸铵,其中n=1000至25000。
组分B优选是具有式(NH4)n+2PnO3n+1的相I聚磷酸铵,其中n=5至100。
根据本发明的组合物优选具有
—小于0.5%的根据ISO 760的残留水分含量(水含量),
—0.3至0.9g/cm3的堆密度,
—小于1.5%的水溶解度(25℃下10%的水中悬浮液),
—小于40mPas的粘度(Brookfield DV3T,速度50rpm,转子1),
—1至50μm的粒度d50,其是通过激光衍射测量的,
—10至60μm的粒度d90,其是通过激光衍射测量的,和
—4至8的pH(25℃下10%的水中悬浮液)。
在根据本发明的组合物中,优选所述聚磷酸氨已经用以下物质微胶囊化:有机官能(聚)硅烷,(聚)硅氧烷,(聚)硅氮烷,改性蜡,聚氨酯,聚环氧化物,脲-甲醛树脂,三聚氰胺-甲醛树脂,基于(甲基)丙烯酸酯树脂、基于苯乙烯/丙烯酸酯共聚物、氨基甲酸酯(urethane)、基于乙烯/乙酸壬酯共聚物、基于橡胶的乳液和/或它们的混合物。
优选以下组合物,其还含有基于组分(A)和(B)的量计最高至10重量%的以下组分:
硫酸铵、硫酸三乙铵、硫酸四甲铵、硫酸三甲铵、硫酸二甲酯、硫酸二乙酯、硫酸二丙酯、辛基硫酸钠、癸基硫酸钠、十八烷基硫酸钠、硫酸月桂酯(lauryl sulfate)、硫酸脲、硫酸三聚氰胺、硫酸羟胺、硫酸肼、硫酸钾、硫酸氢钾、硫酸钠、硫酸氢钠、硫酸镁、硫酸氢镁、硫酸钙、硫酸氢钙、硫酸钡、硫酸铝钾、硫酸铝、硫酸铁(III)、硫酸铁(II)、硫酸钴、硫酸钛、硫酸锌、硫酸锡、硫酸铈、硫酸锂、三甲基锍甲基硫酸盐或它们的混合物。
本发明还涉及根据权利要求1至10中至少一项所述的组合物用于降低膨胀型涂料的起始反应温度,用于提高膨胀型涂料的阻燃能力,用作透明涂料(clearcoat)和膨胀型涂料的阻燃剂,用于或用作木材和其它纤维素产品的阻燃剂,用于或用作聚合物、凝胶涂层(gelcoat)和/或不饱和聚酯树脂的反应性和/或非反应性阻燃剂,用于制备阻燃聚合物模塑配混料,用于制备阻燃聚合物模制件,用于使聚酯以及纯的和混纺的纤维素织物具有阻燃性,用于聚氨酯泡沫,用于聚烯烃,用于不饱和聚酯和酚醛树脂以及用于使纺织品具有阻燃性的用途。
本发明同样还涉及根据权利要求1至10中至少一项所述的组合物在以下物质中或用于以下物质的用途:插塞式连接器、电力分配器中的载流组件(剩余电流保护)、电路板、灌封料(potting compound)、电源连接器、断路器、灯罩、LED灯罩、电容器罩、线圈元件、通风设备、接地触点、插头,在以下物质中/上的用途:印刷电路板、用于插头的罩、电池罩、电缆、柔性电路板、充电电缆、电机盖、纺织品涂层和其它产品。
特别地,本发明涉及根据权利要求1至10中至少一项所述的组合物用于在钢材、木材、木基材料、纸、矿物棉、石膏板、塑料、金属、合金、由合成或天然纤维和其它材料制成的织物上的阻燃涂料和/或用作阻焊层(solder mask)以及用于电气开关和电路的用途。
特别优选根据权利要求1至10中至少一项所述的组合物用于涂覆钢构造、天花板、墙壁、电缆、管道、导管、电缆和组合舱壁(bulkhead)、门、帘、烟道栅栏、百叶窗、安全柜、安装柜和其它制品的用途,所述钢构造例如钢梁和钢支架。
本发明还涉及阻燃涂料,其包含成膜粘结剂、发泡剂、作为泡沫形成物质的根据权利要求1至10中一项或多项所述的组合物、碳形成物质、助剂和添加剂,以及非必要的增稠剂、分散添加剂和溶剂和/或溶剂混合物。
这样的阻燃涂料优选包含成膜粘结剂、发泡剂、作为泡沫形成物质的根据权利要求1至10中一项或多项所述的组合物、作为碳形成物质的至少一种多元醇、助剂和/或添加剂、增稠剂、分散添加剂和溶剂和/或溶剂混合物。
本发明特别优选以下阻燃涂料,其包含:
5重量%至69.4重量%的成膜粘结剂,
5重量%至25重量%的发泡剂,
5重量%至40重量%的作为泡沫形成物质的根据权利要求1至10中一项或多项所述的组合物,
5重量%至25重量%的碳形成物质,
5重量%至40重量%的助剂和/或添加剂,
0.5重量%至10重量%的增稠剂,
0.1重量%至10重量%的润湿和/或分散添加剂,和
10重量%至40重量%的溶剂和/或溶剂混合物,其中所述组分加起来最高至100重量%。
所述成膜粘结剂优选包含基于苯乙烯和丙烯酸系酯(acrylic ester)的共聚物,基于丙烯酸系酯的共聚物,乙烯基甲苯/丙烯酸酯共聚物,苯乙烯/丙烯酸酯聚合物,基于乙酸乙烯酯的均聚物,基于乙酸乙烯酯、乙烯和氯乙烯的共聚物,基于乙酸乙烯酯和长链支化羧酸的乙烯基酯的共聚物,基于乙酸乙烯酯和马来酸二正丁酯和/或丙烯酸系酯的共聚物,乙烯基/丙烯酸酯共聚物,自交联聚氨酯分散体,萜烯和/或聚萜烯和/或它们的混合物;
所述发泡剂是三聚氰胺,三聚氰胺-甲醛缩合物,胍,它们的盐,三聚氰胺缩合产物和/或双氰胺(dicyandiamide);
所述碳形成物质是淀粉,改性淀粉,多元醇(多羟基化合物),例如糖类(saccharide)和多糖,和/或热塑性或热固性聚合物树脂粘结剂,例如酚醛树脂,脲醛树脂(a urea resin),聚氨酯,聚氯乙烯,聚(甲基)丙烯酸酯,聚乙酸乙烯酯,聚乙烯醇,有机硅树脂和/或橡胶;
所述助剂和添加剂是玻璃纤维,矿物纤维,金属纤维,碳纤维,高岭土,滑石,氧化铝,氢氧化铝,氢氧化镁和其它金属氧化物,沉淀二氧化硅,硅酸盐和/或粉状的纤维素;
所述增稠剂和/或流变学添加剂是(改性的)纤维素,二氧化硅,膨润土,蓖麻油衍生物,脂肪衍生物,聚酰胺,聚(甲基)丙烯酸酯,聚丙烯酰胺,聚醚,聚氨酯,聚乙烯醇,聚乙烯基吡咯烷酮,糖聚合物,例如阿拉伯树胶(gum arabic),藻酸盐(alginate),黄原胶(xanthan)和/或琼脂(agar-agar);
所述润湿和分散添加剂是烷基酚乙氧基化物,聚丙烯酸和/或聚氨酯;
所述有机溶剂和/或溶剂混合物是芳族烃,优选二甲苯和/或烷基苯,
优选甲苯和乙苯;醇,优选甲醇,和/或链烷醇(alkanol),优选2-甲基-1-丙醇;酮,例如丙酮或丁酮,链烷酸酯(alkanoic ester)和/或聚醚,优选聚二醇醚(polyglycolether)。
所述多羟基化合物优选是三季戊四醇和/或季戊四醇的缩聚物和/或基于季戊四醇的酯与多羟基化合物、聚乙酸乙烯酯、聚乙烯醇、山梨糖醇和/或环氧乙烷-环氧丙烷多羟基化合物的混合物。
本发明还涉及制备根据权利要求1至10中一项或多项所述的混合物的方法,其特征在于,将各自呈粉末形式或作为粒料的组分(A)和组分(B)彼此混合,或将溶解的组分(B)引入到组分(A)中。
另外一种制备根据本发明的混合物的方法的特征在于将等摩尔量的正磷酸二氢铵和脲加热到250至300℃的温度保持0.5至4小时的时间。
另一种制备根据本发明的混合物的方法的特征在于将等摩尔量的正磷酸铵和脲在潮湿的氨气氛下加热到250至305℃的温度保持0.1至4小时的时间。
一种可另选的制备根据本发明的混合物的方法的特征在于将等摩尔量的正磷酸铵和脲在潮湿的氨气氛下,在同时添加组分(B)的情况下加热到320至350℃的温度保持0.1至4小时的时间。
聚磷酸铵的一个优选应用领域是膨胀型配制剂,该配制剂然后用作阻燃涂料。
还被称为形成绝缘层阻燃涂料的膨胀型涂料的特征在于它们在发生火灾时在相应的热的作用下发泡,并且所述阻燃涂料的这种发泡阻碍或至少阻止热传递到基材,例如钢构造、屋顶、墙壁、电缆、管道和类似物。
由本发明的涂料形成的绝缘层已经具有优异的强度和热绝缘性能,并且特征在于与常规涂料配制剂相比反应更早开始。因此,所述的根据本发明的膨胀型涂料组合物适用于有效保护钢结构和其它物质以及保护热敏性基材。
例如,钢框架建筑物与常规建筑方法相比有许多优点,但也有严重的缺点,即在发生火灾时,未受保护的钢材的温度快速升高到如此高的程度以至于所述钢材软化、失去刚度并因此危及结构的稳定性(倒塌的风险,阻止从建筑物中离开等)。因此,建议对所述钢材进行热绝缘。例如,可以将膨胀型涂料施加于各种结构以延迟火灾的热效应。这种涂料减缓了施加有该涂料的相应基材的温度升高速率,并且因此延长了所述结构由于来自于火灾的热量而倒塌之前的时间。额外的时间增加了灭火和冷却建筑物的机会,并延长了可供逃跑的时间。
非必要地可以将一种或多种反应性阻燃剂添加到根据本发明的组合物中。在本发明情况下,一个实例是反应性有机磷化合物,例如9,10-二氢-9-氧杂-10-磷杂菲10-氧化物(DOPO)及其衍生物和加合物。
本发明的组合物可优选进一步包含次膦酸盐(EP-A-1544206)。
与不含次膦酸盐的配制剂相比,使用上述次膦酸盐或二次膦酸盐将膨胀反应的起始温度降低了超过15℃。
所述有机溶剂优选是芳族烃,优选二甲苯和/或烷基苯,优选乙苯;醇,优选甲醇,和/或链烷醇,更优选2-甲基-1-丙醇;聚醚,优选聚二醇醚,更优选α-异十三烷基-ω-羟基-聚二醇醚。
可向所述组合物中添加额外的添加剂,例如增稠剂和/或流变学添加剂,以及填料。使用的流变学添加剂,例如防沉剂、抗流动剂(anti-running agent)和触变剂,优选是聚羟基羧酸酰胺,脲衍生物,不饱和羧酸酯的盐,酸性磷酸衍生物的烷基铵盐,对甲苯磺酸的胺盐,磺酸衍生物的胺盐,和所述化合物的水性或有机溶液或混合物。此外,可以使用基于热解二氧化硅或沉淀二氧化硅或基于硅烷化的热解二氧化硅或沉淀二氧化硅的流变学添加剂。所述流变学添加剂优选包含热解二氧化硅、改性和未改性的片状硅酸盐、沉淀二氧化硅、纤维素醚、多糖、聚氨酯和丙烯酸酯增稠剂、脲衍生物、蓖麻油衍生物、聚酰胺、脂肪酸酰胺和聚烯烃,条件是它们是固体形式,粉状的纤维素和/或悬浮介质,例如黄原胶。
这样的阻燃涂料(膨胀型涂料)主要以可涂覆的、可涂抹的或可辊涂的漆的形式用于保护各种不同的基材,优选钢梁和钢柱、屋顶、墙壁、电缆、管道、电缆管道、电缆和组合舱壁、门、帘、防烟垂壁、百叶窗、安全柜、安装柜和类似物。
本发明尤其涉及根据本发明的阻燃涂料在钢材、木材、木基材料、纸、矿物棉、石膏板、塑料、金属、合金、由合成或天然纤维制成的织物和其它合适材料上的用途和/或用作阻焊层以及用于电气开关和电路的用途。根据本发明的阻燃涂料非常适用于空心型材和H形型材的结构防火和车间应用;它同样适用于其中需要提高的风化稳定性的区域。
根据本发明的混合物非常适合于上述在膨胀型配制剂中,和然后作为阻燃涂料的用途。
根据本发明的混合物还可优选用于或用作在聚烯烃上的膨胀型涂料。
优选的聚烯烃例如是单烯烃和二烯烃(例如乙烯、丙烯、异丁烯、丁烯、4-甲基戊烯、异戊二烯、丁二烯、苯乙烯)的聚合物,例如聚丙烯,聚异丁烯,聚丁-1-烯,聚-4-甲基戊-1-烯,聚苯乙烯,聚(对甲基苯乙烯)和/或聚(α-甲基苯乙烯),聚异戊二烯或聚丁二烯和聚乙烯(非必要交联的),例如高密度聚乙烯(HDPE)、高密度高分子量聚乙烯(HDPE-HMW)、高密度超高分子量聚乙烯(HDPE-UHMW)、中密度聚乙烯(HMDPE)、低密度聚乙烯(LDPE)、线性低密度聚乙烯(LLDPE)、极低密度聚乙烯(VLDPE)、支化低密度聚乙烯(BLDPE),以及环烯烃的聚合物,例如环戊烯或降冰片烯的聚合物。
优选的聚合物另外是上文列出的聚烯烃的混合物(共混物),例如聚丙烯(PP)与聚异丁烯、聚乙烯与聚异丁烯、聚丙烯与聚乙烯(例如PP/HDPE/LDPE)和各种类型聚乙烯的混合物(例如LDPE/HDPE)。
可优选使用的聚合物另外是单烯烃和二烯烃与彼此的共聚物以及单烯烃和二烯烃与其它乙烯基型单体的共聚物,例如乙烯-丙烯共聚物;LLDPE、VLDPE和它们与LDPE的混合物;丙烯-丁-1-烯共聚物,丙烯-异丁烯共聚物,乙烯-丁-1-烯共聚物,乙烯-己烯共聚物,乙烯-甲基戊烯共聚物,乙烯-庚烯共聚物,乙烯-辛烯共聚物,丙烯-丁二烯共聚物,异丁烯-异戊二烯共聚物,乙烯-丙烯酸烷基酯共聚物,乙烯-甲基丙烯酸烷基酯共聚物,乙烯-乙酸乙烯酯共聚物,苯乙烯或α-甲基苯乙烯与二烯或丙烯酸系衍生物的共聚物,例如苯乙烯-丁二烯,苯乙烯-丙烯腈,苯乙烯-甲基丙烯酸烷基酯,苯乙烯-丁二烯-丙烯酸烷基酯和甲基丙烯酸烷基酯,苯乙烯-马来酸酐,苯乙烯-丙烯腈-丙烯酸甲酯;苯乙烯共聚物和另一种聚合物的高抗冲击性混合物,所述另一种聚合物例如聚丙烯酸酯、二烯聚合物或乙烯-丙烯-二烯三元共聚物;和苯乙烯的嵌段共聚物,例如苯乙烯-丁二烯-苯乙烯、苯乙烯-异戊二烯-苯乙烯、苯乙烯-乙烯/丁烯-苯乙烯或苯乙烯-乙烯/丙烯-苯乙烯,以及苯乙烯或α-甲基苯乙烯的接枝共聚物,例如接枝到聚丁二烯上的苯乙烯,接枝到聚丁二烯-苯乙烯共聚物上或聚丁二烯-丙烯腈共聚物上的苯乙烯,接枝到聚丁二烯上的苯乙烯和丙烯腈(或甲基丙烯腈);接枝到聚丁二烯上的苯乙烯、丙烯腈和甲基丙烯酸甲酯;接枝到聚丁二烯上的苯乙烯和马来酸酐;接枝到聚丁二烯上的苯乙烯、丙烯腈和马来酸酐或马来酰亚胺;接枝到聚丁二烯上的苯乙烯和马来酰亚胺,接枝到聚丁二烯上的苯乙烯和丙烯酸烷基酯或甲基丙烯酸烷基酯,接枝到乙烯-丙烯-二烯三元共聚物上的苯乙烯和丙烯腈,接枝到聚丙烯酸烷基酯或聚甲基丙烯酸烷基酯上的苯乙烯和丙烯腈,接枝到丙烯酸酯-丁二烯共聚物上的苯乙烯和丙烯腈和它们的混合物,如例如作为所谓的ABS、MBS、ASA或AES聚合物已知的那些;以及它们与一氧化碳的共聚物或乙烯-丙烯酸共聚物及其盐(离聚物)以及乙烯与丙烯和二烯的三元共聚物,所述二烯例如己二烯、二环戊二烯或乙叉基降冰片烯;以及这样的共聚物与彼此的和/或与其它聚合物形成的混合物,例如聚丙烯-乙烯-丙烯共聚物、LDPE-乙烯-乙酸乙烯酯共聚物、LDPE-乙烯-丙烯酸共聚物、LLDPE-乙烯-乙酸乙烯酯共聚物、LLDPE-乙烯-丙烯酸共聚物,以及交替或无规的聚亚烷基-一氧化碳共聚物和它们与其它聚合物的混合物,所述其它聚合物例如聚酰胺。
根据本发明的混合物还可用于热塑性聚合物,例如聚酯、聚苯乙烯或聚酰胺,以及热固性聚合物,例如不饱和聚酯树脂、环氧树脂、聚氨酯或丙烯酸酯。
合适的聚酯衍生自二羧酸及其与二醇形成的酯和/或衍生自羟基羧酸或相应的内酯。特别优选使用对苯二甲酸和乙二醇、丙烷-1,3-二醇和丁烷-1,3-二醇。
合适的聚酯包括聚对苯二甲酸乙二醇酯、聚对苯二甲酸丁二醇酯(得自Celanese的2500、/>2002;得自BASF的/>),聚对苯二甲酸1,4-二羟甲基环己烷酯,聚羟基苯甲酸酯和衍生自具有羟基端基的聚醚的嵌段聚醚酯;以及用聚碳酸酯或MBS改性的聚酯。
所述聚合物优选是单烯烃和二烯烃的聚合物,例如聚丙烯、聚异丁烯、聚1-丁烯、聚-4-甲基-1-戊烯、聚异戊烯或聚丁二烯,以及环烯烃的加成聚合物,所述环烯烃例如环戊烯或降冰片烯;以及聚乙烯(其可非必要是交联的),例如高密度聚乙烯(HDPE)、高密度高分子量聚乙烯(HDPE-HMW)、高密度超高分子量聚乙烯(HDPE-UHMW)、中密度聚乙烯(MDPE)、低密度聚乙烯(LDPE)、线性低密度聚乙烯(LLDPE)、支化低密度聚乙烯(BLDPE)和它们的混合物。
所述聚合物优选是单烯烃和二烯烃与彼此的或与其它乙烯基单体的共聚物,例如乙烯-丙烯共聚物,线性低密度聚乙烯(LLDPE)和它们与以下物质的混合物:低密度聚乙烯(LDPE),丙烯-1-丁烯共聚物,丙烯-异丁烯共聚物,乙烯-1-丁烯共聚物,乙烯-己烯共聚物,乙烯-甲基戊烯共聚物,乙烯-庚烯共聚物,乙烯-辛烯共聚物,丙烯-丁二烯共聚物,异丁烯-异戊二烯共聚物,乙烯-丙烯酸烷基酯共聚物,乙烯-甲基丙烯酸烷基酯共聚物,乙烯-乙酸乙烯酯共聚物和它们与一氧化碳的共聚物,或乙烯-丙烯酸共聚物和它们的盐(离聚物),以及乙烯与丙烯和二烯的三元共聚物,所述二烯例如己二烯、二环戊二烯或乙叉基降冰片烯;以及这样的共聚物与彼此的混合物,例如聚丙烯/乙烯-丙烯共聚物,LDPE/乙烯-乙酸乙烯酯共聚物,LDPE/乙烯-丙烯酸共聚物,LLDPE/乙烯-乙酸乙烯酯共聚物,LLDPE/乙烯-丙烯酸共聚物,和交替或无规的聚烯(polyalkylene)/一氧化碳共聚物,和它们与其它聚合物的混合物,所述其它聚合物例如聚酰胺。
所述聚合物优选是烃树脂(例如C5-C9),其包括它们氢化的改性物(例如增粘树脂)和聚烯和淀粉的混合物。
所述聚合物优选是聚苯乙烯(143E(BASF)、聚(对甲基苯乙烯)、聚(α-甲基苯乙烯))。
所述聚合物优选是苯乙烯或α-甲基苯乙烯与二烯或丙烯酸系衍生物的共聚物,例如苯乙烯-丁二烯、苯乙烯-丙烯腈、苯乙烯-甲基丙烯酸烷基酯、苯乙烯-丁二烯-丙烯酸烷基酯和甲基丙烯酸烷基酯、苯乙烯-马来酸酐、苯乙烯-丙烯腈-甲基丙烯酸酯;苯乙烯共聚物和另一种聚合物的高抗冲击性混合物,所述另一种聚合物例如聚丙烯酸酯、二烯聚合物或乙烯-丙烯-二烯三元共聚物;和苯乙烯的嵌段共聚物,例如苯乙烯-丁二烯-苯乙烯、苯乙烯-异戊二烯-苯乙烯、苯乙烯-乙烯/丁烯-苯乙烯或苯乙烯-乙烯/丙烯-苯乙烯。
所述聚合物优选是苯乙烯或α-甲基苯乙烯的接枝共聚物,例如在聚丁二烯上的苯乙烯、在聚丁二烯-苯乙烯或聚丁二烯-丙烯腈共聚物上的苯乙烯,在聚丁二烯上的苯乙烯和丙烯腈(或甲基丙烯腈);在聚丁二烯上的苯乙烯、丙烯腈和甲基丙烯酸甲酯;在聚丁二烯上的苯乙烯和马来酸酐,在聚丁二烯上的苯乙烯、丙烯腈和马来酸酐或马来酰亚胺,在聚丁二烯上的苯乙烯和马来酰亚胺,在聚丁二烯上的苯乙烯和丙烯酸烷基酯/甲基丙烯酸烷基酯,在乙烯-丙烯-二烯三元共聚物上的苯乙烯和丙烯腈,在聚丙烯酸烷基酯或聚甲基丙烯酸烷基酯上的苯乙烯和丙烯腈,在丙烯酸酯-丁二烯共聚物上的苯乙烯和丙烯腈,以及它们的混合物,例如作为ABS、MBS、ASA或AES聚合物已知的那些。
所述苯乙烯聚合物优选是相对粗孔的泡沫,例如EPS(发泡聚苯乙烯),例如(BASF)和/或具有相对细孔的泡沫,例如XPS(挤出硬质聚苯乙烯泡沫),例如(BASF)。优选聚苯乙烯泡沫,例如/>XPS、/>(DowChemical)和类似物。
所述聚合物优选是卤化聚合物,例如聚氯丁二烯、氯丁橡胶(chlorine rubber)、异丁烯-异戊二烯的氯化和溴化共聚物(卤化丁基橡胶)、氯化或氯磺化聚乙烯、乙烯和氯化乙烯的共聚物、表氯醇均聚物和共聚物,尤其是卤化乙烯基化合物的聚合物,例如聚氯乙烯、聚偏二氯乙烯、聚氟乙烯、聚偏二氟乙烯;以及它们的共聚物,例如氯乙烯-偏二氯乙烯、氯乙烯-乙酸乙烯酯或偏二氯乙烯-乙酸乙烯酯。
所述聚合物优选是衍生自以下物质的聚合物:α,β-不饱和酸及其衍生物,例如聚丙烯酸酯和聚甲基丙烯酸酯,用丙烯酸丁酯抗冲改性的聚甲基丙烯酸甲酯、聚丙烯酰胺和聚丙烯腈,和所述单体与彼此的或与其它不饱和单体的共聚物,例如丙烯腈-丁二烯共聚物、丙烯腈-丙烯酸烷基酯共聚物、丙烯腈-丙烯酸烷氧基烷基酯共聚物、丙烯腈-乙烯基卤共聚物或丙烯腈-甲基丙烯酸烷基酯-丁二烯三元共聚物。
所述聚合物优选是衍生自以下物质的聚合物:不饱和醇和胺或它们的酰基衍生物或缩醛,例如聚乙烯醇,聚乙酸乙烯酯,聚硬脂酸乙烯酯,聚苯甲酸乙烯酯或聚马来酸乙烯酯,聚乙烯醇缩丁醛,聚邻苯二甲酸烯丙酯,聚烯丙基三聚氰胺;以及它们与烯烃的共聚物。
所述聚合物优选是环状醚的均聚物和共聚物,例如聚亚烷基二醇、聚环氧乙烷、聚环氧丙烷或它们与双缩水甘油基醚的共聚物。
所述聚合物优选是聚缩醛,例如聚甲醛,以及包含共聚单体的聚甲醛,所述共聚单体例如环氧乙烷;用热塑性聚氨酯、丙烯酸酯或MBS改性的聚缩醛。
所述聚合物优选是聚苯醚和聚苯硫醚以及它们与苯乙烯聚合物或聚酰胺的混合物。
所述聚合物优选是衍生自以下物质的聚氨酯:聚醚、聚酯和聚丁二烯,其既具有末端羟基基团又具有脂族或芳族多异氰酸酯,以及它们的前体。
所述聚合物优选是衍生自二胺和二羧酸和/或衍生自氨基羧酸或相应内酰胺的聚酰胺和共聚酰胺,例如尼龙-2/12、尼龙-4、尼龙-4/6、尼龙-6、尼龙-6/6、尼龙-6/9、尼龙-6/10、尼龙-6/12、尼龙-6/66、尼龙-7、尼龙-7,7、尼龙-8、尼龙-8,8、尼龙-9、尼龙-9,9、尼龙-10、尼龙-10,9、尼龙-10,10、尼龙-11、尼龙-12、基于间二甲苯、二胺和己二酸的芳族聚酰胺;由六亚甲基二胺和间苯二甲酸和/或对苯二甲酸制备的聚酰胺(聚六亚甲基间苯二甲酰胺、聚六亚甲基对苯二甲酰胺)和非必要的弹性体作为改性剂,例如聚-2,4,4-三甲基六亚甲基对苯二甲酰亚胺或聚间苯二甲酰间苯二胺。上述聚酰胺与以下物质的嵌段共聚物:聚烯烃、烯烃共聚物、离聚物或化学键合或接枝的弹性体;或聚醚,例如聚乙二醇、聚丙二醇或聚丁二醇。此外,EPDM-或ABS-改性的聚酰胺或共聚酰胺;以及在加工过程中缩合的聚酰胺(“RIM聚酰胺体系”)。
所述聚合物优选是聚脲、聚酰亚胺、聚酰胺酰亚胺、聚醚酰亚胺、聚酯酰亚胺、聚乙内酰脲和聚苯并咪唑。
所述聚合物优选是衍生自以下物质的聚酯:二羧酸和二醇,和/或羟基羧酸,或相应的内酯,例如聚对苯二甲酸乙二醇酯,聚对苯二甲酸丁二醇酯,聚-1,4-二羟甲基环己烷对苯二甲酸酯,聚羟基苯甲酸酯,以及衍生自具有羟基端基的聚醚的嵌段聚醚酯;还有用聚碳酸酯或MBS改性的聚酯。
所述聚合物优选是聚碳酸酯和聚酯碳酸酯。
所述聚合物优选是聚砜、聚醚砜和聚醚酮。
所述聚合物优选是经交联的聚合物,其一方面衍生自醛和另一方面衍生自酚、脲或三聚氰胺,例如酚-甲醛、脲-甲醛和三聚氰胺-甲醛树脂。
所述聚合物优选是干性(drying)和非干性醇酸树脂。
所述聚合物优选是不饱和聚酯树脂,其衍生自饱和的和不饱和的二羧酸与多元醇以及作为交联剂的乙烯基化合物形成的共聚酯,以及它们的卤化阻燃变型物。
所述聚合物优选是可交联的丙烯酸系树脂,其衍生自取代的丙烯酸系酯,例如衍生自环氧丙烯酸酯、氨基甲酸酯丙烯酸酯或聚酯丙烯酸酯。
所述聚合物优选是已经与三聚氰胺树脂、脲-甲醛树脂、异氰酸酯、异氰脲酸酯、聚异氰酸酯或环氧树脂交联的醇酸树脂、聚酯树脂和丙烯酸酯树脂。
所述聚合物优选是经交联的环氧树脂,其衍生自脂族的、环脂族的、杂环的或芳族的缩水甘油基化合物,例如以下物质的产物:双酚A二缩水甘油基醚、双酚F二缩水甘油基醚,它们在有或没有加速剂的情况下借助于常规硬化剂进行交联,所述常规硬化剂例如酸酐或胺。
所述聚合物优选是上述聚合物的混合物(聚合物共混物),例如PP/EPDM(聚丙烯/乙烯-丙烯-二烯橡胶)、聚酰胺/EPDM或ABS(聚酰胺/乙烯-丙烯-二烯橡胶或丙烯腈-丁二烯-苯乙烯),PVC/EVA(聚氯乙烯/乙烯-乙酸乙烯酯),PVC/ABS(聚氯乙烯/丙烯腈-丁二烯-苯乙烯),PVC/MBS(聚氯乙烯/甲基丙烯酸酯-丁二烯-苯乙烯),PC/ABS(聚碳酸酯/丙烯腈-丁二烯-苯乙烯),PBTP/ABS(聚对苯二甲酸丁二醇酯/丙烯腈-丁二烯-苯乙烯),PC/ASA(聚碳酸酯/丙烯酸系酯-苯乙烯-丙烯腈),PC/PBT(聚碳酸酯/聚对苯二甲酸丁二醇酯),PVC/CPE(聚氯乙烯/氯化聚乙烯),PVC/丙烯酸酯(聚氯乙烯/丙烯酸酯),POM/热塑性PUR(聚甲醛/热塑性聚氨酯),PC/热塑性PUR(聚碳酸酯/热塑性聚氨酯),POM/丙烯酸酯(聚甲醛/丙烯酸酯),POM/MBS(聚甲醛/甲基丙烯酸酯-丁二烯-苯乙烯),PPO/HIPS(聚苯醚/高冲击性聚苯乙烯),PPO/PA 6,6(聚苯醚/尼龙6,6)和共聚物,PA/HDPE(聚酰胺/高密度聚乙烯),PA/PP(聚酰胺/聚乙烯),PA/PPO(聚酰胺/聚苯醚),PBT/PC/ABS(聚对苯二甲酸丁二醇酯/聚碳酸酯/丙烯腈-丁二烯-苯乙烯)和/或PBT/PET/PC(聚对苯二甲酸丁二醇酯/聚对苯二甲酸乙二醇酯/聚碳酸酯)。
根据本发明的混合物也可以相应地在纺织品之中或之上使用,而不损害其性能。
根据本发明的混合物可以以随机分布的方式或以特定图案,例如以点图案,施加到柔性材料,尤其是纺织品材料上。这样的纺织品例如用于酒店、剧院和会议中心的内部装修中,以及用于交通工具(公共汽车、火车、小汽车、飞机等)中。
根据本发明的混合物可以与其它阻燃剂一起使用,如例如在Chemie-Lexikon,第9版(1996),第1369至1371页中的“Flammschutzmittel(阻燃剂)”下所描述的。
总的来说,根据本发明的混合物,单独地或与其它物质一起作用,可以具有促进碳化、灭火、形成阻挡层、形成绝缘层或一些其它种类的作用。
对于在聚合物(尤其是聚烯烃)之中和之上的,以及在以下物质中或用于以下物质的所有上述应用,所述物质为形成绝缘层膨胀型涂料和纺织品,可以添加另外的添加剂,尤其是抗氧化剂、抗静电剂、发泡剂、另外的阻燃剂、热稳定剂、抗冲改性剂、加工助剂、润滑剂、光稳定剂、抗滴落剂、增容剂、增强剂、填料、成核剂、用于激光标记的添加剂、水解稳定剂、增链剂、颜料和/或增塑剂。
所述膨胀型配制剂—然后用作防火涂料—按如下方式制备:
a)最初在室温下加入所述溶剂或溶剂混合物,并在搅拌的同时将相应的树脂溶解在其中,然后在搅拌的同时添加涂料添加剂,例如分散添加剂和非必要的消泡剂,
b)在低速下搅拌的同时撒入泡沫形成物质、发泡剂和碳形成物质,以及助剂和添加剂(例如二氧化钛、纤维和填料),
c)在搅拌下撒入触变剂,
d)在保持50℃至60℃温度的同时,用高剪切力进行分散至少25分钟,
e)进行均匀分散至少5分钟,和通过添加溶剂或溶剂混合物建立所需的粘度。
这些配制剂可例如在根据本发明的用于制备形成绝缘层阻燃涂料的方法中使用。在这种情况下,将有机硅树脂乳液(粘结剂)与在火灾时形成泡沫的试剂以及非必要的其它助剂和添加剂在高剪切溶解器中混合,并调节至所需的粘稠度。
本发明的涂料组合物可以直接地或通过底漆涂层施加到待涂覆的表面上。所述涂料组合物通常在-10至60℃的温度下以液体形式施加。例如,可以通过无空气喷涂、浇铸(在模具中使用)、涂覆或抹平来实现所述施加。
根据本发明的涂料组合物可以被施加到多种基材上。本发明优选钢和铝基材,以及复合材料,例如玻璃纤维增强的塑料。
具体实施方式
本发明在以下实施例中进行了非限制性的阐述。
首先,通过将从表1中公开的量的晶相II聚磷酸铵与相应量的晶相I聚磷酸铵在滚动混合机(得自Heidolph)中以320转/分钟(rpm)混合5小时来制备聚磷酸铵的混合物。
在实施例1中使用纯晶相II聚磷酸铵。
在实施例11中使用纯晶相I聚磷酸铵。
由此获得的混合物显示出在表1中再现的性能。
上述值按如下方式测定:
粘度
为了测定粘度,在25℃下在水中制备得自实施例1至11的相应产物的10重量%悬浮液并将其搅拌。粘度是借助布氏(Brookfield)粘度计根据DIN ISO 2555(转子61,100rpm)测定的。
电导率
为了测定pH,在25℃下在水中制备得自实施例1至11的相应产物的10重量%悬浮液并将其搅拌5分钟。电导率是通过电位测定法(得自Knick,型号703电导计)测定的。
pH
为了测定pH,在25℃下在水中制备得自实施例1至11的相应产物的10重量%悬浮液并将其搅拌5分钟。pH是借助于电位测定法(Metrohm,LL Aquatrode Plus WOC)测定的。
酸值
为了测定酸值,在25℃下在水中制备得自实施例1至11的相应产物的10重量%悬浮液并将其搅拌5分钟。酸值是根据ISO 2114测定的。
水溶解度
在25℃下在水中制备聚磷酸氨或其混合物的10重量%悬浮液,并将其搅拌和过滤。基于所用量的滤液干燥残渣(10%悬浮液)对应于这种聚磷酸铵的水溶解度。
质量损失
质量损失可以多种方式表示:
1)2%质量损失的温度(℃)
2)300℃下的质量损失,以%表示
借助得自Sartorius的MA35M-230N仪器通过热重分析法在氮气气氛下测定质量损失。
所述阻燃混合物的堆密度是根据EN ISO;DIN 53468在25℃下测定的。
粒度d50是借助Malvern Mastersizer测定的。
从表1中的实施例1至11明显看出,其中所述产物的一些性能受到将相I聚磷酸铵添加到相II聚磷酸铵中的不利影响。例如,溶解度增加到大于3%,并且电导率显著增加。作为另一个缺点,当在所述混合物中的相I聚磷酸铵含量增加时,酸值会升高到大于5mg KOH/g,并且热稳定性会降低。
当在暴露于风化或其它外部影响的区域中使用相应的涂料时,水分的作用可能导致聚磷酸铵的浸出,该聚磷酸铵不再可用于膨胀反应。预期这会导致膨胀作用的降低。出于这个原因,使所述APP的溶解度保持是低的是有成效的。
与短链(聚)磷酸铵的溶解度相关的溶液中升高的盐浓度尤其可以通过电导率的测定来说明。
此外,在具有水性粘结剂的膨胀型体系的储存过程中,高盐负荷通过破坏分散稳定性可能导致不希望的缩短的储存稳定性,表现为不可逆的粘度增加。
例如,在将实施例1、4和6并入到在WO2017153227A1中描述的膨胀型配制剂中的情况下,观察到良好的相容性。
通过与使用纯的相II APP(实施例1)相比,在实施例4和6的情况下,24小时后不可能检测到最终产物中的粘度有任何增加。不可能观察到已经用晶相混合物(实施例4和6)制备的膨胀型涂料的阻燃时间(干燥层厚度为2000μm)有任何增加。泡沫特性额外还表现出轻微的不均匀性和降低的稳定性。尤其是在施加相对高的层厚度的情况下,这可能导致泡沫在耐火试验(fire test)过程中发生脱离。
相反,如果将本发明的混合物在基于溶剂的膨胀型涂料中使用,则会观察到绝缘作用的明显提高。
使用得自实施例1和4的产物制备实施例12和13的基于溶液的膨胀型配制剂。
实施例12
使用得自实施例1的聚磷酸铵制备具有以下组成的膨胀型配制剂:
28重量份的得自实施例1的聚磷酸铵,
10重量份的树脂(Omnova,Ultra 100),
8重量份的三聚氰胺(OCI,),
8重量份的季戊四醇(Perstorp,PT 40),
9重量份的二氧化钛(Cristal,696),
6重量份的氯化石蜡(chloroparaffin)(Dover Chemicals,NP70),
和100重量份的增稠剂(VP 031),助剂和添加剂(二乙二醇丁醚醋酸酯(butyldiglycol acetate,BDGA),/>),分散添加剂,漆添加剂,溶剂(100/140,二甲苯)。
实施例13
过程如实施例12中那样,不同的是,使用的不是28重量份的得自实施例1的聚磷酸铵,而是28重量份的得自实施例4的由相II聚磷酸铵(85重量%)和相I聚磷酸铵(15重量%)形成的混合物。
实施例12和13中的各自的膨胀型配制剂按如下方式制备:
a)最初在室温下加入溶剂,并在搅拌的同时添加漆添加剂(得自BYK的-2163)、分散助剂和非必要的消泡剂,
b)将得自实施例1或4的各自混合物、发泡剂、碳源、二氧化钛、填料在低速下搅拌的同时撒入,接着是触变剂,
c)将所述混合物在保持30至70℃温度的同时用高剪切力分散20至60分钟,并然后通过在低剪切力下添加溶剂来建立所需的粘度。
将由此制备的膨胀型配制剂作为膨胀型涂料施加到经涂覆的钢板(S235JRno.1.0122,符合标准EN 10025-2:2004;尺寸:280×280×5mm)上,并类似于DIN 4102第8部分,耐火曲线ISO 834进行耐火试验,其中干燥膜厚度为2000μm。图1显示了所述板的背面的温度随时间变化的进程。
本发明已经发现,令人惊奇地,在使用得自实施例4的混合物的情况下,在所述板的背面上的温度达到T临界=500℃的时间为109分钟,其与得自实施例1的纯物质的100分钟相比,是明显更高的。这意味着,在根据本发明的用途的情况下,钢材的临界软化温度仅在较晚的时刻达到,并且因此保护作用更有效。钢结构的结构完整性因此可以保持更长时间。
因此,这是9%的性能增益。在实施例1的情况下,在背面上达到仅300℃的温度需要花32分钟,而在实施例4的情况下需要花48分钟;这意味着火灾保护时间增加了50%。
如果,如图2中所示的,绘制实施例12和13的钢材背面上温度的温差随时间的变化,可以发现实施例13的绝缘效果在整个火灾进程中都更高。在约27分钟的时间后观察到45℃的最大温差。
在得自实施例12和13的本发明的混合物的情况下,与实施例1相比,尤其是在较低温度下已经发生起始反应,因此绝缘作用更早(更快)开始,并且用根据本发明的膨胀型配制剂涂覆的基材可以被更好地热绝缘。当所描述的系统在结构钢构造中使用时,这可以实现寿命更长和/或更有效的防火系统。由于更长的阻燃时间,建筑物的居民在发生火灾时可以有更长的时间离开,并且消防员能够在安全环境中灭火。
考虑到较早开始的绝缘作用,根据本发明的膨胀型配制剂现在可用于使迄今为止由于其低熔点而不能防热的基材具有阻燃性。例如,还可以保护甚至在低温(例如300℃)下也会软化或释放可燃和/或有毒的热解气体的聚合物和其它基材。
从另一个角度来看,根据本发明的膨胀型配制剂的优点也是显而易见的:
例如,在实施例1(对比例)中仅17分钟后基材温度就达到250℃,而在本发明实施例4中直到29分钟才达到该温度。因此,根据本发明的膨胀型涂料在合适的温度范围内的有效性几乎是纯相II聚磷酸铵的两倍。
因此,在通常具有300℃或更低的熔点或分解温度的基于非金属的基材(例如热塑性塑料)的情况下,可以非常有效地防止火灾蔓延。这里的实际实例是,诸如屋顶板、隔墙等的结构材料板,或者复合材料,其是在极端环境(电池罩或加压储氢设施)中使用的。
由使用根据本发明的混合物导致的在较低温度下较高的阻燃时间有利地导致材料节省;同样还可以施加较低的层厚度以实现相同的效果。
在相对低的温度范围内,在250℃,性能提升百分比为71%。
因此,本发明的不同晶相的聚磷酸铵的混合物非常适合用于制备更快速发挥作用的膨胀型涂料,其另外还具有提高的材料效率。
将基于实施例1和4的实施例12和13的膨胀型涂料施加于由各种塑料制成的板材料上,并根据DIN 4102第8部分,耐火曲线ISO 834进行耐火试验,其中干燥膜厚度为2000μm。
实施例14
施加于A3K(BASF;根据ISO 11357的熔融温度:260℃):
采用实施例12的膨胀型配制剂,仅21分钟后就达到所述聚合物的260℃的临界软化温度,但采用得自实施例13的本发明的膨胀型配制剂,只有在35分钟后才达到所述温度。由此可见,当使用根据本发明的膨胀型配制剂时,阻燃时间延长了67%。
实施例15
施加于2205聚碳酸酯板(Covestro;根据ISO 11357的熔融温度:300℃):
采用实施例12的膨胀型配制剂,仅37分钟后就达到所述聚合物的300℃的临界软化温度,但采用得自实施例13的本发明的膨胀型配制剂,只有在58分钟后才达到所述温度。由此可见,当使用根据本发明的膨胀型配制剂时,阻燃时间延长了57%。
实施例16
施加于内部制备的填充了玻璃纤维的复合板(DICY-固化的双酚A环氧树脂):
采用实施例12的膨胀型配制剂,仅62分钟后就达到所述基材的320℃的临界分解温度,但采用得自实施例13的本发明的膨胀型配制剂,只有在74分钟后才达到所述温度。由此可见,当使用根据本发明的膨胀型配制剂时,阻燃时间延长了19%。
实施例17
施加于铝板
采用实施例12的膨胀型配制剂,仅62分钟后就达到所述基材的320℃的临界软化温度,但采用得自实施例13的本发明的膨胀型配制剂,只有在74分钟后才达到所述温度。由此可见,当使用根据本发明的膨胀型配制剂时,阻燃时间延长了19%。
得自本发明实施例4的混合物还用于使用以下树脂制备基于溶剂的膨胀型配制剂(表3):
实施例18:苯乙烯-丙烯酸酯共聚物——Ultra100(Omnova/Synthomer)
实施例19:甲基丙烯酸酯共聚物——TB 080(Evonik)
实施例20:甲基丙烯酸酯——LP 65/11(Evonik)/>
实施例21:苯乙烯-丙烯酸酯共聚物——AC 80(Omnova/Synthomer)
实施例22:甲基丙烯酸酯——SC 124/50WS(Allnex)
实施例23:甲基丙烯酸酯——LP 63/11(Evonik)
表3:具有各种树脂的基于溶剂的膨胀型配制剂
1使用实施例7
表3描述了根据本发明的阻燃剂混合物的灵活性。尽管在一些情况下,在最高至500℃都没有观察到FRT的延长,但更早的激活表现为横穿所述板的开始反应更早开始。
此外,在所有实验中,都保持了与表面粘附、膨胀、均匀性和孔尺寸有关的优选泡沫性能。
在此已经发现,与得自实施例1的混合物相比,得自实施例4的本发明混合物在根据本发明的相应膨胀型配制剂中在每种情况下都导致达到临界温度的时间更长。
因此,由相II聚磷酸铵与相I聚磷酸铵形成的本发明混合物非常适合于制备有效的膨胀型配制剂。
Claims (18)
1.组合物,其包含:
作为组分(A)的0.1重量%至99.9重量%的相II聚磷酸铵,和
作为组分(B)的0.1重量%至99.9重量%的相I和/或相III、IV、V和/或VI聚磷酸铵,其中所述组分的总和为100重量%。
2.根据权利要求1所述的组合物,其包含:
60重量%至99.9重量%的组分A,和
0.1重量%至40重量%的组分B。
3.根据权利要求1或2所述的组合物,其包含:
75重量%至92重量%的组分A和8重量%至35重量%的组分B。
4.根据权利要求1至3中至少一项所述的组合物,其特征在于,组分A是相II聚磷酸铵,和组分B是相I聚磷酸铵。
5.根据权利要求1至4中至少一项所述的组合物,其特征在于,组分A是具有式(NH4)n+ 2PnO3n+1的相II聚磷酸铵,其中n=300至100000。
6.根据权利要求1至5中至少一项所述的组合物,其特征在于,组分A是具有式(NH4)n+ 2PnO3n+1的相II聚磷酸铵,其中n=1000至25000。
7.根据权利要求1至6中至少一项所述的组合物,其特征在于,组分B是具有式(NH4)n+ 2PnO3n+1的相I聚磷酸铵,其中n=5至100。
8.根据权利要求1至7中至少一项所述的组合物,其特征在于,它们具有:
—小于0.5%的根据ISO 760的残留水分含量(水含量),
—0.3至0.9g/cm3的堆密度,
—小于1.5%的水溶解度(25℃下10%的水中悬浮液),
—小于40mPas的粘度(Brookfield DV3T,速度50rpm,转子1),
—5至50μm的粒度d50,其是通过激光衍射测量的,
—10至60μm的粒度d90,其是通过激光衍射测量的,和
—4至8的pH(25℃下10%的水中悬浮液)。
9.根据权利要求1至8中至少一项所述的组合物,其特征在于,所述聚磷酸氨已经用以下物质微胶囊化:有机官能(聚)硅烷,(聚)硅氧烷,(聚)硅氮烷,改性蜡,聚氨酯,聚环氧化物,脲-甲醛树脂,三聚氰胺-甲醛树脂,基于(甲基)丙烯酸酯树脂、基于苯乙烯/丙烯酸酯共聚物、氨基甲酸酯、基于乙烯/乙酸壬酯共聚物、基于橡胶的乳液和/或它们的混合物。
10.根据权利要求1至9中至少一项所述的组合物,其特征在于,它们额外还包含基于组分(A)和(B)的量计最高至10重量%的硫酸铵、硫酸三乙铵、硫酸四甲铵、硫酸三甲铵、硫酸二甲酯、硫酸二乙酯、硫酸二丙酯、辛基硫酸钠、癸基硫酸钠、十八烷基硫酸钠、硫酸月桂酯、硫酸脲、硫酸三聚氰胺、硫酸羟胺、硫酸肼、硫酸钾、硫酸氢钾、硫酸钠、硫酸氢钠、硫酸镁、硫酸氢镁、硫酸钙、硫酸氢钙、硫酸钡、硫酸铝钾、硫酸铝、硫酸铁(III)、硫酸铁(II)、硫酸钴、硫酸钛、硫酸锌、硫酸锡、硫酸铈、硫酸锂、三甲基锍甲基硫酸盐或它们的混合物。
11.根据权利要求1至10中至少一项所述的组合物用于降低膨胀型涂料的起始反应温度,用于提高膨胀型涂料的阻燃能力,用作透明涂料和膨胀型涂料的阻燃剂,用于或用作木材和其它纤维素产品的阻燃剂,用于或用作聚合物、凝胶涂层、不饱和聚酯树脂的反应性和/或非反应性阻燃剂,用于制备阻燃聚合物模塑配混料,用于制备阻燃聚合物模制件,用于通过浸渍使聚酯以及纯的和混纺的纤维素织物具有阻燃性,用于聚氨酯泡沫,用于聚烯烃,用于不饱和聚酯和酚醛树脂以及用于使纺织品具有阻燃性的用途。
12.根据权利要求1至10中至少一项所述的组合物在以下物质中或用于以下物质的用途:插塞式连接器、电力分配器中的载流组件(剩余电流保护)、电路板、灌封料、电源连接器、断路器、灯罩、LED灯罩、电容器罩、线圈元件、通风设备、接地触点、插头,在以下物质中/上的用途:印刷电路板、用于插头的罩、电池罩、电缆、柔性电路板、充电电缆、电机盖、纺织品涂层和其它产品。
13.根据权利要求1至10中至少一项所述的组合物用于在钢材、木材、木基材料、纸、矿物棉、石膏板、塑料、金属、合金、由合成或天然纤维制成的织物和其它合适材料上的阻燃涂料和/或用作阻焊层以及用于电气开关和电路的用途。
14.根据权利要求1至10中至少一项所述的组合物用于涂覆钢构造、天花板、墙壁、电缆、管道、导管、电缆和组合舱壁、门、帘、烟道栅栏、百叶窗、安全柜、安装柜和其它制品的用途,所述钢构造例如钢梁和钢支架。
15.阻燃涂料,其包含成膜粘结剂、发泡剂、作为泡沫形成物质的根据权利要求1至10中一项或多项所述的组合物、碳形成物质、助剂和添加剂以及非必要的增稠剂、分散添加剂和溶剂和/或溶剂混合物。
16.根据权利要求15所述阻燃涂料,其包含:
5重量%至69.4重量%的成膜粘结剂,
5重量%至25重量%的发泡剂,
5重量%至40重量%的作为泡沫形成物质的根据权利要求1至10中一项或多项所述的组合物,
5重量%至25重量%的碳形成物质,
5重量%至40重量%的助剂和添加剂,
0.5重量%至10重量%的增稠剂,
0.1重量%至10重量%的分散添加剂,和
10重量%至40重量%的溶剂和/或溶剂混合物,其中所述组分总和为100重量%。
17.根据权利要求15或16所述的阻燃涂料,其特征在于,
所述成膜粘结剂包含基于苯乙烯和丙烯酸系酯的共聚物,基于丙烯酸系酯的共聚物,乙烯基甲苯/丙烯酸酯共聚物,苯乙烯/丙烯酸酯聚合物,基于乙酸乙烯酯的均聚物,基于乙酸乙烯酯、乙烯和氯乙烯的共聚物,基于乙酸乙烯酯和长链支化羧酸的乙烯基酯的共聚物,基于乙酸乙烯酯和马来酸二正丁酯和/或丙烯酸系酯的共聚物,乙烯基/丙烯酸酯共聚物,自交联聚氨酯分散体,萜烯和/或聚萜烯和/或它们的混合物;
所述发泡剂是三聚氰胺,三聚氰胺-甲醛缩合物,胍,它们的盐,三聚氰胺缩合产物和/或双氰胺;
所述碳形成物质是淀粉,改性淀粉,多元醇(多羟基化合物),例如糖类和多糖,和/或热塑性或热固性聚合物树脂粘结剂,例如酚醛树脂,脲醛树脂,聚氨酯,聚氯乙烯,聚(甲基)丙烯酸酯,聚乙酸乙烯酯,聚乙烯醇,有机硅树脂和/或橡胶;
所述助剂和添加剂是玻璃纤维,矿物纤维,金属纤维,碳纤维,高岭土,滑石,氧化铝,氢氧化铝,氢氧化镁和其它金属氧化物,沉淀二氧化硅,硅酸盐和/或粉状的纤维素;
所述增稠剂和/或流变学添加剂是(改性的)纤维素,二氧化硅,膨润土,蓖麻油衍生物,脂肪衍生物,聚酰胺,聚(甲基)丙烯酸酯,聚丙烯酰胺,聚醚,聚氨酯,聚乙烯醇,聚乙烯基吡咯烷酮,糖聚合物,例如阿拉伯树胶,藻酸盐,黄原胶和/或琼脂;
所述润湿和分散添加剂是烷基酚乙氧基化物,聚丙烯酸和/或聚氨酯;
所述有机溶剂和/或溶剂混合物是芳族烃,优选二甲苯和/或烷基苯,
优选甲苯和乙苯;醇,优选甲醇,和/或链烷醇,优选2-甲基-1-丙醇;酮,例如丙酮或丁酮,链烷酸酯和/或聚醚,优选聚二醇醚。
18.根据权利要求15至17中一项或多项所述的阻燃涂料,其特征在于,所述多羟基化合物是三季戊四醇和/或季戊四醇的缩聚物和/或基于季戊四醇的酯与多羟基化合物、聚乙酸乙烯酯、聚乙烯醇、山梨糖醇和/或环氧乙烷-环氧丙烷多羟基化合物的混合物。
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