CN117242131A - 热塑性聚合物的阻燃剂-稳定剂组合物 - Google Patents
热塑性聚合物的阻燃剂-稳定剂组合物 Download PDFInfo
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- CN117242131A CN117242131A CN202280030520.XA CN202280030520A CN117242131A CN 117242131 A CN117242131 A CN 117242131A CN 202280030520 A CN202280030520 A CN 202280030520A CN 117242131 A CN117242131 A CN 117242131A
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Classifications
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Abstract
本发明涉及阻燃剂‑稳定剂混合物,包含以重量计5%至50%的二乙基次膦酸铝(DEPAL)或二乙基次膦酸锌(DEPZN)作为组分A,以重量计5%至50%的式(I)的钛次膦酸盐和/或钛氧次膦酸盐(DEPTI)作为组分B,其中x是0‑1.9、优选1‑1.05的数,其意味着Ti与二乙基次膦酸盐之比为1.9‑2,以重量计0%至10%的式(II)和(III)的亚磷酸铝或亚磷酸锌作为组分C[HP(=O)O2]2‑Zn2+(II)[HP(=O)O2]2‑ 3Al3+ 2(III)以重量计0%至30%的含氮增效剂和/或含磷和/或含氮阻燃剂作为组分D,以重量计0%至70%的填料和增强剂作为组分E,以重量计0%至3%的有机亚膦酸酯/盐或有机亚磷酸酯/盐和与酚类抗氧化剂的混合物作为组分F,和以重量计0%至3%的通常具有C14‑C40的链长度的长链脂族羧酸(脂肪酸)的酯和/或盐作为组分G,其中组分的总和总是以重量计100%。
Description
本发明涉及使用含钛的次膦酸盐阻燃剂的用于不含卤素的热塑性聚合物的新型阻燃剂组合物,并涉及包含这样的阻燃剂组合物的聚合物模塑配混物和模塑件。
可燃烧的塑料通常必须配备有阻燃剂以便能够达到由塑料加工者并在一些情况下由立法者制定的高阻燃性要求。优选地—也出于环境原因—使用形成仅少量烟气(如果有的话)的非卤化阻燃剂体系。
在这些阻燃剂中,已经发现烷基次膦酸的盐(次膦酸盐)对于热塑性聚合物特别有效(DE-2252258A和DE-2447727A)。最初描述了主要涉及碱金属次膦酸盐并要求保护它们在聚酯模塑配混物(DE-A-2 252 258)和聚酰胺(DE-A-2 447 727)中的阻燃作用。兴趣之后特别集中在锌盐(US-A-4,180,495、US-A-4,208,321)和最近集中在钙和铝次膦酸盐(EP-A-0699 708、DE-A-196 07 635),因为这些被认为是最合适的该类型的阻燃剂。
另外,已经发现次膦酸盐与特定的含氮化合物的协同组合物,并且已经发现这些组合物在许多情况下具有比单独的次膦酸盐更好的作为阻燃剂的功效(WO 97/39053,以及DE-A-197 34 437和DE-A-197 37727)。
虽然在聚合物树脂中使用阻燃剂可明显降低可燃性,但是这可导致当聚合物树脂暴露于热或火焰时烟的高散出。应避免烟的这种散出,因为它可导致严重损坏以及中毒,从而导致死亡。次膦酸盐是非常有效的阻燃剂,尤其是对于聚酰胺和聚酯而言,但是次膦酸盐和与分子中的磷原子连接的烷基基团的气相活性通常导致增加的烟形成。
令人惊讶地,现在已经发现钛次膦酸盐和钛氧次膦酸盐,与铝次膦酸盐或锌次膦酸盐组合,并任选与亚磷酸铝或亚磷酸锌和另外的增效剂和添加剂组合,在热塑性聚合物中具有特别好的阻燃作用并因非常低的烟气密度而出名。
钛次膦酸盐和钛氧次膦酸盐的使用在EP 1 479 718 B1中描述。强调了钛次膦酸盐和钛氧次膦酸盐的特别好的阻燃作用。在玻璃纤维增强的PBT和PA 66中,使用20%DEPTI或10%DEPTI和10%三聚氰胺氰尿酸盐实现了UL 94 V-0燃烧等级。没有描述烟气密度和烟气毒性。
本发明因此提供阻燃剂-稳定剂混合物,包含:
以重量计5%至95%的二乙基次膦酸铝(DEPAL)和/或二乙基次膦酸锌(DEPZN)作为组分A,
以重量计5%至95%的式(I)的钛次膦酸盐和/或钛氧次膦酸盐(DEPTI)作为组分B,
其中x是0-1.9的数,
以重量计0%至10%的式(II)和(III)的亚磷酸铝或亚磷酸锌作为组分C,
[HP(=O)O2]2-Zn2+ (II)
[HP(=O)O2]2- 3Al3+ 2 (III)
以重量计0%至30%的含氮增效剂和/或含磷和/或含氮阻燃剂作为组分D,
以重量计0%至70%的填料和增强剂作为组分E,
以重量计0%至3%的有机亚膦酸酯/盐和/或有机亚磷酸酯/盐和/或与酚类抗氧化剂的混合物作为组分F,
以重量计0%至3%的通常具有C14-C40的链长度的长链脂族羧酸(脂肪酸)的酯和/或盐作为组分G,其中组分的总和总是以重量计100%。
根据本发明的阻燃剂-稳定剂组合物优选包含:
以重量计5%至95%的组分A,
以重量计5%至95%的组分B,
以重量计0%至10%的组分C,
以重量计0%至20%的组分D,
以重量计20%至60%的组分E,
以重量计0%至3%的组分F,和
以重量计0%至2%的组分G,
其中组分的总和总是以重量计100%。
根据本发明的阻燃剂-稳定剂组合物更优选包含:
以重量计5%至95%的组分A,
以重量计5%至95%的组分B,
以重量计0%至10%的组分C,
以重量计0%至20%的组分D,
以重量计20%至60%的组分E,
以重量计0%至3%的组分F,和
以重量计0%至2%的组分G,
其中组分的总和总是以重量计100%。
根据本发明的阻燃剂-稳定剂组合物尤其包含:
以重量计10%至69%的组分A,
以重量计10%至69%的组分B,
以重量计1%至20%的组分C,
以重量计0%至30%的组分D,
以重量计20%至50%的组分E,
以重量计0%至3%的组分F,和
以重量计0%至2%的组分G,
其中组分的总和总是以重量计100%。
还优选根据本发明的阻燃剂-稳定剂组合物包含:
以重量计10%至67.8%的组分A,
以重量计10%至40%的组分B,
以重量计1%至10%的组分C,
以重量计2%至20%的组分D,
以重量计20%至60%的组分E,
以重量计0.1%至3%的组分F,和
以重量计0.1%至2%的组分G,
其中组分的总和总是以重量计100%。
在优选实施方案中,根据本发明的阻燃剂-稳定剂组合物包含:
以重量计10%至68.8%的组分A,
以重量计10%至40%的组分B,
以重量计20%至50%的组分E,
以重量计0.1%至3%的组分F,和
以重量计0.1%至2%的组分G,
其中组分的总和总是以重量计100%。
在另一优选实施方案中,根据本发明的阻燃剂-稳定剂组合物包含:
以重量计10%至68.9%的组分A,
以重量计10%至40%的组分B,
以重量计1%至30%的组分D,
以重量计20%至50%的组分E和
以重量计0.1%至2%的组分G,
其中组分的总和总是以重量计100%。
在另外优选实施方案中,根据本发明的阻燃剂-稳定剂组合物包含:
以重量计10%至69%的组分A,
以重量计10%至40%的组分B,
以重量计1%至20%的组分C,
以重量计0%至30%的组分D,和
以重量计20%至50%的组分E,
其中组分的总和总是以重量计100%。
式(I)中的X优选为1至1.05,使得Ti与二乙基次膦酸盐之比为1.9-2。
组分C优选是亚磷酸锌、仲亚磷酸锌(secondary zincphosphi te)(ZnHPO3)、Zn(H2PO3)2、Zn2/3HPO3、亚磷酸锌水合物、焦亚磷酸锌(ZnH2P2O5)、下式的碱式亚磷酸锌
Zn1+xHPO3(OH)2x
其中x=0至0.25和/或下式的亚磷酸锌钠
Zn1-xNa2xHPO4其中x=0.001至0.5。
组分C更优选是具有CAS号14332-59-3、114332-59-3、1431544-62-5、14902-88-6、52385-12-3和51728-08-6的磷酸的锌盐(这里也称作锌亚磷酸盐)。
组分C优选包含亚磷酸铝[Al(H2PO3)3]、仲亚磷酸铝[Al2(HPO3)3]、碱式亚磷酸铝[Al(OH)(H2PO3)2*2aq]、四水合亚磷酸铝[Al2(HPO3)3*4aq]、膦酸铝、Al7(HPO3)9(OH)6(己-1,6-二胺)1.5*12H2O、Al2(HPO3)3*xAl2O3*nH2O其中x=2.27-1和/或Al4H6P16O18,和式(IV)、(V)和/或(VI)的铝亚磷酸盐,其中
Al2(HPO3)3x(H2O)q (IV)
其中
q是0至4,
Al2.00Mz(HPO3)y(OH)v x(H2O)w (V)
其中
M表示碱金属离子
z是0.01至1.5
y是2.63至3.5
v是0至2,和
w是0至4,
Al2.00(HPO3)u(H2PO3)t x(H2O)s (VI)
其中
u是2至2.99,
t是2至0.01,和
s是0至4,
和/或包含式(IV)的亚磷酸铝与微溶的铝盐和不含氮的外来离子的混合物,式(VI)的亚磷酸铝与以下铝盐的混合物:亚磷酸铝[Al(H2PO3)3]、仲亚磷酸铝[Al2(HPO3)3]、碱式亚磷酸铝[Al(OH)(H2PO3)2*2aq]、四水合亚磷酸铝[Al2(HPO3)3*4aq]、膦酸铝、Al7(HPO3)9(OH)6(己-1,6-二胺)1.5*12H2O、Al2(HPO3)3*xAl2O3*nH2O其中x=2.27-1和/或Al4H6P16O18。
本发明还涵盖根据权利要求1至12中的一项或多项的阻燃剂-稳定剂组合物的用途:作为阻燃剂,在用于清漆和膨胀型涂料的阻燃剂中或作为用于清漆和膨胀型涂料的阻燃剂,在木材和其他纤维素产品的阻燃剂中或作为木材和其他纤维素产品的阻燃剂,在聚合物的反应性和/或非反应性阻燃剂中或作为聚合物的反应性和/或非反应性阻燃剂,用于阻燃聚合物模塑配混物的生产,用于阻燃聚合物模塑件的生产和/或通过浸渍使聚酯和纯的和共混的纤维素织物阻燃,和/或作为增效剂和/或作为另外阻燃剂混合物中的增效剂。
本发明还涉及阻燃热塑性或热固性聚合物模塑配混物或聚合物模塑件、膜、纤丝和/或纤维,其包含以重量计2%至50%的根据权利要求1至9中的一项或多项的阻燃剂-稳定剂组合物、以重量计50%至98%的热塑性或热固性聚合物或它们的混合物、以重量计0%至50%的添加剂和以重量计0%至60%的填料或增强材料,其中组分的总和为以重量计100%。
优选阻燃热塑性或热固性聚合物模塑配混物或聚合物模塑件、膜、纤丝和/或纤维,其包含以重量计7%至30%的根据权利要求1至12中的一项或多项的阻燃剂-稳定剂组合物、以重量计30%至92%的热塑性或热固性聚合物或它们的混合物、以重量计1%至30%的添加剂和以重量计0%至40%的填料或增强材料,其中组分的总和为以重量计100%。
优选阻燃热塑性或热固性聚合物模塑配混物或聚合物模塑件、膜、纤丝和/或纤维,其包含根据权利要求1至11中的一项或多项的阻燃剂混合物,特征在于聚合物包含以下热塑性聚合物:HI(高抗冲)聚苯乙烯、聚苯醚、聚酰胺、聚酯或聚碳酸酯类型,和ABS(丙烯腈-丁二烯-苯乙烯)或PC/ABS(聚碳酸酯/丙烯腈-丁二烯-苯乙烯)或PPE/HIPS(聚苯醚/HI聚苯乙烯)聚合物类型的共混物或聚合物共混物。
包含根据权利要求1至12中的一项或多项的阻燃剂混合物的阻燃热塑性或热固性聚合物模塑配混物或聚合物模塑件、膜、纤丝和/或纤维中的聚合物尤其是尼龙-6或尼龙-6,6类型的热塑性聚合物、半芳族聚酰胺和聚对苯二甲酸丁二醇酯(PBT)、聚对苯二甲酸亚环己基二甲酯(PCT)和/或聚对苯二甲酸乙二醇酯(PET)类型的聚酯。
添加剂优选是抗氧化剂、UV吸收剂、光稳定剂、金属钝化剂、破坏过氧化物的化合物、聚酰胺稳定剂、碱式助稳定剂、成核剂、另外的阻燃剂和/或其他添加剂。
组分E优选包含填料和增强剂例如碳酸钙、硅酸盐、玻璃纤维、石棉、滑石、高岭土、云母、硫酸钡、金属氧化物和氢氧化物、炭黑、石墨和/或其他合适的物质。
根据权利要求14至19中的一项或多项的阻燃热塑性或热固性聚合物模塑配混物或聚合物模塑件、膜、纤丝和/或纤维优选使用在以下中或用于以下:插头连接器、电力分配器中的电流承载部件(剩余电流保护)、电路板、封装配混物、电源连接器、断路器、灯罩、LED灯罩、电容器壳、线圈元件、通风装置、接地触点、插头、印刷电路板中/上、插头壳、电缆、柔性电路板、充电电缆、引擎盖、织物涂料和其他产品。
优选合适的组分C是具有CAS号119103-85-4、220689-59-8、56287-23-1、156024-71-4、71449-76-8和15099-32-8的铝亚磷酸盐。
特别优选具有CAS号[CAS 56287-23-1]的铝亚磷酸盐。
优选合适的组分C也是具有以下组成的铝亚磷酸盐和铝氢氧化物的混合物:以重量计5-95%的Al2(HPO3)3*nH2O和以重量计95-5%的Al(OH)3、更优选以重量计10-90%的Al2(HPO3)3*nH2O和以重量计90-10%的Al(OH)3、最优选以重量计35-65%的Al2(HPO3)3*nH2O和以重量计65-35%的Al(OH)3,并且在每种情况下n=0至4。
前述铝亚磷酸盐优选具有0.2至100μm的粒度。
组分D优选包含三聚氰胺的缩合产物和/或三聚氰胺与聚磷酸的反应产物和/或三聚氰胺的缩合产物与聚磷酸的反应产物或它们的混合物;和/或三聚氰胺氰尿酸盐。
组分D更优选包含蜜勒胺、蜜白胺、密隆(melon)、二(三聚氰胺)焦磷酸盐、三聚氰胺多磷酸盐、蜜勒胺多磷酸盐、蜜白胺多磷酸盐、密隆多磷酸盐和/或它们的混合多盐。
特别优选使用200(来自BASF,D)三聚氰胺多磷酸盐(称作MPP)、MC50(来自BASF,D)三聚氰胺氰尿酸盐(称作MC)、/>20(来自DelaminLtd.,UK)蜜勒胺和其他产品作为组分D。
填料和增强剂(组分E)优选是碳酸钙、硅酸盐、玻璃纤维、硅灰石、滑石、高岭土、云母、硫酸钡、金属氧化物和氢氧化物、炭黑、石墨和/或其他合适的物质。
组分E更优选包含玻璃纤维。
合适的组分F例如是对于尼龙-6,6而言168//>1098 1:1和对于PBT而言/>626//>1076 1:1的混合物。
合适的组分G例如是来自Clar iant Produkte(德国)GmbH的CaV102(褐煤蜡酸的Ca盐)。
作为组分F成分的合适的抗氧化剂的实例是烷基化的单酚,例如2,6-二叔丁基-4-甲基苯酚;1.2烷基硫代甲基苯酚,例如2,4-二辛基硫代甲基-6-叔丁基苯酚;氢醌和烷基化氢醌,例如2,6-二叔丁基-4-甲氧基苯酚;生育酚,例如α-生育酚、β-生育酚、γ-生育酚、δ-生育酚和它们的混合物(维生素E);羟基化硫代二苯醚,例如2,2'-硫代双(6-叔丁基-4-甲基苯酚)、2,2'-硫代双(4-辛基苯酚)、4,4'-硫代双(6-叔丁基-3-甲基苯酚)、4,4'-硫代双(6-叔丁基-2-甲基苯酚)、4,4'-硫代双(3,6-二仲戊基苯酚)、4,4'-双(2,6-二甲基-4-羟基苯基)二硫化物;烷叉基双酚,例如2,2'-甲叉基双(6-叔丁基-4-甲基苯酚);
O-、N-和S-苄基化合物,例如3,5,3',5'-四叔丁基-4,4'-二羟基二苄基醚;羟基苄基化丙二酸酯,例如2,2-双(3,5-二叔丁基-2-羟基苄基)丙二酸二(十八烷基酯);羟基苄基芳族化合物,例如1,3,5-三(3,5-二叔丁基)-4-羟基苄基)-2,4,6-三甲基苯、1,4-双(3,5-二叔丁基-4-羟基苄基)-2,3,5,6-四甲基苯、2,4,6-三(3,5-二叔丁基-4-羟基苄基)苯酚;三嗪化合物,例如2,4-双辛基巯基-6-(3,5-二叔丁基-4-羟基苯胺基)-1,3,5-三嗪;苄基膦酸酯,例如2,5-二叔丁基-4-羟基苄基膦酸二甲酯;酰氨基苯酚、4-羟基月桂酰胺、4-羟基硬脂酰苯胺、N-(3,5-二叔丁基-4-羟基苯基)氨基甲酸辛酯;β-(3,5-二叔丁基-4-羟基苯基)丙酸与一元醇或多元醇的酯;β-(5-叔丁基-4-羟基-3-甲基苯基)丙酸与一元醇或多元醇的酯;β-(3,5-二环己基-4-羟基苯基)丙酸与一元醇或多元醇的酯;3,5-二叔丁基-4-羟基苯基乙酸与一元醇或多元醇的酯;β-(3,5-二叔丁基-4-羟基苯基)丙酸的酰胺,例如N,N'-双(3,5-二叔丁基-4-羟基苯基丙酰基)六亚甲基二胺、N,N'-双(3,5-二叔丁基-4-羟基苯基丙酰基)三亚甲基二胺、N,N'-双(3,5-二叔丁基-4-羟基苯基丙酰基)肼。
作为另外添加剂的合适的UV吸收剂和光稳定剂的实例是2-(2'-羟基苯基)苯并三唑,例如2-(2'-羟基-5'-甲基苯基)苯并三唑;2-羟基苯甲酮,例如4-羟基,4-甲氧基,4-辛氧基,4-癸氧基,4-十二烷氧基,4-苄氧基,4,2',4-三羟基,2'-羟基-4,4'-二甲氧基衍生物;任选取代的苯甲酸的酯,例如水杨酸4-叔丁基苯酯、水杨酸苯酯、水杨酸辛基苯酯、二苯甲酰基间苯二酚、双(4-叔丁基苯甲酰基)间苯二酚、苯甲酰基间苯二酚、3,5-二叔丁基-4-羟基苯甲酸2,4-二叔丁基苯酯、3,5-二叔丁基-4-羟基苯甲酸十六烷酯、3,5-二叔丁基-4-羟基苯甲酸十八烷酯、3,5-二叔丁基-4-羟基苯甲酸2-甲基-4,6-二叔丁基苯酯;丙烯酸酯,例如α-氰基-β,β-二苯基丙烯酸乙酯或异辛酯,α-甲酯基肉桂酸甲酯,α-氰基-β-甲基-对-甲氧基肉桂酸甲酯或丁酯,α-甲酯基-对甲氧基肉桂酸甲酯,N-(β-甲酯基-β-氰基乙烯基)-2-甲基二氢吲哚。
合适的聚酰胺稳定剂的实例是铜盐组合有碘化物和/或磷化合物,和二价锰的盐。
合适的碱性助稳定剂是三聚氰胺、聚乙烯吡咯烷酮、双氰胺、氰脲酸三烯丙酯、尿素衍生物、肼衍生物、胺、聚酰胺、聚氨酯、高级脂肪酸的碱金属和碱土金属盐,例如硬脂酸钙、硬脂酸锌、山嵛酸镁、硬脂酸镁、蓖麻酸钠、棕榈酸钾、儿茶酚锑或儿茶酚锡。
合适的成核剂的实例是4-叔丁基苯甲酸、己二酸和二苯乙酸。
合适的另外的阻燃剂是例如磷酸芳基酯、有机膦酸酯/盐、次磷酸的盐和红磷。
其他添加的物质的实例包括增塑剂、可膨胀石墨、乳化剂、颜料、光学增白剂、阻燃剂、抗静电剂、起泡剂。
可以在各种不同的方法步骤中将上述添加剂引入聚合物。例如,在聚酰胺或聚酯的情况下,可以在聚合/缩聚的开始时或结束时或在随后的配混操作中将添加剂混合至聚合物熔体中。另外,存在直至后来阶段才添加添加剂的加工操作。这尤其当使用颜料或添加剂母料时实施。还可以施加添加剂(特别是以粉末形式)至聚合物粒料,其由于通过转鼓施加干燥操作可以是温热的。
阻燃剂-稳定剂组合物优选处于粒料、薄片、细粒、粉末和/或微粉形式。
阻燃剂-稳定剂组合物优选处于固体的物理混合物、熔融混合物、压制品(compactate)、挤出物的形式,或母料的形式。
阻燃剂-稳定剂组合物优选具有0.1-50μm的平均粒度。
混合物中的DEPAL和DEPTi优选具有≤50μm、更优选≤25μm的粒度D50(体积%,借助于Malvern Mas ters izer 2000粒度分析仪器中的激光衍射在丙酮中测量)。
本发明还提供包含根据本发明的阻燃剂混合物的热塑性或热固性聚合物的模塑配混物。
可例如以以下方式制备亚磷酸锌:
在2h内向8763.6g的七水合硫酸锌和736.2g的脱盐水的初始装料中添加5235.8g的亚磷酸氢二钠溶液(39.3%),并然后添加370g的脱盐水。将所得亚磷酸锌在150℃下结晶5h。随后,排出淤浆并在吸滤器中使用五倍的脱盐水质量过滤三次,并在130℃下在干燥橱中干燥滤饼。这产生2096g的产物(97%收率)。
锌亚磷酸盐优选具有0.1至100μm和更优选0.1至30μm的粒度。
聚合物更优选包含聚酰胺和/或聚酯。
合适的聚酯衍生自二羧酸和它们的酯和二元醇和/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-1,3-二醇和丁-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(2500、/>2002,来自Celanese;/>来自BASF)、聚对苯二甲酸-1,4-二羟甲基环己酯、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。
合适的聚苯乙烯是聚苯乙烯、聚(对甲基苯乙烯)和/或聚(α-甲基苯乙烯)。
聚合物优选是聚酰胺和共聚酰胺,其衍生自二胺和二羧酸和/或衍生自氨基羧酸或相应的内酯,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-7,7、尼龙-8,8、尼龙-9,9、尼龙-10,9、尼龙-10,10、尼龙-11、尼龙-12等。这些已知为例如商品名(来自DuPont)、/>(来自BASF)、K122(来自DSM)、/>7301(来自DuPont)、/>B 29(来自Bayer)和/>(来自EmsChemie)。
还合适的是由间二甲苯、二胺和己二酸得到的芳族聚酰胺;由六亚甲基二胺和间-和/或对苯二甲酸制备的聚酰胺和任选的作为改性剂的弹性体,例如聚对苯二甲酰-2,4,4-三甲基己二胺或聚间苯二甲酰间苯二胺;前述聚酰胺与聚烯烃、烯烃共聚物、离聚物或化学结合或接枝弹性体的嵌段共聚物;或与聚醚,例如与聚乙二醇、聚丙二醇或聚丁二醇的嵌段共聚物。另外,EPDM-或ABS-改性聚酰胺或共聚酰胺;和在加工过程中缩合的聚酰胺(“RIM聚酰胺体系”)。
聚合物优选是热塑性弹性体。
热塑性弹性体(缩写:TPE)是可热塑性加工并具有橡胶状使用性质的材料。
可非常容易地成型热塑性弹性体,因为它们在加工过程中经历塑性状态。它们可以5肖氏A至大于70肖氏D的所有硬度生产。
热塑性弹性体在部分范围内具有物理交联点,所述物理交联点随加热而分解,而没有大分子的分解。因此,它们比正常弹性体具有好得多的加工性。因此,也可再次熔融并进一步加工聚合物废料。根据内部结构,在嵌段共聚物和弹性体合金之间进行区分。
嵌段共聚物在一个分子内具有硬链段和软链段。该聚合物因此由一种类型的分子组成,在该分子中分布两种性质。
弹性体合金是聚合共混物,即成品聚合物的混合物(共混物),即该聚合物由两种或更多种分子类型组成。通过不同的混合比和添加剂,获得调整的材料(例如由聚丙烯(PP)和天然橡胶(NR)形成的聚烯烃弹性体-根据比率,它们覆盖宽的硬度范围)。
在以下组中进行区分:
-TPE-O或TPO=基于烯烃的热塑性弹性体,主要是PP/EPDM,例如(AES/Monsanto)
-TPE-V或TPV=交联的基于烯烃的热塑性弹性体,主要是PP/EPDM,例如(DSM)
-TPE-U或TPU=基于氨基甲酸酯的热塑性弹性体,例如(Bayer)
-TPE-E或TPC=热塑性共聚酯
-TPE-S或TPS=苯乙烯嵌段共聚物(SBS、SEBS、SEPS、SEEPS和MBS),例如(Kuraray)或/>(Kra iburg TPE)
-TPE-A或TPA=热塑性共聚酰胺例如(Arkema)
特别优选的热塑性弹性体是热塑性共聚酯和热塑性共聚酰胺。
适合于根据本发明的组合物的共聚醚酯是通过使C2-C6二元醇与芳族二酸单元和聚(氧化亚烷基)二元醇反应来制备的聚合物。
特别优选的共聚醚酯选自:
1.丁二醇、对苯二甲酸酯和PTMEG(聚四亚甲基醚二醇)的共聚醚酯;
2.丁二醇、对苯二甲酸酯和间苯二酸酯的混合物和PTMEG的共聚醚酯;
3.丁二醇、对苯二甲酸酯和聚(氧化亚乙基)二醇的共聚醚酯;
4.丙二醇、对苯二甲酸酯和PTMEG的共聚醚酯;和
5.丙二醇、对苯二甲酸酯和聚(氧化亚乙基)二醇的共聚醚酯。
特别优选丁二醇、对苯二甲酸酯和PTMEG的共聚醚酯。
本发明最后还涉及生产阻燃聚合物成型体的方法,特征在于通过在升高的温度下注塑(例如Aarburg Al lrounder型号的注塑机)和压制、泡沫注塑、内部气压注塑、吹塑、膜流延、压延、层合或涂覆来加工本发明阻燃聚合物模塑配混物以产生阻燃聚合物成型体。
根据本发明的组合物实现低可燃性和减小烟散出的良好组合。
可根据测试标准ISO 5659在NBS烟箱中进行烟密度测试。试样生产为具有75mm×75mm的面积和2mm的厚度的片材。试样水平安装在箱中并在它们的顶侧通过冷却器锥和热流计暴露于25kW/m2的恒定热流,并在点火火焰的存在下持续约40min的时段。在箱中收集随着时间推移形成的烟,并使用包含6.5V白炽灯、光电倍增管和高精度光检测器的测光系统来测量穿过烟的光束的衰减。结果测量为随着时间的透明度并报道为比光密度Ds。其与透明度成反比例并对于对应于成型样品厚度的特定路径长度进行报道。烟的散出报道为最大比光密度Ds,max。记录测试期间发生的从板测试试样的每次滴落。低的Ds,max值是期望的并表明材料在火灾的情况下以较小的程度损害视力,并因此能够使人员从狭小空间快速逃离。没有烟时,透明度为100%且Ds为0。
1.使用的组分
热塑性聚合物
聚对苯二甲酸丁二醇酯(PBT):4500BASF
尼龙-6,6:A27,BASF
尼龙-6T/6,6:Arlen 3000,Mi tsui
热塑性共聚酯:包含聚氧化四亚甲基和聚苯二甲酸丁二醇酯作为聚酯嵌段链段的共聚醚酯弹性体
组分A:
二乙基次膦酸的铝盐,下文称作DEPAL
二乙基次膦酸的锌盐,下文称作DEPZN
组分B:
二乙基次膦酸的钛盐,下文称作DEPTI
DEPTI如EP 1 479 718B1中描述由二乙基次膦酸和钛酸正丁酯根据实施例1制备。
组分C:
亚磷酸铝,下文称作PHOPAL,和如以上所述制备的亚磷酸锌,下文称作PHOPZN
组分D:
MC 50(三聚氰胺氰尿酸盐),来自BASF,称作MC
200/70(三聚氰胺多磷酸盐=MPP),BASF,称作MPP
20(蜜勒胺),Delamin,UK,称作蜜勒胺
组分E:
PPG HP 3610EC 10 4.5mm玻璃纤维,用于聚酰胺
PPG HP 3786EC 10 4.5mm玻璃纤维,用于PBT,两者均来自NipponElectr icGlass,NL
组分F:
1010(季戊四醇四(3-(3,5-二叔丁基-4-羟苯基)丙酸酯),来自BASF,称作空间位阻酚
1330(3,3',3',5,5',5'-六-叔丁基-a,a',a'-(均三甲苯-2,4,6-三基)三对甲酚),来自BASF,称作空间位阻酚
245(亚乙基双(氧亚乙基)双(3-(5-叔丁基-4-羟基-间甲苯基)丙酸酯),称作空间位阻酚
组分G:
润滑剂:E,褐煤蜡,来自Clariant,CH
2.阻燃聚酯和聚酰胺配混物的生产、加工和测试
将阻燃剂组分与聚合物粒料和任何添加剂以表中规定的比率混合并在双螺杆挤出机(Leistritz ZSE 27/HP-44D)中在240至280℃的温度下并入。抽出均化的聚合物股线,在水浴中冷却并然后造粒。
在充分干燥之后,在注塑机(Arburg 320C/KT)中在260至280℃的熔融温度下加工模塑配混物从而产生测试试样。通过方法UL94V(Underwriters Laboratories Inc.安全标准,"Test for Flammability of Plastic Materials for Parts in Devices andAppliances",第14页至第18页,Northbrook 1998)测试模塑配混物的阻燃性。
通过UL 94垂直测试进行防火测试。UL 94防火等级如下:
V-0:续燃时间不超过10秒,10次火焰施加的总续燃时间不大于50秒,没有燃烧滴落,试样没有完全消耗,在火焰施加结束之后试样的续灼时间不超过30秒
V-1:在火焰施加结束之后续燃时间不超过30秒,10次火焰施加的总续燃时间不大于250秒,在火焰施加结束之后试样的续灼时间不超过60秒,其他标准与V-0相同
V-2:燃烧滴落引燃棉花指示剂,其他标准与V-1相同
无法分类(n.c.):不符合防火等级V-2。
实施例报道了5个测试试样的10次火焰施加的续燃时间。
D烟密度
根据标准ISO 5659在来自Fire Testing Technologies,UK的NBS烟箱中测定光学烟气密度。试样通过注塑生产,具有75mm×75mm的尺寸和2mm的厚度。试样水平夹紧并用25kW/m2在引燃火焰的存在下照射40min。使用光检测器来测量光束通过烟的衰减。烟气密度与光的衰减成反比例。
使用Z 010拉伸测试仪(来自Zwick)根据DIN EN ISO 527-1/-2/-3来测定拉伸性质。使用该方法以便检查测试试样的拉伸变形特性并确定拉伸强度、拉伸模量和固定条件下拉伸应力/应变关系的其他特征。测试试样优选通过注塑生产。测试试样数由样品制备需要的测试决定,测试试样储存在23℃/50%相对湿度下气候控制室中至少16h。聚酰胺测试试样和其他强吸水测试试样必须储存在气密密封袋中。
通过在275℃/2.16kg下确定熔体体积流动速率(MVR)来测定模塑配混物的流动性。MVR值的迅速升高表明聚合物降解。
表1:PBT GF 30:V1-V3是比较例;B1至B6是本发明实施例
表1显示特别地DepAl或DepZn和DepTi的组合甚至以10%阻燃剂的用量达到了UL94 V-0防火等级。另外,DepAl和DepTi的组合实现了低的烟气密度Ds。
表2:尼龙-6,6 GF 30
V5 | V6 | V7 | V8 | B7 | B8 | B9 | B10 | B11 | B12 | |
PA 66 | 57.7 | 49.7 | 54.7 | 49.7 | 54.7 | 54.7 | 54.7 | 54.7 | 54.7 | 54.7 |
玻璃纤维 | 30 | 30 | 30 | 30 | 30 | 30 | 30 | 30 | 30 | 30 |
DepAl | 12 | 20 | 5 | 7.5 | 10 | 5 | 7.5 | |||
DepTi | 15 | 20 | 10 | 7.5 | 5 | 10 | 5 | 2.5 | ||
MPP | 5 | 5 | 5 | |||||||
Licowax E | 0.3 | 0.3 | 0.3 | 0.3 | 0.3 | 0.3 | 0.3 | 0.3 | 0.3 | 0.3 |
UL 94 1.6mm | n.c. | n.c. | V-1 | V-0 | V-0 | V-0 | V-1 | V-1 | V-0 | V-0 |
AFT/s | 165 | 123 | 67 | 33 | 12 | 15 | 54 | 55 | 39 | 32 |
表2显示DepAl和DepTi的组合甚至以15%阻燃剂的用量实现了UL 94 V-0防火等级;组合有MPP时,同样仅需要15%阻燃剂。
表3:尼龙-6T/66 GF 30
表3显示DepAl和DepTi的组合甚至以10%阻燃剂的用量实现了UL 94 V-0防火等级;组合有蜜勒胺时,仅需要12%阻燃剂。
表4显示添加磷酸锌和亚磷酸铝如何降低尼龙-6,6与二乙基次膦酸铝和二乙基次膦酸钛的烟气密度。只有使用二乙基次膦酸铝和二乙基次膦酸钛连同PHOPZN和/或PHOPAL才实现了UL 94 V-0防火等级连同低的烟气密度。
表4:PA 6,6 GF 30测试结果。V12-V14是比较例;B17至B20是根据本发明的阻燃剂-稳定剂混合物
V12 | V13 | V14 | B17 | B18 | B19 | B20 | |
尼龙-6,6 | 50 | 50 | 50 | 55 | 55 | 55 | 55 |
3610玻璃纤维 | 30 | 30 | 30 | 30 | 30 | 30 | 30 |
DEPAL | 13 | 15 | 7.5 | 7 | 7 | 5 | |
DRPTI | 20 | 7.5 | 7 | 7 | 5 | ||
PHOPAL | 5 | 1 | 1 | ||||
PHOPZN | 1 | ||||||
MPP | 7 | 5 | |||||
UL 94 0.8mm | V-0 | V-0 | V-0 | V-0 | V-0 | V-0 | V-0 |
烟气密度 | 高 | 高 | 高 | 平均 | 低 | 低 | 低 |
表5:PA 6,6 GF 30测试结果。V2至V4是比较例;B12至B15是根据本发明的阻燃剂-稳定剂混合物
表5显示其中使用基于二乙基次膦酸铝与MPP和PHOPZN的阻燃剂-稳定剂组合物的比较例V15和V16。
使用根据本发明的阻燃剂-稳定剂混合物的结果列于实施例B21至B24。所有的量报道为以重量%计并以包括阻燃剂-稳定剂组合物和添加剂的聚合物模塑配混物为基础。
表6显示热塑性共聚酯中的结果。仅Depa l与Dept i和亚磷酸盐的本发明组合可实现与低的烟气密度Ds,max同时相结合的高LOI。
表6:热塑性聚酯共聚物(TPE-E)。V17-V19是比较例;B25至B28是根据本发明的阻燃剂-稳定剂混合物
从实施例B21-B24明显可见,具有二乙基次膦酸铝和二乙基次膦酸钛组分以及PHOPZN和/或PHOPAL和任选的MPP的根据本发明的混合物实现了UL 94 V-0防火等级、低的MVR(很少聚合物降解)和低的光学烟气密度。
此外,具有根据本发明的阻燃剂-稳定剂组合物的聚酰胺具有良好的熔体稳定性、高的抗冲击性和拉伸强度、良好的热老化性质、低的渗出和600V或更高的CTI值。
Claims (20)
1.阻燃剂-稳定剂混合物,包含:
以重量计5%至95%的二乙基次膦酸铝(DEPAL)和/或二乙基次膦酸锌(DEPZN)作为组分A,
以重量计5%至95%的式(I)的钛次膦酸盐和/或钛氧次膦酸盐(DEPTI)作为组分B
其中x是0-1.9的数,
以重量计0%至10%的式(II)和(III)的亚磷酸铝或亚磷酸锌作为组分C,
[HP(=O)O2]2-Zn 2+(II)
[HP(=O)O2]2- 3Al 3+ 2(III)
以重量计0%至30%的含氮增效剂和/或含磷和/或含氮阻燃剂作为组分D,
以重量计0%至70%的填料和增强剂作为组分E,
以重量计0%至3%的有机亚膦酸酯/盐和/或有机亚磷酸酯/盐和/或与酚类抗氧化剂的混合物作为组分F,和
以重量计0%至3%的通常具有C14-C40的链长度的长链脂族羧酸(脂肪酸)的酯和/或盐作为组分G,其中组分的总和总是以重量计100%。
2.根据权利要求1所述的阻燃剂-稳定剂组合物,特征在于它包含:
以重量计5%至95%的组分A,
以重量计5%至95%的组分B,
以重量计0%至10%的组分C,
以重量计0%至20%的组分D,
以重量计20%至60%的组分E,
以重量计0%至3%的组分F,和
以重量计0%至2%的组分G,
其中组分的总和总是以重量计100%。
3.根据权利要求1所述的阻燃剂-稳定剂组合物,特征在于它包含:以重量计10%至69%的组分A,
以重量计10%至69%的组分B,
以重量计1%至20%的组分C,
以重量计0%至30%的组分D,
以重量计20%至50%的组分E,
以重量计0%至3%的组分F,和
以重量计0%至2%的组分G,
其中组分的总和总是以重量计100%。
4.根据权利要求1所述的阻燃剂-稳定剂组合物,特征在于它包含:以重量计10%至67.8%的组分A,
以重量计10%至40%的组分B,
以重量计1%至10%的组分C,
以重量计2%至20%的组分D,
以重量计20%至60%的组分E,
以重量计0.1%至3%的组分F,和
以重量计0.1%至2%的组分G,
其中组分的总和总是以重量计100%。
5.根据权利要求1所述的阻燃剂-稳定剂组合物,特征在于它包含:以重量计10%至68.8%的组分A,
以重量计10%至40%的组分B,
以重量计20%至50%的组分E,
以重量计0.1%至3%的组分F,和
以重量计0.1%至2%的组分G,
其中组分的总和总是以重量计100%。
6.根据权利要求1或2所述的阻燃剂-稳定剂组合物,特征在于它包含
以重量计10%至68.9%的组分A,
以重量计10%至40%的组分B,
以重量计1%至30%的组分D,
以重量计20%至50%的组分E,和
以重量计0.1%至2%的组分G,
其中组分的总和总是以重量计100%。
7.根据权利要求1或2所述的阻燃剂-稳定剂组合物,特征在于它包含:
以重量计10%至69%的组分A,
以重量计10%至40%的组分B,
以重量计1%至20%的组分C,
以重量计0%至30%的组分D,和
以重量计20%至50%的组分E,
其中组分的总和总是以重量计100%。
8.根据权利要求1至7中一项或多项所述的阻燃剂-稳定剂组合物,特征在于式(I)中的x为1至1.05。
9.根据权利要求1至8中一项或多项所述的阻燃剂-稳定剂组合物,特征在于组分C包含亚磷酸锌、仲亚磷酸锌(ZnHPO3)、Zn(H2PO3)2、Zn2/3HPO3、亚磷酸锌水合物、焦亚磷酸锌(ZnH2P2O5)、式Zn1+xHPO3(OH)2x的碱式亚磷酸锌,其中x=0至0.25和/或式Zn1-xNa2xHPO4的亚磷酸锌钠,其中x=0.001至0.5。
10.根据权利要求1至9中一项或多项所述的阻燃剂-稳定剂组合物,特征在于组分C包含亚磷酸铝[Al(H2PO3)3]、仲亚磷酸铝[Al2(HPO3)3]、碱式亚磷酸铝[Al(OH)(H2PO3)2*2aq]、四水合亚磷酸铝[Al2(HPO3)3*4aq]、膦酸铝、Al7(HPO3)9(OH)6(己-1,6-二胺)1.5*12H2O、Al2(HPO3)3*xAl2O3*nH2O其中x=2.27-1和/或Al4H6P16O18,并包含式(IV)、(V)和/或(VI)的铝亚磷酸盐
Al2(HPO3)3x(H2O)q(IV)
其中
q是0至4,
Al2.00Mz(HPO3)y(OH)v x(H2O)w(V)
其中
M表示碱金属离子
z是0.01至1.5
y是2.63至3.5
v是0至2,和
w是0至4,
Al2.00(HPO3)u(H2PO3)t x(H2O)s(VI)
其中
u是2至2.99,
t是2至0.01,和
s是0至4,
和/或包含式(IV)的铝亚磷酸盐与微溶的铝盐和不含氮的外来离子的混合物,式(VI)的铝亚磷酸盐与以下铝盐的混合物:亚磷酸铝[Al(H2PO3)3]、仲亚磷酸铝[Al2(HPO3)3]、碱式亚磷酸铝[Al(OH)(H2PO3)2*2aq]、四水合亚磷酸铝[Al2(HPO3)3*4aq]、膦酸铝、Al7(HPO3)9(OH)6(己-1,6-二胺)1.5*12H2O、Al2(HPO3)3*xAl2O3*nH2O其中x=2.27-1和/或Al4H6P16O18。
11.根据权利要求1至10中一项或多项所述的阻燃剂-稳定剂组合物,特征在于组分D包含三聚氰胺的缩合产物和/或三聚氰胺与聚磷酸的反应产物和/或三聚氰胺的缩合产物与聚磷酸的反应产物或它们的混合物;和/或三聚氰胺氰尿酸盐。
12.根据权利要求11所述的阻燃剂-稳定剂组合物,其中组分D包含蜜勒胺、蜜白胺、密隆、二(三聚氰胺)焦磷酸盐、三聚氰胺多磷酸盐、蜜勒胺多磷酸盐、蜜白胺多磷酸盐、密隆多磷酸盐和/或它们的混合多盐。
13.根据权利要求1至12中的一项或多项的阻燃剂-稳定剂组合物的用途:作为阻燃剂,在用于清漆和膨胀型涂料的阻燃剂中或作为用于清漆和膨胀型涂料的阻燃剂,在木材和其他纤维素产品的阻燃剂中或作为木材和其他纤维素产品的阻燃剂,在聚合物的反应性和/或非反应性阻燃剂中或作为聚合物的反应性和/或非反应性阻燃剂,用于阻燃聚合物模塑配混物的生产,用于阻燃聚合物模塑件的生产和/或通过浸渍使聚酯和纯的和共混的纤维素织物阻燃,和/或作为增效剂和/或作为另外的阻燃剂混合物中的增效剂。
14.阻燃热塑性或热固性聚合物模塑配混物或聚合物模塑件、膜、纤丝和/或纤维,其包含以重量计2%至50%的根据权利要求1至9中的一项或多项的阻燃剂-稳定剂组合物、以重量计50%至98%的热塑性或热固性聚合物或它们的混合物、以重量计0%至50%的添加剂和以重量计0%至60%的填料或增强材料,其中组分的总和为以重量计100%。
15.阻燃热塑性或热固性聚合物模塑配混物或聚合物模塑件、膜、纤丝和/或纤维,其包含以重量计7%至30%的根据权利要求1至12中的一项或多项的阻燃剂-稳定剂组合物、以重量计30%至92%的热塑性或热固性聚合物或它们的混合物、以重量计1%至30%的添加剂和以重量计0%至40%的填料或增强材料,其中组分的总和为以重量计100%。
16.阻燃热塑性或热固性聚合物模塑配混物或聚合物模塑件、膜、纤丝和/或纤维,其包含根据权利要求1至11中的一项或多项的阻燃剂混合物,特征在于聚合物包含以下热塑性聚合物:HI(高抗冲)聚苯乙烯、聚苯醚、聚酰胺、聚酯或聚碳酸酯类型,和ABS(丙烯腈-丁二烯-苯乙烯)或PC/ABS(聚碳酸酯/丙烯腈-丁二烯-苯乙烯)或PPE/HIPS(聚苯醚/HI聚苯乙烯)聚合物类型的共混物或聚合物共混物。
17.阻燃热塑性或热固性聚合物模塑配混物或聚合物模塑件、膜、纤丝和/或纤维,其包含根据权利要求1至12中的一项或多项的阻燃剂混合物,特征在于聚合物包含尼龙-6或尼龙-6,6类型的热塑性聚合物、半芳族聚酰胺和聚对苯二甲酸丁二醇酯(PBT)、聚对苯二甲酸亚环己基二甲酯(PCT)和/或聚对苯二甲酸乙二醇酯(PET)类型的聚酯。
18.根据权利要求14至17中的一项或多项所述的阻燃热塑性或热固性聚合物模塑配混物或聚合物模塑件、膜、纤丝和/或纤维,特征在于添加剂是抗氧化剂、UV吸收剂、光稳定剂、金属钝化剂、破坏过氧化物的化合物、聚酰胺稳定剂、碱式助稳定剂、成核剂、另外的阻燃剂和/或其他添加剂。
19.根据权利要求14至18中的一项或多项所述的阻燃热塑性或热固性聚合物模塑配混物或聚合物模塑件、膜、纤丝和/或纤维,特征在于组分E包含填料和增强剂例如碳酸钙、硅酸盐、玻璃纤维、石棉、滑石、高岭土、云母、硫酸钡、金属氧化物和氢氧化物、炭黑、石墨和/或其他合适的物质。
20.根据权利要求14至19中的一项或多项所述的阻燃热塑性或热固性聚合物模塑配混物或聚合物模塑件、膜、纤丝和/或纤维在以下中或用于以下的用途:插头连接器、电力分配器中的电流承载部件(剩余电流保护)、电路板、封装配混物、电源连接器、断路器、灯罩、LED灯罩、电容器壳、线圈元件、通风装置、接地触点、插头、印刷电路板中/上、插头壳、电缆、柔性电路板、充电电缆、引擎盖、织物涂料和其他产品。
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EP21172633.6 | 2021-05-07 | ||
EP21172633.6A EP4086302A1 (en) | 2021-05-07 | 2021-05-07 | Flame retardant-stabilizer combination for thermoplastic polymers |
PCT/EP2022/060835 WO2022233619A1 (en) | 2021-05-07 | 2022-04-25 | Flame retardant-stabilizer combination for thermoplastic polymers |
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US (1) | US20240218160A1 (zh) |
EP (2) | EP4086302A1 (zh) |
JP (1) | JP7510019B2 (zh) |
KR (1) | KR20230172611A (zh) |
CN (1) | CN117242131A (zh) |
TW (1) | TW202244186A (zh) |
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- 2022-04-25 WO PCT/EP2022/060835 patent/WO2022233619A1/en active Application Filing
- 2022-04-25 KR KR1020237042479A patent/KR20230172611A/ko not_active Application Discontinuation
- 2022-04-25 CN CN202280030520.XA patent/CN117242131A/zh active Pending
- 2022-04-25 EP EP22725225.1A patent/EP4334385A1/en active Pending
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EP4086302A1 (en) | 2022-11-09 |
JP2024513441A (ja) | 2024-03-25 |
US20240218160A1 (en) | 2024-07-04 |
KR20230172611A (ko) | 2023-12-22 |
WO2022233619A1 (en) | 2022-11-10 |
EP4334385A1 (en) | 2024-03-13 |
TW202244186A (zh) | 2022-11-16 |
JP7510019B2 (ja) | 2024-07-02 |
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