CN1127550C - 阻燃的粘接组合物 - Google Patents
阻燃的粘接组合物 Download PDFInfo
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- C08L2666/28—Non-macromolecular organic substances
Abstract
一种基于乙烯/醋酸乙烯共聚物的热熔粘接组合物,以整个组合物的重量计,含有不多于35%(优选不多于30%,更优选不多于25%)的无卤素的烧结阻燃添加剂,其量至少足可以防止按照保险商实验室测试方法UL-94(1993)的20mm垂直燃烧试验,V-1,优选V-0的由吸收底棉点火造成的粘接剂试条燃烧时产生的火焰滴下。优选的不含有卤素的阻燃添加剂包括磷酸铵、氰尿酸三聚氰胺、硼酸锌和特别是红磷。
Description
本发明涉及阻燃的热熔粘接组合物,它可以用于尺寸可热恢复的制品,当该制品在使用时发生热恢复时,发生流动和产生密封。
在热收缩领域和其它领域中,基于非阻燃的乙烯/醋酸乙烯共聚物(EVA)或聚酰胺(PAm)的热熔粘接剂是已知的。在US-A-5,346,539中叙述了可热收缩管的内表面上使用的含有卤化有机添加剂的阻燃粘接剂。本发明通过提供更为环境所接受的用无卤素添加剂的阻燃组合物来改善这一点,尽管它在意外低的低添加剂水平方面就可以通过严格的可燃性测试的要求,而令人惊奇地是保持了所希望的热软化和热流动性能。
因此,本发明提供一种基于乙烯/醋酸乙烯共聚物(EVA)的热熔粘接组合物,以整个组合物的重量计,含有不多于35%(优选不多于30%,更优选不多于25%)的无卤素烧结(优选含磷的)阻燃添加剂,其量至少足可以防止按照保险商(Underwriters)实验室测试方法UL-94(1993)的20mm垂直燃烧试验,V-1,优选V-0的由吸收底棉点火造成的粘接剂试条燃烧时产生的火焰滴下。
按照本发明已经发现,EVA热熔体能够充分地被无卤素添加剂阻燃,最好是在没有另外的阻燃剂或增大触变性填料存在下,在与聚酰胺基的热熔体中相类似的添加剂含量下,这些添加剂意外地不能达到相同的所需效果。再有,聚酰胺倾向于比各EVA更昂贵。也已意外地发现,比较高的熔流指数(MFI)有助于EVA粘接剂通过上述的UL94要求。
规定的(优选含磷的)添加剂是无卤素的,除了可能的极少量的含卤杂质外,最好整个的粘接剂或腻子组合物基本是完全不含有卤素的。按照本发明的组合物最好是基本不含有细分散的二氧化硅、滑石粉或氧化铝填料的,是基本不含有细分散的增大触变性填料的。
在本发明的一个优选组合物中,阻燃添加剂含有磷酸铵,优选多磷酸铵,或者磷酸的有机胺盐,优选磷酸乙二胺。这种组合物优选含有至少20%、更优选25~35%、最优选25~30%(重量)的磷酸铵或磷酸的有机胺盐,优选没有其它的阻燃添加剂存在。
在本发明的另一个优选实施方案中,该组合物包括了上述多磷酸铵的增效剂,优选聚{[6-(4-吗啉基)-1,3,5-三嗪-2,4-二基]-1,4-哌嗪二基}(C11H16N6O)n。在此情况下,该组合物优选含有至少15%、更优选15~30%,最优选15~20%(重量)的结合的磷酸铵和增效剂,最好是没有其它的阻燃剂存在。
在本发明的一个特别优选的实施方案中,阻燃添加剂包括红磷。该组合物优选含有至少1%、更优选至少1.25%、最优选至少1.5%(重量)的红磷,最好是没有其它的阻燃添加剂存在。该组合物最好含有不多于10%、优选不多于5%、更优选不多于3%(重量)的红磷。红磷最好以大约50%(重量)的母料形式配合在与组合物的基础聚合物相容的载体聚合物中,所述聚合物最好是相同或相似的化学种类,或者最好是相同的聚合物,然后使用这种母料在最终组合物中提供适当的红磷水平。
作为含磷添加剂的发明替换物,阻燃添加剂可以包括比如硼酸锌或氰尿酸三聚氰胺酯。因此本发明可以包括(a)含有至少10%、优选10~25%、更优选10~20%、特别优选10~15%(整个组合物重量)的氰尿酸三聚氰胺酯作为阻燃添加剂,最好是不含有其它的阻燃添加剂的热熔体粘接组合物;或者(b)含有至少10%、优选10~25%、更优选15~20%、(整个组合物重量)的硼酸锌作为阻燃添加剂,最好是不含有其它的阻燃添加剂的热熔体粘接组合物。在此范围内的组合物,它们也优选是不含有卤素的,被发现能够通过按照UL94的最高性能水平的V-0级的前述的“火焰下滴”测试要求,同时对于在前述的可热恢复制品中使用时保持所需的流动特性。
意外地发现,这样的比较少量的无卤素阻燃添加剂能够使组合物满足前述的标准中的“火焰下滴”要求,这样低的添加剂比例在保持用于可热恢复制品时所需的流动特性和粘度特性方面是特别有利的。因此,本发明的组合物可以用于尺寸热恢复制品,阻燃添加剂的用量少于如下的数量,即在该数量下能防止组合物软化和/或流动以便所述的制品在使用时的正常热恢复条件下进行密封。热恢复(特别是热收缩)制品,比如管、“套”、“udders”、包卷片和模塑件是为人们充分了解的,在此无须进一步叙述。根据制造它们的聚合物材料不同,这些制品一般在从大约120℃(聚烯烃)至190℃(聚偏氟乙烯)的外表面温度恢复(收缩)。用在这些制品的内表面上的粘接组合物在正常的热恢复使用时倾向于经受比外表面低至少20℃的温度。
本发明使用的粘接级EVA优选含有至少16%,更优选含有至少20%,最优选含有至少25%(重量)的醋酸乙烯。此EVA的熔流指数(下面称为MFI),以g/10min为单位,在190℃下用2.16Kg的重量,按照ASTMD138(1979)的方法测试时,至少为100,特别优选为至少500。本发明的阻燃EVA热熔粘接组合物的MFI如上为至少50,优选至少100,更优选至少200,特别是至少300。
下面将更详细地叙述本发明的组合物的实施例。
热熔粘接剂的实施例
热熔粘接组合物按照如下的方法制备,所有的比例都是基于整个组合物的重量。阻燃添加剂单独与下面的共聚物当中的每一种[自杜邦(DuPont)公司购买的商品名为Elvax的共聚物]混合:MFI为550的Elvax4310乙烯/醋酸乙烯三元共聚物,醋酸乙烯(VA)含量289%,含有1~2%的甲基丙烯酸;Elvax 410 EVA(VA18%,MFI 500);Elvax 46 EVA(VA 46%,MFI 100)。其他聚合物组合物(E+N)是通过将Elvax 4310与2%的含有1,1-硫二萘酚的抗辐射材料和5%的已知的增粘树脂(商品名Nevpene 9500)在小亨谢尔(Henschel)混合器中混合,然后在ZSK双螺杆挤出机中混料,以已知的方式从挤出机中得到最终聚合物组合物的粒料。然后按下面表I中指出的比例,通过在室温下,在双辊混炼机上研磨这些聚合物原料中的每一种,以得到最终的阻燃组合物片,随后再用平板模压,切条,按照UL-94测试方法进行测试。
使用在EP-B-40926(B053)中叙述的那种聚酰胺热熔粘接剂(PAm)类似地制备其它的实施例,该专利的内容引入本文作为参考,它含有添加的乙烯/丙烯酸三元共聚物。在表中给出了对不同百分比重量的特定的阻燃添加剂的UL-94火焰滴下法的测试结果,该结果用在V-0级通过(P),或者未通过(Fl)表示。
实施例 | 添加剂 | Elvax 4310 | E410 | E46 | E+N | PAm | |||
1 | AmMC | 25/P | 20/P | 15/Fl | 10/Fl | 20/P | 20/P | 25/P | 30/Fl |
2 | Spinfl | 25/P | 20/P | 15/P | 10/Fl | - | - | 20/P | - |
3 | AmNL | 25/P | 20/P | 15/Fl | 10/Fl | - | - | - | - |
4 | ZnBort | 25/P | 20/P | 15/P | 10/Fl | 10/P | 20/Fl | 15/P | 20/Fl |
5 | Mel.cy | 25/P | 20/P | 15/P | 10/P | 10/P | 15/P | 10/P | 15/Fl |
6 | Novams | 9/P | 6/P | 2.4/P | 1.2/Fl | - | - | - | - |
7 | AmRYC | 10/P | 5/P | 2.5/P | 1.2/P | 5/P | 5/P | 1/P | 10/P |
添加剂如下,“TM”表示商品牌号:
AmMC:Amgard MC(TM)Albright &Wilson公司的多磷酸铵;
Spinfl:Spinflam MF82/PE(TM)多磷酸铵+前述的增效剂;
AmNL:Amgard NL(TM)磷酸乙二胺;
ZnBort:硼酸锌;
Mel.cy:氰尿酸三聚氰胺
Novams:Novomasse(TM)酚醛树脂中的60%红磷母料;
AmRYC:Elvax 4310(TM)EVA中的50%红磷母料。
Claims (8)
1.一种基于乙烯/醋酸乙烯共聚物的热熔粘接组合物,所述共聚物包含16-50%重量的醋酸乙烯和余数的乙烯,
该组合物以整个组合物的重量计,含有不多于35%的烧结阻燃添加剂,其量至少足可以防止按照保险商实验室测试方法UL-94(1993)的20mm垂直燃烧试验,V-1的由吸收底棉点火造成的粘接剂试条燃烧时产生的火焰滴下,其中阻燃添加剂包括以整个组合物的重量计的下列成分:
(a)20-35%的磷酸铵或有机磷酸胺,或
(b)15-30%的磷酸铵和磷酸铵的增效剂,或
(c)1-10%红磷,或
(d)10-25%的氰尿酸三聚氰胺,或
(e)10-25%的硼酸锌。
2.按照权利要求1的组合物,其在190℃下用2.16kg的重量,按照ASTMD138(1979)的方法测量的熔流指数,以g/10min为单位时至少为50。
3.按照权利要求2的组合物,其中基础聚合物的熔流指数如权利要求2所定义为至少100。
4.按照权利要求1的组合物,其中的阻燃添加剂是含磷的。
5.按照权利要求4的组合物,其中的阻燃添加剂包括(a)磷酸铵,或者(b)磷酸的有机胺化合物。
6.按照权利要求1的组合物,它是一种基于乙烯/醋酸乙烯共聚物的热熔粘接剂,所述共聚物含有至少16%重量的醋酸乙烯。
7.按照前面任一项权利要求的组合物,它载在尺寸可热恢复制品上,其中阻燃添加剂的用量少于如下的数量,即在该数量下能防止组合物软化和/或流动以便所述的制品在使用时的正常热恢复条件下进行密封。
8.具有权利要求7的组合物的电线或电缆接头或者导线系统,它们与已经发生了热恢复的所述可热恢复制品接触,或者被该制品包围。
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GBGB9523002.5A GB9523002D0 (en) | 1995-11-09 | 1995-11-09 | Flame-retarded adhesive composition |
GB9523002.5 | 1995-11-09 |
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US (1) | US6043304A (zh) |
EP (1) | EP0859818B1 (zh) |
JP (1) | JP2000500163A (zh) |
KR (1) | KR100471506B1 (zh) |
CN (1) | CN1127550C (zh) |
AT (1) | ATE215981T1 (zh) |
DE (1) | DE69620624T2 (zh) |
GB (1) | GB9523002D0 (zh) |
WO (1) | WO1997017410A1 (zh) |
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US10138421B2 (en) | 2013-11-12 | 2018-11-27 | 3M Innovative Properties Company | Hot melt intumescent materials for fire protection |
CN103788895A (zh) * | 2014-01-14 | 2014-05-14 | 安徽金门工贸有限公司 | 一种电缆生产专用热熔胶 |
CN106604967B (zh) * | 2014-06-26 | 2019-07-16 | 沙特基础工业全球技术公司 | 具有良好流动特性的阻燃导热聚合物组合物及其用途 |
CN104893642A (zh) * | 2015-05-29 | 2015-09-09 | 饶玉明 | 一种高强阻燃聚氨酯密封胶 |
CN104893641A (zh) * | 2015-05-29 | 2015-09-09 | 饶玉明 | 一种高强阻燃聚氨酯密封胶的制备方法 |
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US4284542A (en) * | 1979-05-07 | 1981-08-18 | E. I. Du Pont De Nemours And Company | Hot melt adhesive composition |
US4426549A (en) * | 1981-01-19 | 1984-01-17 | High Voltage Engineering Corporation | Track and erosion resistant electrical insulation comprising zinc borate and ethylene polymer |
US4440888A (en) * | 1982-06-28 | 1984-04-03 | Eastman Kodak Company | Fire resistant hot-melt adhesives containing modified polyethylene |
CA1309789C (en) * | 1987-06-26 | 1992-11-03 | Ichiro Sakon | Method for producing red phosphorus flame retardant and nonflammable resinous composition |
EP0352729B1 (en) * | 1988-07-27 | 1994-07-13 | Toyo Aluminium Kabushiki Kaisha | Sheet for forming article having electromagnetic wave shieldability |
JP3433457B2 (ja) * | 1991-07-26 | 2003-08-04 | 住友電気工業株式会社 | 難燃性接着剤及び熱収縮性チューブ |
US5456539A (en) * | 1993-05-25 | 1995-10-10 | Duplex Printer, Inc. | Printer with dual opposing printheads |
US5498476A (en) * | 1993-10-08 | 1996-03-12 | Minnesota Mining And Manufacturing Company | Electrically insulating film backing |
JPH07126451A (ja) * | 1993-10-29 | 1995-05-16 | Nakata Kooteingu:Kk | 樹脂組成物 |
GB2289680A (en) * | 1994-05-25 | 1995-11-29 | Minnesota Mining & Mfg | Flame-retardant pressure sensitive adhesives and tapes |
-
1995
- 1995-11-09 GB GBGB9523002.5A patent/GB9523002D0/en active Pending
-
1996
- 1996-11-08 CN CN96198173A patent/CN1127550C/zh not_active Expired - Fee Related
- 1996-11-08 DE DE69620624T patent/DE69620624T2/de not_active Expired - Lifetime
- 1996-11-08 KR KR10-1998-0703425A patent/KR100471506B1/ko not_active IP Right Cessation
- 1996-11-08 JP JP9509596A patent/JP2000500163A/ja active Pending
- 1996-11-08 AT AT96937422T patent/ATE215981T1/de not_active IP Right Cessation
- 1996-11-08 WO PCT/GB1996/002735 patent/WO1997017410A1/en active IP Right Grant
- 1996-11-08 EP EP96937422A patent/EP0859818B1/en not_active Expired - Lifetime
- 1996-11-08 US US09/051,973 patent/US6043304A/en not_active Expired - Lifetime
Patent Citations (4)
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JPS5214305A (en) * | 1974-10-11 | 1977-02-03 | Int Standard Electric Corp | Telecommunication type electronic switching station |
JPS5483939A (en) * | 1977-12-19 | 1979-07-04 | Matsushita Electric Ind Co Ltd | Flame-retardant adhesive |
GB2267498A (en) * | 1992-04-24 | 1993-12-08 | Minnesota Mining & Mfg | Flame retardants |
EP0653458A1 (en) * | 1993-11-16 | 1995-05-17 | Sumitomo Chemical Company, Limited | Fire retardant additive and fire retardant thermoplastic resin composition |
Also Published As
Publication number | Publication date |
---|---|
WO1997017410A1 (en) | 1997-05-15 |
CN1201477A (zh) | 1998-12-09 |
US6043304A (en) | 2000-03-28 |
EP0859818A1 (en) | 1998-08-26 |
DE69620624D1 (de) | 2002-05-16 |
JP2000500163A (ja) | 2000-01-11 |
EP0859818B1 (en) | 2002-04-10 |
ATE215981T1 (de) | 2002-04-15 |
KR19990067414A (ko) | 1999-08-16 |
DE69620624T2 (de) | 2002-11-21 |
KR100471506B1 (ko) | 2005-12-21 |
GB9523002D0 (en) | 1996-01-10 |
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