CN1955214A - 阻燃聚碳酸酯树脂组合物 - Google Patents
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Classifications
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/36—Sulfur-, selenium-, or tellurium-containing compounds
- C08K5/41—Compounds containing sulfur bound to oxygen
- C08K5/42—Sulfonic acids; Derivatives thereof
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/0008—Organic ingredients according to more than one of the "one dot" groups of C08K5/01 - C08K5/59
- C08K5/0066—Flame-proofing or flame-retarding additives
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/54—Silicon-containing compounds
- C08K5/549—Silicon-containing compounds containing silicon in a ring
Abstract
通过将包括全氟链烷磺酸盐如全氟丁烷磺酸钾，和环硅氧烷如八苯基环四硅氧烷的阻燃组分加入聚碳酸酯中，可赋予聚碳酸酯树脂组合物改进的阻燃性能。该阻燃组分按合适的量加入以形成聚碳酸酯组合物，其中全氟链烷磺酸盐的存在量相对于整个组合物为0.02至0.1phr，环硅氧烷的存在量相对于整个组合物为至少0.02phr。
Description
本发明专利申请是申请号为01808669.1(国际申请号为PCT/US01/05427)，申请日为2001年2月20日、发明名称为“阻燃聚碳酸酯树脂组合物”的发明专利申请的分案申请。
技术领域
本申请涉及阻燃聚碳酸酯树脂组合物。因其强度和透明性，聚碳酸酯树脂具有特别多的显著工业用途。不幸的是，聚碳酸酯树脂本身可燃，并且会滴下热熔体物质，造成附近的材料也着火。因此，为在很多应用中安全地使用聚碳酸酯，必须包括阻止材料的可燃性能和/或降低滴淌的添加剂。挑战是，在不损害所需的强度和透明性、不引入新问题(如与卤化添加剂相关的潜在环境问题)和不使价格上升过高的情况下，确定完成此目的的添加剂。
背景技术
已公开了用于生产阻燃和/或耐滴淌聚碳酸酯的各种不同材料。这些材料的例子是描述于US Patents 3,971,756、4,028,297、4,110,299、4,130,530、4,303,575、4,335,038、4,552,911、4,916,194、5,218,027和5,508,323中的材料。尽管存在这些各种类型的公开文献，然而，仍然留有改进阻燃聚碳酸酯树脂配方的空间。
商品化的广泛用于阻燃聚碳酸酯树脂组合物的添加剂是有机盐类，特别是磺酸盐。这些盐的具体例子是全氟链烷磺酸盐，如全氟丁烷磺酸钾(“KPFBS”，又称为“Rimar盐”)，和二苯基砜磺酸钾(“KSS”)，当它们与聚碳酸酯树脂掺混时得到无混浊(haze)组合物。在聚碳酸酯树脂中使用全氟链烷磺酸盐描述于US Patents 3,775,367中。然而，仅使用这些材料可获得的益处是有限的，实际上通常要包括另外的添加剂。在保持透明度下用于增强这些类型的组合物阻燃性质的常规方式是加入可溶有机卤添加剂。例如，工业等级的LEXAN聚碳酸酯树脂(如940A，920A)含KSS(0.3phr)和四溴双酚A/双酚A共聚物(0.5phr，净0.13phr溴含量)的混合物。若没有溴，920A和940A等级在预定这些等级满足的UL 94 V0 125mil可燃性试验中存在不一致/不可靠的性能。然而，溴化的添加剂不适合要求满足“ECO-便利”标准的组合物，因为这些标准限制包括溴或氯。
发明内容
现已发现，通过将包括全氟链烷磺酸盐如全氟丁烷磺酸钾，和环硅氧烷如八苯基环四硅氧烷的阻燃组分加入聚碳酸酯中，可赋予聚碳酸酯树脂组合物改进的阻燃性能。该阻燃组分按合适的量加入以形成聚碳酸酯组合物，其中全氟链烷磺酸盐的存在量相对于整个组合物为0.02至0.1phr，环硅氧烷的存在量相对于整个组合物为至少0.02。
发明详述
本发明涉及包括聚碳酸酯树脂的阻燃组合物。本发明组合物的聚碳酸酯组分可为任何等级的并可由任何方法制备。因此，例如该聚碳酸酯可通过界面方法或通过催化酯基转移方法制备。该聚碳酸酯可为支化或线性结构，并可包括官能取代基。聚碳酸酯共聚物也包括在本发明之内。通过这些方法制备聚碳酸酯的技术是公知的例如从USPatents 3,030,331、3,169,121、4,130,548、4,286,083、4,552,704、5,210,268和5,606,007。
当聚碳酸酯树脂制备后，可将其与阻燃组分掺混。根据本发明，这种阻燃组分包括全氟链烷磺酸盐和环硅氧烷。
如上所述，可用于本发明的全氟磺酸盐描述于US Patents3,775,367中。最常用的这些材料是全氟丁烷磺酸钾，可从多种途径市购。该全氟链烷磺酸盐以足够赋予阻燃性质的量包含在组合物中。通常，其用量为0.02至0.1phr，按组合物总重量计。用量超过0.1phr会导致混合的产品混浊(haze)、而不会导致改进的阻燃性能。
环硅氧烷以在全氟链烷磺酸盐存在下足够提供改进的阻燃性能的量包括于组合物中。通常其用量为0.02至0.3phr，按组合物总重量计。可用于本发明的合适环硅氧烷包括具有如下通式的那些：
其中R独立地选自C1至C36烷基、氟化或全氟C1至C36烷基、C1至C36烷氧基、C6至C14芳基、6至14个碳原子的芳氧基、7至36个碳原子的芳烷氧基和6至14个碳原子的芳基取代的C1至C36烷基。环硅氧烷的具体例子包括但不限于：八苯基环四硅氧烷、六甲基环三硅氧烷、八甲基环四硅氧烷、十甲基环五硅氧烷、十二甲基环六硅氧烷、三甲基三苯基环三硅氧烷和四甲基四苯基环四硅氧烷。
将全氟链烷磺酸盐和环硅氧烷与熔融聚碳酸酯，例如在螺杆型挤出机中掺混，并挤出并模制为所需形状的部件。可将它们混合，例如作为包括全氟链烷磺酸盐和环硅氧烷的阻燃添加剂组合物，或以任何顺序连续加入聚碳酸酯中。本发明的阻燃组合物合适地包括比例约0.07至5(重量)的全氟链烷磺酸盐和环硅氧烷。
为测试阻燃性能，由含各种量的全氟丁烷磺酸钾和环硅氧烷的挤出聚碳酸酯模制成棒。发现这些组合物显示明显改进的阻燃性能，如下面所列实施例中反映的。尽管作用机理不清楚，但这一结果可能是由于各阻燃组分的协同相互作用带来的，因为对于KSS与环硅氧烷的组合未观察到类似的改进。此外，尽管这里报道的小规模试验未确实证明这一点，但大规模试验证明使用本发明的阻燃组合物导致聚碳酸酯降低混浊。
本发明组合物可包括本领域已知的包括于聚碳酸酯组合物中的常规添加剂。这些添加剂包括但不限于稳定剂、脱模剂、光稳定剂、热稳定剂、颜料和染料。
具体实施方式
本发明将通过下面的非限制性实施例进一步描述。
实施例1
通过如下方法制备用于按照UL94程序进行燃烧性能测试的聚碳酸酯样品：将两种不同分子量等级的线性LEXAN聚碳酸酯树脂掺混以使其达到目标熔体流动15至16，按照ASTM D1238在300℃、1.2kg下测量。某些组合物还包括0.35phr季戊四醇四硬脂酸酯(PETS)脱模剂。将该粉末共混物样品在温度范围230至290℃下挤出并切割为珠粒。将这些珠粒样品在温度295℃下注塑为具有尺寸5英寸×1/2英寸、厚度125mil的测试部件。
将这些部件用标准Underwriters Laboratory UL94测试方法(2天处理法)测试，不同的是测试20个棒，而不是通常的5个棒。通过如下方法分析数据：首先计算平均起火时间(avFOTsec)、起火时间的标准偏差(sdFOTsec)和总滴数，并用统计方法将此数据转化为特定样品配方达到在5个棒试验的常规UL 94测试中的V0“通过”分级的第一次通过预期概率，或“p(FTP)”。对于UL测试中的最大阻燃性能，优选p(FTP)尽可能接近1。
将珠粒样品还模塑为具有尺寸2英寸×英寸×125mil的测试部件。将这些部件用于采用ASTM D1003测试法的浊度测量。
这些实验的结果概述于表1A-D中。如该表所示，同时包括全氟丁烷磺酸钾和环硅氧烷(八苯基环四硅氧烷)的本发明配方的第一次通过概率“p(FTP)”比仅用全氟丁烷磺酸钾观察到的至少高数倍。仅用环硅氧烷进行的实验显示很小的阻燃性能改进(如存在任何改进的话)。使用KSS和环硅氧烷的相应实验未显示增强的阻燃性能。
用相同的配方，但不包括KPFDS制备对比组合物。这些对比组合物中的硅氧烷量为0.05、0.1、0.2、1.0和2.0phr。所有对比样品未通过UL94 V0测试。
表1A
表1B
表1C
表1D
实施例2
按照与实施例1相同的方式制备样品，不同的是使用的聚碳酸酯树脂为70重量份含0.42mol％1，1，1-三(羟苯基)乙烷的支化聚碳酸酯树脂和30重量份线性聚碳酸酯树脂的共混物，以使其达到目标熔体流动2至3，按照ASTM D1238在300℃、1.2kg下测量。还包括UV稳定剂(UV5411，2-(2-羟基-5-叔辛基苯基)苯并三唑)。将样品在240至305℃下挤出并在320-332℃注塑为具有厚度60mil、75mil和125mil的测试部件。这些配方和结果概述于表2A和B中。在60mil和125mil下进行对比性试验。60mil试验仅显示边缘性能，并且对于所有含KPFBS的样品无此趋势，并且对所有无KPFBS的样品滴淌失败。125mil测试对于具有0.07KPFBS的样品具有p(FTP)0.9867。其它含KPFBS的样品由于在75mil时通过因此未测试。无KPFBS的所有样品具有滴淌失败。
| 表2A | |||||||
| KPFBS，Bayer(phr) | 0 | 0.07 | 0.08 | 0.09 | 0.07 | 0.08 | 0.09 |
| 硅氧烷(phr) | - | - | - | - | 0.05 | 0.05 | 0.05 |
| UV稳定剂(phr) | 0.27 | 0.27 | 0.27 | 0.27 | 0.27 | 0.27 | 0.27 |
| p(FTP)UL 94 V075mils | nd | 0.2125 | 0.9157 | 0.9054 | 0.9802 | 0.9218 | 0.9867 |
| ％浊度 | 1 | 1.2 | 1.8 | 1.1 | 0.9 | 1.3 | 1.6 |
| avFOTsec | 2.8 | 2.4 | 2.5 | 2.3 | 2.4 | 2.3 | |
| sdFOTsec | 2.1 | 1.7 | 1.9 | 1.4 | 1.8 | 1.3 | |
| 滴数 | 5 of 5 | 4 | 0 | 0 | 0 | 0 | 0 |
| 熔体流动 | 2.65 | 2.4 | 2.4 | 2.65 | 2.23 | 2.23 | 2.82 |
| 表2B | |||||
| KPFBS，Bayer(phr) | 0.07 | 0.08 | 0.09 | 0 | 0 |
| 硅氧烷(phr) | 0.1 | 0.1 | 0.1 | 0.05 | 0.1 |
| UV稳定剂(phr) | 0.27 | 0.27 | 0.27 | 0.27 | 0.27 |
| p(FTP)UL 94 V075mils | 0.965 | 0.9509 | 0.9568 | nd | nd |
| ％浊度 | 0.6 | 0.9 | 1.3 | 1 | 0.7 |
| avFOTsec | 2.4 | 2.4 | 2.5 | ||
| sdFOTsec | 1.5 | 1.6 | 1.6 | ||
| 滴数 | 0 | 0 | 0 | 7 of 10 | 5 of 5 |
| 熔体流动 | 2.50 | 2.35 | 2.39 | 2.98 | 3.03 |
Claims (4)
1.一种阻燃添加剂组合物，包括全氟链烷磺酸盐和环硅氧烷，其中全氟链烷磺酸盐和环硅氧烷以重量比例0.07至5存在。
2.根据权利要求1的添加剂组合物，其中环硅氧烷为八苯基环四硅氧烷。
3.根据权利要求2的添加剂组合物，其中全氟链烷磺酸盐为全氟丁烷磺酸钾。
4.根据权利要求1的添加剂组合物，其中全氟链烷磺酸盐为全氟丁烷磺酸钾。
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US09/560770 | 2000-04-28 | ||
| US09/560,770 US6353046B1 (en) | 2000-04-28 | 2000-04-28 | Fire-retarded polycarbonate resin composition |
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| Application Number | Title | Priority Date | Filing Date |
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| CNB018086691A Division CN100402590C (zh) | 2000-04-28 | 2001-02-20 | 阻燃聚碳酸酯树脂组合物 |
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| CN1955214B CN1955214B (zh) | 2012-02-22 |
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| CN2006101603302A Expired - Lifetime CN1955214B (zh) | 2000-04-28 | 2001-02-20 | 阻燃添加剂组合物 |
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| Country | Link |
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| US (1) | US6353046B1 (zh) |
| EP (2) | EP2065436B1 (zh) |
| JP (1) | JP2003531940A (zh) |
| KR (1) | KR100747011B1 (zh) |
| CN (2) | CN100402590C (zh) |
| WO (1) | WO2001083606A1 (zh) |
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| CN105073892A (zh) * | 2013-02-28 | 2015-11-18 | 拜耳材料科学有限责任公司 | 阻燃性聚碳酸酯组合物 |
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-
2000
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- 2001-02-20 WO PCT/US2001/005427 patent/WO2001083606A1/en active Application Filing
- 2001-02-20 CN CNB018086691A patent/CN100402590C/zh not_active Expired - Lifetime
- 2001-02-20 CN CN2006101603302A patent/CN1955214B/zh not_active Expired - Lifetime
- 2001-02-20 KR KR1020027014411A patent/KR100747011B1/ko active IP Right Grant
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105073892A (zh) * | 2013-02-28 | 2015-11-18 | 拜耳材料科学有限责任公司 | 阻燃性聚碳酸酯组合物 |
Also Published As
| Publication number | Publication date |
|---|---|
| EP2065436A2 (en) | 2009-06-03 |
| EP2065436A3 (en) | 2010-11-17 |
| EP2065436A8 (en) | 2010-06-30 |
| CN1955214B (zh) | 2012-02-22 |
| EP1278798A1 (en) | 2003-01-29 |
| WO2001083606A1 (en) | 2001-11-08 |
| KR100747011B1 (ko) | 2007-08-07 |
| CN100402590C (zh) | 2008-07-16 |
| KR20020091248A (ko) | 2002-12-05 |
| JP2003531940A (ja) | 2003-10-28 |
| CN1426436A (zh) | 2003-06-25 |
| EP2065436B1 (en) | 2012-10-31 |
| US6353046B1 (en) | 2002-03-05 |
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