CN106905363B - 一种阻燃沙发布 - Google Patents
一种阻燃沙发布 Download PDFInfo
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- CN106905363B CN106905363B CN201710079696.5A CN201710079696A CN106905363B CN 106905363 B CN106905363 B CN 106905363B CN 201710079696 A CN201710079696 A CN 201710079696A CN 106905363 B CN106905363 B CN 106905363B
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- retardant
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Abstract
本发明涉及一种阻燃沙发布。其由坯布料和阻燃涂层组成，所述阻燃涂层由聚丙烯树脂和阻燃化合物组成。根据现有技术中已知工艺将所述涂料涂于布料之上，所得布料具有良好的阻燃效果。
Description
技术领域
本发明涉及纺织领域，具体而言，本发明涉及可有效阻燃的沙发布。
背景技术
阻燃面料是经过特种生产技术整理，技能有效防止火焰的蔓延，又能保护织物原有性能的产品。阻燃织物与普通织物的不同指出在于不同程度的降低纺织材料的燃烧速度并且离开火源之后能迅速停止燃烧，减少由于纺织品引起的火灾事故，避免不必要的损失。
沙发布料是在沙发制造过程中所用到的各种主体覆盖物的统称或者简称，现在的沙发、靠垫等用布制作外层越来越成为一种新潮流。但是由于表面的沙发布料为人体接触经常接触的面，极易由人引发布料的燃烧。
阻燃布料由于不仅要求较高的持久阻燃性能，还要有较好的舒适性。早期的芳香族聚酰胺“Nomex”纤维，它的耐热性非常好，极限氧指数达29，虽然其极限氧指数不是很高，但在其离开火源后，能自行熄灭且不产生熔滴；索罗蒂亚公司也公开了关于聚合物键合非卤素的阻燃聚合物制备的纤维、织物具有阻燃性。另外一些如氨纶纤维布、腈纶纤维布、腈氯纶纤维布、阻燃黏胶纤维布、阻燃涤纶布等，这类纤维均存在着遇火熔融滴落，致使皮肤烫伤，不能达到安全防火的效果。
因此亟需开发一种具有优良耐久使用，其具有优良阻燃性能的，可有多种用途的布料。
发明内容
织物的燃烧是一个复杂的过程。它们的易燃性除了纤维的化学组成以外还和织物结构以及织物上的染料等有关。纤维索纤维易燃，所以对其阻燃整理研究得最多。纤维素纤维主要为碳水化合物，是非热塑性纤维，受热不熔融，遇火焰后燃烧较快，其分解燃烧模式图参见图1。
一般认为，纤维素纤维的热裂解首先是高分子的纤维素纤维降解为低分子的纤维素，然后脱水炭化和分解成左旋葡萄糖。左旋葡萄糖在热的作用下可分解成乙烷、乙烯、乙醛、异丁烯醛、羟基丙酮、甲醇、羧酸等，并形成二次焦炭。其中可燃性气体和挥发性液体产生有火焰燃烧。固体残渣(主要是炭)的氧化产生无焰燃烧(阻燃)。
任何阻燃剂一般都是通过一种或几种作用方式而达到阻燃目的。阻燃剂升华和熔融都需要吸收热能，发生吸热反应。高温下在纤维表面形成覆盖层，起遮蔽作用，使纤维不易燃烧或阻止炭化纤维继续氧化，如硼砂—硼酸覆盖层。分解产生不燃性气体，将纤维震分解出来的可燃性气体浓度冲淡到不能产生火焰的浓度以下，如含卤阻燃剂。使纤维素脱水炭化，减少可燃气体，从而阻止火焰的蔓延。如含磷阻燃剂在燃饶过程中产生磷酸好或磷酸与纤维素逐基形成酯，阻止左旋葡萄糖的形成，促使织物脱水炭化而不易产生可燃的挥发性物质，阻止或减少可燃性气体的产生，起到阻燃作用。另外，磷酸酐会在热裂解时形成类似玻璃状的熔融物覆盖在织物上，促使有机物直接氧化成CO2，减少可燃性气体CO的生成，从而降低织物燃烧性能。
纤维素纤维用阻燃剂可分为无机化合物和有机化合物，其中无机化合物包括：硼酸盐和硼砂、磷酸盐、硫酸盐和氨基磺酸胺、钦和锑盐；有机化合物包括：聚氯乙烯、氯化石蜡、有机溴化合物和有机磷化合物。目前，具有实用价值，被广泛应用的纤维素纤维永久型阻燃剂有以下三类：
THPC(四羟甲基氯化磷)：采用THPC整理时，如与含氮或含卤素的化合物并用，可提高阻燃效果。THPC可与纤维素纤维发生交联，又能与三羟甲基三聚氰胺(TMM)等发生缩合反应，常与尿素及三羟甲基三聚氰胺等混合组成浸轧液。织物经浸轧后烘干，在140～150℃焙烘4～5min，使阻燃剂发生缩合反应而固着在纤维上，产品具有耐洗的阻燃性和防皱性，但织物的断裂强度和撕破强度有所降低。THPC和氨(NH3)起缩合反应能生成网状结构的聚合物而固着在纤维上，所以也可用THPC溶液浸轧织物。随后烘去大部分水分，用氨熏固着法进行阻燃整理，氨熏固着法处理的产品手感柔软，但设备复杂。此外，THPC在整理过程中会释出氯化氢，而损伤纤维，因此须在浸轧液中加入适量缓冲剂。THPC与氢氧化钠作用后可生成四羟甲基氢氧化鳞(THPOH)，也是良好的阻燃整理剂，由于在整理过程中无氯化氢释出，因而被广泛应用。
Pyrovatex CP(N-羟甲基二甲氧基膦酰基丙酰胺)：Pyrovatex CP和一般树脂拼用，在普通设备中浸轧烘干，焙烘时和纤维反应，产生耐洗的阻燃效果。在所有阻燃剂中，其毒性和整理后织物的毒性最低，可以满足儿童睡衣的要求，并且手感较好。
Fyrol 76，主要成分为乙烯基磷酸酯：采用浸轧、烘干、焙烘工艺处理织物，耐洗性较好。
纯涤纶织物属于可燃性材料，在受热后，当温度超过玻璃化温度(Tg)时，首先会软化，当温度达到熔融温度(Tm)时会熔融，熔化成黏稠橡胶状物体，产生熔融后再发生热分解作用，热分解能产生有毒气体及烟雾，对人是十分有害的，以至危及人的生命。熔融物一旦教着人体皮肤就会造成深度烧伤，是火灾中致人死命的主要原因之一。热分解过程中游离基链式反应是重要一环，所以要求阻燃剂能抑制游离基的形成，阻断链式反应，这便可以阻止有害气体和烟雾的生成。经过阻燃整理后的涤纶织物，可以由原来的易燃性材料，变成阻燃或难燃性材料，并且经过多次洗涤后，仍具有阻燃性。
在聚合过程中进行改性，即在聚合阶段将阻燃剂与聚合物单体共聚，或在高分子链上引入难燃基团进行接枝改性。在纺丝过程中进行改性，即在纺丝成型之前，将一定量的阻燃剂加到聚合物中，经混合加工使阻燃剂均匀地分散在聚合物熔体中。在后整理过程中进行改性，即采用浸轧、焙烘、高温高压涅渍、涂层等方法，使阻燃剂固着在纤维或织物上，从而获得阻燃效果。
涤纶是合成纤维中应用较广的品种，燃烧时熔融，熔融体落下能阻碍继续燃烧。涤棉混纺织物燃烧时，棉纤维生成的炭化物使涤纶熔融体落下受阻，燃烧不易熄灭。选择阻燃剂时，除了考虑阻燃效果和耐久程度外，还要考虑对织物的强度、手感、外观、色泽和牢度有元不良影响，以及对皮肤有无刺激等。
涤纶织物阻燃整理是通过吸附、沉积、渗透等作用，使阻燃剂与织物或纤维结合起来。目前，国内以六溴十二烷(HBCD)、环磷酸酯低聚物和二(2，3二溴丙基)磷酸酯为纯涤纶阻燃主要原料，现在国内应用较多的涤纶阻燃剂为北京洁尔爽高科技有限公司生产的纯涤纶阻燃整理剂ATF，它是一种适合于各种纯涤纶纺织品的耐洗型阻燃剂。当涤纶织物用ATF整理时，小分子的阻燃剂进入涤纶内部。ATF分解释放的低能自内基Br等，能有效地在火焰中捕获高能自由基(R、H和HO等)，从而阻止涤纶燃烧。同时ATF使涤纶热解机理发生变化，减少可燃性气体的生成。
羊毛本身的含氮量高，回潮率和受热分解气体的着火点也比较高，羊毛不易燃烧并且着火后有自熄性。羊毛织物阻燃整理剂主要有钛盐、锆盐和硼酸盐等化合物。羊毛织物的阻燃整理通常在染色后进行，一般是在60℃下处理20～40min，也可以与染色工艺同浴进行。用于羊毛的阻燃整理剂也可用于兔毛、犊牛毛的阻燃整理。
常见的测试方法有：测定织物燃烧的限氧指数，也就是测定织物在氧氮混合气体中能维持燃烧所需最少的氧气体积含量；按规定条件测定织物着火后的燃烧持续时间和织物被烧焦的程度；测定织物燃烧时效的传导速率。
目前现有技术中常用的阻燃剂有ATF、SCJ-968、SCJ-969、ATP、CP、THPC、AFW。
因此亟需提供一种具有良好阻燃性能且尽量无其它确定的新型阻燃剂化合物及应用其的布料。
本发明的目的在于提供一种阻燃布料，尤其是一种阻燃沙发布；
本发明的另一目的在于提供一种阻燃化合物；
本发明还有一目的在于所述阻燃化合物在阻燃或纺织方面的用途。
一种阻燃沙发布，其包括布料和阻燃涂层，所述涂层由聚丙烯树脂和下述式I所示的阻燃化合物组成，其中聚丙烯树脂占涂层总重的90wt％～95wt％，式I所示的阻燃化合物占涂层总重的5wt％～10wt％，涂层厚度为0.1～0.2mm，
其中，
R1选自氢、卤素、硝基、三氟甲基、酰基、氰基、羟基、C1-8烷基、C3-8环烷基、C1-8烷氧基、6-10元芳基、6-10元杂芳基；
A选自C1-8亚环烷基、C2-10亚烯基、C2-10亚炔基、6-10元亚芳基、6-10元亚杂芳基；
R2和R3选自C1-8烷基、C3-8环烷基、C1-8烷氧基、C2-10烯基。
优选地，式I阻燃化合物中：
R1选自氢、卤素、硝基、三氟甲基、酰基、氰基、羟基、甲基、乙基、丙基、丁基、环丙基、环丁基、环戊基、环己基、环庚基、环辛基、苯、萘、蒽、菲、四氢呋喃基、四氢吡喃基、氮杂环丁烷基、哌啶基；苯并噻唑基、苯并咪唑基、二氧杂环己基、噻唑基、吡唑基、吡咯基、咪唑基、噻吩基、硫代吗啉基、1,1-二氧代-1λ6-硫代吗啉基、吗啉基、吡啶基、嘧啶基、哒嗪基、吡嗪基、三嗪基、吡咯烷基、哌嗪基、嘌呤基、喹啉基、二氢-2H-喹啉基、异喹啉基、喹唑啉基、吲唑基、吲哚基、苯并呋喃基、苯并吡喃基或苯并二氧杂环戊基；
A选自亚甲基、亚乙基、亚丙基、亚丁基、亚环丙基、亚环丁基、亚环戊基、亚环己基、亚环庚基、亚环辛基、亚苯基、亚萘基、亚蒽基、亚菲基、亚四氢呋喃基、亚四氢吡喃基、亚哌啶基、亚噻唑基、亚吡唑基、亚吡咯基、亚咪唑基、亚噻吩基、亚吗啉基、亚吡啶基、亚嘧啶基、亚哒嗪基、亚吡嗪基、亚三嗪基、亚吡咯烷基、亚哌嗪基、亚嘌呤基、亚喹啉基、亚异喹啉基、亚喹唑啉基、亚吲唑基、亚吲哚基；
R2和R3选自甲基、乙基、丙基、丁基、环丙基、环丁基、环戊基、环己基、环庚基、环辛基、乙烯基、丙烯基、丁烯基、戊烯基、环丁烯基、环戊烯基、环己烯基、环庚烯基、环辛烯基。
更优选地，式I阻燃化合物如下所示：
优选地，所述布料选自棉、涤纶、锦纶、涤棉混纺、高密NC布或3M防水摩丝布。
所述的阻燃沙发布的制备方法，其包括下述步骤：
(1)配置阻燃涂层原料；
(2)将步骤(1)的涂层涂于布料表面；
(2)将步骤(2)的布料烘干整平。
本发明还提供了一种式I所示的阻燃化合物，其如下式所示：
其中，
R1选自氢、卤素、硝基、三氟甲基、酰基、氰基、羟基、C1-8烷基、C3-8环烷基、C1-8烷氧基、6-10元芳基、6-10元杂芳基；
A选自C1-8亚环烷基、C2-10亚烯基、C2-10亚炔基、6-10元亚芳基、6-10元亚杂芳基；
R2和R3选自C1-8烷基、C3-8环烷基、C1-8烷氧基、C2-10烯基。
优选地，R1选自氢、卤素、硝基、三氟甲基、酰基、氰基、羟基、甲基、乙基、丙基、丁基、环丙基、环丁基、环戊基、环己基、环庚基、环辛基、苯、萘、蒽、菲、四氢呋喃基、四氢吡喃基、氮杂环丁烷基、哌啶基；苯并噻唑基、苯并咪唑基、二氧杂环己基、噻唑基、吡唑基、吡咯基、咪唑基、噻吩基、硫代吗啉基、1,1-二氧代-1λ6-硫代吗啉基、吗啉基、吡啶基、嘧啶基、哒嗪基、吡嗪基、三嗪基、吡咯烷基、哌嗪基、嘌呤基、喹啉基、二氢-2H-喹啉基、异喹啉基、喹唑啉基、吲唑基、吲哚基、苯并呋喃基、苯并吡喃基或苯并二氧杂环戊基；
优选地，A选自亚甲基、亚乙基、亚丙基、亚丁基、亚环丙基、亚环丁基、亚环戊基、亚环己基、亚环庚基、亚环辛基、亚苯基、亚萘基、亚蒽基、亚菲基、亚四氢呋喃基、亚四氢吡喃基、亚哌啶基、亚噻唑基、亚吡唑基、亚吡咯基、亚咪唑基、亚噻吩基、亚吗啉基、亚吡啶基、亚嘧啶基、亚哒嗪基、亚吡嗪基、亚三嗪基、亚吡咯烷基、亚哌嗪基、亚嘌呤基、亚喹啉基、亚异喹啉基、亚喹唑啉基、亚吲唑基、亚吲哚基；
优选地，R2和R3选自甲基、乙基、丙基、丁基、环丙基、环丁基、环戊基、环己基、环庚基、环辛基、乙烯基、丙烯基、丁烯基、戊烯基、环丁烯基、环戊烯基、环己烯基、环庚烯基、环辛烯基。
优选地，所述阻燃化合物，是如下化合物：
所述式I化合物可用于阻燃和纺织领域。
由表明在所示化学基团中找到的碳原子总数的简化符号在前面标示本文中命名的某些化学基团。例如，C1-8烷基描述具有总数为1至8个碳原子的如下定义的烷基，并且C3-8环烃基烷基描述具有总数为3至8个碳原子的如下定义的环烃基烷基。简化符号中碳原子总数并不包含可能存在于所述基团的取代基中的碳。
因此，非另有相反的说明，否则说明书及所附权利要求中所用的下列术语具有以下的意思：
本申请所用的术语“烷基”是指直链或支链的烃链基团，仅由碳与氢原子组成，不含有不饱和键，具有一至十二个碳原子，优选为一至八个碳原子或一至六个碳原子，且其通过单键连接至分子的其余部份，例如甲基、乙基、正丙基、1-甲基乙基(异丙基)、正丁基、正戊基、1，1-二甲基乙基(叔丁基)、3-甲基己基、2-甲基己基等。
烷基基团可具有1至8个碳原子(在本申请中每次出现时，诸如“1至8”的数值范围是指给定范围中的每一整数；如“1至8”意为所述烷基基团可由1个碳原子、2个碳原子、3个碳原子等直至并包括8个碳原子，尽管本定义还涵盖未指定数值范围的术语“烷基”的出现)。烷基基团还可以是具有1至8个碳原子的中等大小的烷基。烷基基团还可以是具有1至5个碳原子的低级烷基。本申请化合物的烷基基团可被指定为“C1-4烷基”或类似的指定。仅以实例的方式，“C1-4烷基”表明烷基链中存在1至4个碳原子，即烷基链选自甲基、乙基、丙基、异丙基、正丁基、异丁基、仲丁基或叔丁基。
烷基基团可以是任意取代的，亦即取代或未取代的。当被取代时，取代基团是单独地并且独立地选自下列的一个或多个基团：环烃基、芳基、杂芳基、杂脂环基、羟基、烷氧基、芳氧基、巯基、烷硫基、芳硫基、氰基、卤代、羰基、硫代羰基、O-氨基甲酰基、N-氨基甲酰基、O-硫代氨基甲酰基、N-硫代氨基甲酰基、C-酰氨基、N-酰氨基、S-亚磺酰氨基、N-亚磺酰氨基、C-羧基、O-羧基、异氰酸根合、氰硫基、异硫氰酸根合、硝基、甲硅烷基、三卤代甲烷磺酰基、-NR’R”或包括单-和二-取代的氨基基团在内的氨基，及其被保护的衍生物。通常烃基基团包括但不限于甲基、乙基、丙基、异丙基、丁基、异丁基、叔丁基、戊基、己基、乙烯基、丙烯基、丁烯基、环丙基、环丁基、环戊基、环己基等等。每当取代基被描述为被“任意取代的”时，取代基可被上述取代基之一取代。
“C1-8烷基”指含有一至八个碳原子的上述定义的烷基基团。C1-8烷基基团可以如对烷基基团定义的那样被任意地取代。
在某些实施方案中，烷基为C1-8烷基。
在某些实施方案中，烷基为C1-6烷基。
在某些实施方案中，烷基为C1-4烷基。
本申请所用的“烷氧基”是指通式-OR，其中R是上文所定义的烷基，如甲氧基、乙氧基、正丙氧基、1-甲基乙氧基(异丙氧基)、正丁氧基、异丁氧基、仲丁氧基、叔丁氧基、戊氧基、叔戊氧基等等。
在某些实施方案中，烷氧基为C1-8烷氧基。
在某些实施方案中，烷氧基为C1-6烷氧基。
在某些实施方案中，烷氧基为C1-4烷氧基。
本申请所用的“亚烷基”指仅由碳和氢组成的，并且具有一至八个碳原子，连接分子的其余部分与残基基团的直链或支链二价烃链，例如亚甲基、亚乙基、亚丙基、正亚丁基。亚烷基链可以通过链中的一个碳或通过链中的任意二个碳与分子的其余部分和残基基团相连。
在某些实施方案中，亚烷基为C1-8亚烷基。
在某些实施方案中，亚烷基为C1-6亚烷基。
在某些实施方案中，亚烷基为C1-4亚烷基。
本申请所用的“亚烷氧基”是指通式-OR，其中R是上文所定义的亚烷基，如亚甲氧基、亚乙氧基、亚正丙氧基、亚异丙氧基、亚正丁氧基、亚异丁氧基、亚仲丁氧基、亚叔丁氧基、亚戊氧基、亚叔戊氧基等等。
在某些实施方案中，亚烷氧基为O(C1-8)亚烷基。
在某些实施方案中，亚烷氧基为O(C1-6)亚烷基。
在某些实施方案中，亚烷氧基为O(C1-4)亚烷基。
本申请所用的“芳基”是指具有完全离域的π电子体系的碳环(全碳)或两个或多个稠合环(共享两个相邻碳原子的环)。芳基基团的实例包括但不限于芴基、苯基及萘基。芳基基团例如可以具有五至十二个碳原子。本申请的芳基基团可以是取代的或未取代的。当被取代时，氢原子被一个或多个独立地选自下列取代基的基团取代：烷基、环烃基、芳基、杂芳基、杂脂环基、羟基、被保护的羟基、烷氧基、芳氧基、巯基、烷硫基、芳硫基、氰基、卤素、羰基、硫代羰基、O-氨基甲酰基、N-氨基甲酰基、O-硫代氨基甲酰基、N-硫代氨基甲酰基、C-酰氨基、N-酰氨基、S-亚磺酰氨基、N-亚磺酰氨基、C-羧基、被保护的C-羧基、O-羧基、异氰酸根合、氰硫基、异硫氰酸根合、硝基、甲硅烷基、三卤代甲烷磺酰基、-NR’R”(R’和R”为本申请中定义的烷基)或被保护的氨基。
在某些实施方案中，芳基为C6-18芳基。
在某些实施方案中，芳基为C6-12芳基。
在某些实施方案中，芳基为C6-10芳基。
“杂芳基(芳香杂环基)”是指5-至18-元芳香族环基团，其包含一至十七个碳原子与一至十个选自氮、氧及硫的杂原子。对于本发明的目的，杂芳基可为单环、双环、三环或四环的环系统，其可包含稠合的或桥接的环系统；且在杂芳基中的氮、碳或硫原子可任选地被氧化；氮原子可任选地被季铵化。实例包括但不限于氮杂基、吖啶基、苯并咪唑基、苯并噻唑基、苯并吲哚基、苯并二氧戊环基、苯并呋喃基、苯并噁唑基、苯并噻唑基、苯并噻二唑基、苯并[b][1，4]二氧杂环庚基、1，4-苯并二噁烷基、苯并萘并呋喃基、苯并二氧戊环基、苯并二噁烯基、苯并吡喃基、苯并吡喃酮基、苯并呋喃基、苯并呋喃酮基、苯并噻吩基、苯并三唑基、苯并[4，6]咪唑并[1，2-a]吡啶基、咔唑基、噌啉基、二苯并呋喃基、二苯并噻吩基、呋喃基、呋喃酮基、异噻唑基、咪唑基、吲唑基、吲哚基、吲唑基、异吲哚基、二氢吲哚基、异二氢吲哚基、异喹啉基、中氮茚基、异噁唑基、萘基、二氮杂萘基、二唑啉基、2-氧代氮杂基、噁唑基、环氧乙烷基、1-苯基-1H-吡咯基、吩嗪基、吩噻嗪基、吩噁嗪基、2，3-二氮杂萘基、蝶啶基、嘌呤基、吡咯基、吡唑基、吡啶基、吡嗪基、嘧啶基、哒嗪基、吡咯基、喹唑啉基、喹喔啉基、喹啉基、奎宁环基、异喹啉基、四氢喹啉基、噻唑基、噻二唑基、三唑基、四唑基、三嗪基及噻吩基。除非本说明书中另外明确述及，术语“杂芳基”意为包括可任选地被一个或多个独立地选自下列基团的取代基取代的杂芳基：烷基、环烃基、芳基、杂芳基、杂脂环基、羟基、被保护的羟基、烷氧基、芳氧基、巯基、烷硫基、芳硫基、氰基、卤素、羰基、硫代羰基、O-氨基甲酰基、N-氨基甲酰基、O-硫代氨基甲酰基、N-硫代氨基甲酰基、C-酰氨基、N-酰氨基、S-亚磺酰氨基、N-亚磺酰氨基、C-羧基、被保护的C-羧基、O-羧基、异氰酸根合、氰硫基、异硫氰酸根合、硝基、甲硅烷基、三卤代甲烷磺酰基、-NR’R”(R’和R”为本申请中定义的烷基)或被保护的氨基。
在某些实施方案中，杂芳基为C6-18杂芳基。
在某些实施方案中，杂芳基为C6-12杂芳基。
在某些实施方案中，杂芳基为C6-10杂芳基。
本申请所用的“杂环基”指由碳原子和一至五个选自氮、氧和硫的杂原子组成的稳定的三至十二员的非芳香族环基团。这样的杂环基基团的实例包括但不限于二氧环戊基、十氢异喹啉基、咪唑啉基、咪唑烷基、异噻唑烷基、异噁唑烷基、吗啉基、八氢吲哚基、八氢异吲哚基、2-氧代哌嗪基、2-氧代哌啶基、2-氧代吡咯烷基、噁唑烷基、哌啶基、哌嗪基、4-哌啶酮基、吡咯烷基、吡唑烷基、噻唑烷基、四氢呋喃基、三噻烷基、四氢吡喃基、硫代吗啉基、噻吗啉基、1-氧代-硫代吗啉基和1，1-二氧代-硫代吗啉基。除非说明书中另有明确说明，否则术语“杂环基”旨在包括被一个或多个选自如下取代基的基团所任意取代的上述定义的杂环基：环烃基、芳基、杂芳基、杂脂环基、羟基、烷氧基、芳氧基、巯基、烷硫基、芳硫基、氰基、卤代、羰基、硫代羰基、O-氨基甲酰基、N-氨基甲酰基、O-硫代氨基甲酰基、N-硫代氨基甲酰基、C-酰氨基、N-酰氨基、S-亚磺酰氨基、N-亚磺酰氨基、C-羧基、O-羧基、异氰酸根合、氰硫基、异硫氰酸根合、硝基、甲硅烷基、三卤代甲烷磺酰基、-NR’R”(R’和R”为本申请中定义的烷基)或包括单-和二-取代的氨基基团在内的氨基，及其被保护的衍生物。
在某些实施方案中，杂环基为C6-18杂环基。
在某些实施方案中，杂环基为C6-12杂环基。
在某些实施方案中，杂环基为C6-10杂环基。
附图说明：图1是织物分解燃烧模式图。
实施例
下面通过实施例对本发明作进一步说明。应该理解的是，本发明实施例所述方法仅仅是用于说明本发明，而不是对本发明的限制，在本发明的构思前提下对本发明制备方法的简单改进都属于本发明要求保护的范围。如无特别说明，实施例中用到的所有原料和溶剂均购为市售产品。
实施例1：式I化合物的制备
1)将1-氟-苯并环戊-5胺(25.1mmol)、无水乙醇(100ml)、4-溴苯甲醛(30mmol)加入200毫升三口瓶中，搅拌，向其中加入催化量的对甲苯磺酸，回流反应，TLC监测。反应混合物减压浓缩，干燥，不经纯化直接用于下一步反应，粗产率56％。
2)将步骤1)的反应产物(15mmol)、亚磷酸二乙酯(50mmol)以及催化量的醋酸钯，100毫升无水乙醇，加入到200毫升三口瓶中，搅拌加入10mmol的三乙胺以及5mmol的三苯基磷，回流反应，TLC监测。减压浓缩溶剂，收集固体沉淀。固体通过硅胶快速色谱纯化(无水甲醇/己烷(体积比＝1:3)洗脱)得到产物，产率68％。
1HNMR(DMSO)：δ8.13(s,CH,1H),7.95(d,CH,2H),7.75(d,CH,2H),7.11(m,CH,1H),6.99(m,CH,1H),6.91(m,CH,1H),4.55(t,CH,1H),3.78(m,CH3,6H),3.21(m,CH2,2H),2.48(m,CH2,2H).
实施例2-6：式I化合物的制备
以类似于实施例1的制备方法，根据A以及R1～R3取代基的不同，选取相应的原料制备实施例2-6相应的化合物。相应数据如下表所示：
实施例7：阻燃沙发布的制备：
(1)将聚丙烯树脂与式I所示的阻燃化合物混和，其中聚丙烯树脂为90wt％～95wt％，式I所示的阻燃化合物占5wt％～10wt％，上述原料混和之后，研磨，在常温下用搅拌机搅拌均匀；
(2)通过浸轧上浆的方式将步骤1)制得的混合物涂料均匀地涂布在布料表层；浸轧上浆是本领域技术人员所熟知的，当然本领域技术人员还可采用其它方法进行制备，不再赘述。
(3)对制得的布料送入烘箱塑化烘干，整平。
性能测试：
按照GB/T 17591-2006和GB/T 5455-1997所述的方法对本发明所制备的阻燃沙发布进行测试，所述布料均为涤纶。
布料1：阻燃涂层含有90wt％的聚丙烯树脂和10wt％的实施例1阻燃化合物；
布料2：阻燃涂层含有90wt％的聚丙烯树脂和10wt％的实施例2阻燃化合物；
布料3：阻燃涂层含有95wt％的聚丙烯树脂和5wt％的实施例6阻燃化合物。
试样应从距离布边1/10幅宽的部位量取，试样尺寸为300mm×80mm，长的一边要与织物经向(纵向)或纬向(横向)平行。每一样品，经向及纬向(纵向及横向)各取五块试样，经向(纵向)试样不能取自同一经纱，纬向(横向)试样不能取自同一纬纱。试样应按GB 6529规定，在二级标准大气中，即温度20℃±2℃，相对湿度65％士3％，视样品薄厚放置8～24h。直至达到平衡，然后取出放入密封容器内。
试验在温度为10-30℃及相对湿度为30％-80％的大气中进行。将试验箱前门关好，按下电源开关，指示灯亮表示电源已通，将条件转换开关放在焰高测定位置，打开气体供给阀门，按点火开关，点着点火器，用气阀调节装置调节火焰，使其高度稳定达到40mm±2mm，然后将条件转换开关放在试验位置。检查续燃、阴燃计时器是否在零位上。点燃时间设定为12s，将试样放入试样夹中，试样下沿应与试样夹两下端齐平打开试验箱门，将试样夹连同试样垂直挂于试验箱中。关闭箱门，此时指示灯应明亮，按点火开关，点着点火器，待30s火焰稳定后，按起动开关，使点火器移到试样正下方，点燃试样。此时距试样从密封容器内取出的时间必须在1min以内。12s后，点火器恢复原位，续姗计时器开始计时，待续燃停止，立即按计时器的停止开关，阴燃计时器开始计时，待阴燃停止后，按计时器的停止开关。读取续燃时间和阴燃时间，读数应精确到0.1s。当试验熔融性纤维制成的织物时，如果被测试样在然烧过程中有溶滴产生，则应在试验箱的箱底平铺上10mm厚的脱脂棉。注意熔融脱落物是否引起脱脂棉的燃烧或阴燃，并记录。打开试验箱前门，取出试样夹，卸下试样，先沿其长度方向炭化处对折一下，然后在试样的下端一侧，距其底边及侧边各约6mm处。挂上按试样单位面积的质量选用的重锤，再用手级缓提起试样下端的另一侧，让重锤悬空。再放下，测量试样撕裂的长度，即为损毁长度，结果精确到1mm。清除试验箱中碎片，并开动通风设备，排除试验箱中的烟雾及气体，然后再测试下一个试样。所得样品性能如下所示：
布料1：在285℃的温度下保持71min无滴落。水洗前氧指数36.9％，水洗30次后氧指数36.0％；垂直燃烧测试续燃时间：未洗0mm，10次洗后0mm；引燃时间：未洗0mm，50次洗后0mm；损毁长度：未洗171mm，30次洗后173mm；
布料2：在285℃的温度下保持72min无滴落。水洗前氧指数36.9％，水洗30次后氧指数36.2％；垂直燃烧测试续燃时间：未洗0mm，10次洗后0mm；引燃时间：未洗0mm，50次洗后0mm；损毁长度：未洗168mm，30次洗后170mm；
布料3：在285℃的温度下保持70min无滴落。水洗前氧指数37.1％，水洗30次后氧指数36.5％；垂直燃烧测试续燃时间：未洗0mm，10次洗后0mm；引燃时间：未洗0mm，50次洗后0mm；损毁长度：未洗170mm，30次洗后171mm。
Claims (5)
1.一种阻燃沙发布，其特征在于：包括布料和阻燃涂层，所述涂层由聚丙烯树脂和下述式I所示的阻燃化合物组成，其中聚丙烯树脂占涂层总重的90wt％～95wt％，式I所示的阻燃化合物占涂层总重的5wt％～10wt％，涂层厚度为0.1～0.2mm，
其中，式I阻燃化合物如下所示
2.根据权利要求1所述的阻燃沙发布，其特征在于所述布料选自棉、涤纶、锦纶、涤棉混纺、高密NC布或3M防水摩丝布。
3.权利要求1或2所述的阻燃沙发布的制备方法，其特征在于包括下述步骤：
(1)配置阻燃涂层原料；
(2)将步骤(1)的涂层涂于布料表面；
(2)将步骤(2)的布料烘干整平。
4.一种式I所示的阻燃化合物，其特征在于如下式所示：
其中，所述式I化合物是如下化合物
5.根据权利要求4式I化合物在阻燃和纺织领域中的用途。
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