CN112323517A - 磷硼杂链羟端基预聚物嵌段聚氨酯共聚物水性印染防火涂料及其制备方法与应用 - Google Patents
磷硼杂链羟端基预聚物嵌段聚氨酯共聚物水性印染防火涂料及其制备方法与应用 Download PDFInfo
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Abstract
本发明涉及防火涂料技术领域,具体涉及一种磷硼杂链羟端基预聚物嵌段聚氨酯共聚物水性印染防火涂料及其制备方法与应用,按质量百分数计,该涂料的原料组成包括:11.5~13.5%颜料或染料、3.0~4.0%填料,83.5~84.5%磷硼杂链预聚物嵌段聚氨酯水性共聚物,该共聚物结构式如下:
Description
技术领域
本发明涉及防火涂料技术领域,具体涉及一种磷硼杂链羟端基预聚物嵌段聚氨酯共聚物水性印染防火涂料及其制备方法与应用。
背景技术
公开该背景技术部分的信息仅仅旨在增加对本发明的总体背景的理解,而不必然被视为承认或以任何形式暗示该信息构成已经成为本领域一般技术人员所公知的现有技术。
阻燃防火布料广泛用于帘幕装饰、消防服饰、消防工程,防火包装等领域,织造布料的天然纤维和合成纤维大多属于易燃物,遇明火容易燃烧,在使用过程中存在火灾隐患,布料阻燃防火一直受到国内外科技工作者和工程技术人员的高度重视。在布料表面通过印染整理涂覆防火涂料是实现布料阻燃防火功能最便捷的技术途径,经涂覆防火涂料的布料经干燥形成一层吸附于纤维表面的阻燃涂层,可以有效阻止布料燃烧,降低布料的火灾风险。研究表明,卤素、磷、硼、氮、硅等元素在有机材料燃烧过程具有优异的阻燃效果,含卤阻燃剂因在燃烧过程中生成高毒性气体而限用, P、B、N、Si等元素阻燃剂具有无卤低烟、环保高效的阻燃功能。将P、 B、N、Si等元素通过分子设计与合成,合成具有本征阻燃功能的聚合物,是制备无卤低烟、长效阻燃高分子材料的有效途径。
文献1公开了一种织物涂料染色工艺,该工艺染液由涂料色浆、阳离子改性剂、表面活性剂、pH调节剂和粘合剂等物质组成,染液按照一定的加料顺序混合均匀后对织物直接进行轧染,经过烘干、固色后得到涂料染色织物产品。
文献2公开了具有防水阻燃功能的涤纶面料,其在纳米银纤维面料层的顶部通过耐温环氧胶连接了阻燃层,可有效提高本面料的阻燃性,在聚酯纤维基底层的底部通过PS胶水连接了防水层,可有效提高本面料的防水性,从而在保障本面料具有较强耐磨性的同时,也具备了防水和阻燃的能力,扩大了本面料的使用范围。
文献3公开了含磷醇酸树脂饰面型防火涂料及其制备方法,该涂料配方为:含磷醇酸树脂30%~36%,聚磷酸铵11.5%~15.8%,三聚氰胺 9.5%~10.8%,季戊四醇4.2%~4.8%,硼酸锌2.7%~3.6%,钛白粉4.1%~4.8%,三氧化二钼1%~1.2%,二甲基硅油0.1%~0.12%,催干剂0.9%~1.08%,溶剂30%~36%。
综上,现有的一些印染防火涂料技术具有以下特点:
①无机阻燃剂居多,有机阻燃剂较少。无机阻燃剂的优点在于价格低廉,品种较多,缺点在于比重大、用量多、耐水性差、相容性差、迁移性大,用于织物阻燃上浆剂制备,浆料稳定性差,以此整理的织物手感差、易掉粉、毒性大、阻燃效果依时衰减等。有机物阻燃剂的优点在于阻燃效率高、比重小、耐水性好、相容性较好,不足之处在于品种较少、价格较高、毒性大、含卤高烟、不耐有机介质,因迁移造成人身伤害和应用环境污染,发生火灾时因含卤高烟会造成更大的环境污染。
②添加型阻燃剂居多,本征型阻燃剂较少。添加型阻燃剂是以具有阻燃功能的低分子化合物,通过共混方式添加于非阻燃聚合物体系,在应用过程中其优点在于品种多、使用方便,由此制备的织物上浆剂,其缺点在于浆料稳定性差,上浆整理的织物阻燃时效差、毒理风险高。本征型阻燃剂是通过分子设计和合成,将具有阻燃功能的元素通过化学键的方式键接到聚合物分子结构中,或合成元素杂化本征阻燃聚合物采取物理共混方式形成高分子合金,由此制备的织物上浆剂,其优点在于提高了阻燃元素化合物的存在稳定性,达到聚合物织物环保安全、长效阻燃的效果,其不足之处在于品种少、价格高、技术难度大。
现有技术文献:
文献1:中国专利,申请号为200610096923.7,名称为一种织物涂料染色工艺。
文献2:中国专利,申请号为201921195737.8,名称为具有防水阻燃功能的涤纶面料。
文献3:中国专利,申请号为201310259043.7,名称为含磷醇酸树脂饰面型防火涂料及其制备方法。
发明内容
本发明的目的是制备具有阻燃防火功能和适合布料印染性能的水性防火涂料,且经该水性防火涂料印染整理的布料具有低毒环保、低烟无卤、长效阻燃和防水防火的协效功能。
为此,本发明公开一种磷硼杂链羟端基预聚物嵌段聚氨酯共聚物水性印染防火涂料及其制备方法与应用,其通过分子设计与合成将磷硼阻燃元素和亲水基团以化学键形式键接于聚合物分子结构之中,得到适用于制备适合布料印染的涂料。
为实现上述目的,本发明的技术方案如下所示:
在本发明的第一方面,公开一种磷硼杂链预聚物嵌段聚氨酯水性共聚物,其结构式如式(1)所示:
所述式(1)中,R包括-HCH2CH2OH、-(CH2CH2OH)2、-HCH2CH3、 -(CH2CH3)2等中的任意一种。
在本发明的第二方面,公开所述磷硼杂链预聚物嵌段聚氨酯水性共聚物的制备方法,包括如下步骤:
(1)将有机溶剂、磷硼杂链预聚物、二月桂酸二丁基锡混合后在保护气氛与加热条件下保温,待体系温度均匀后加入甲苯二异氰酸酯和二羟甲基丙酸,并将体系升温后保温,分离溶剂。
(2)将体系降温后加入中和剂和水,搅拌后调整pH值至合格,即得。
进一步地,步骤(1)中,所述有机溶剂包括二甲苯、甲苯、环己酮等中的任意一种,其添加量能够充分溶解各原料即可,本发明不做具体限定。
进一步地,所述共聚物的制备方法中,按质量百分数计,磷硼杂链预聚物(PDCP-DGB)、甲苯二异氰酸酯(TDI)、二羟甲基丙酸(DMPA)的添加比例依次序为:75.9~76.9%、16.2~17.3%、6.8~6.9%。
进一步地,步骤(1)中,所述二月桂酸二丁基锡与甲苯二异氰酸酯物质的量比为1:0.01~0.03。在本发明中,利用二月桂酸二丁基锡的催化作用,通过逐步加聚合成磷硼杂链预聚物聚氨酯嵌段共聚物。
进一步地,步骤(1)中,所述磷硼杂链预聚物的数均分子量为 1500~2500、分布指数为1.1~1.2。
进一步地,步骤(1)中,所述保护气氛包括氮气、氩气等惰性气体,避免氧气对逐步加聚反应的阻聚效应。
进一步地,步骤(1)中,所述加热温度为60~65℃,加热方式为水浴加热,保温时间为20~35min。在一定温度下反应有助于加速反应速率,提高反应效率。
进一步地,步骤(1)中,所述体系升温后温度为70~75℃,进一步提高缩聚反应的反应程度,保温时间为1.5~2.5h。
进一步地,步骤(2)中,所述中和剂包括一乙醇胺、二乙醇胺、一乙胺、二乙胺等中的至少一种本发明中,所述中和剂的主要作用是与体系中的二羟甲基丙酸反应,进而将反应产物的pH值调节至合格。
进一步地,步骤(2)中,所述体系降温后温度为45~50℃。
进一步地,步骤(2)中,所述pH值保持在7.5~9.0范围内,以保持聚合物水性体系稳定。
在本发明的第三方面,公开一种磷硼杂链羟端基预聚物嵌段聚氨酯共聚物水性印染防火涂料,按质量百分数计,其原料组成包括:11.5~13.5%颜料或染料、3.0~4.0%填料,83.5~84.5%本发明所述的磷硼杂链预聚物嵌段聚氨酯水性共聚物。
进一步地,所述颜料或染料根据所需色彩选择。所述填料包括纳米碳酸钙、滑石粉、膨润土、纳米凹凸棒土等中的至少一种。
进一步地,所述涂料的原料组成还包括助剂,可选地,所述助剂包括消泡剂,例如:聚甲基硅油、磷酸三丁酯等中的至少一种,其用量为涂料配方总质量的1~2%。
进一步地,所述涂料的细度≤40μm,以便将涂料均匀涂覆在布料表面。
进一步地,所述涂料的原料组成还包括水复合溶剂。可选地,所述水复合溶剂的添加量以25℃下将涂料的粘度用水调节至1000~1500Cp为准。
进一步地,所述水复合溶剂为水、乙醇和乙二醇二甲醚的混合体系,可选地,所述水、乙醇和乙二醇二丁醚的体积比为3:1:2。
在本发明的第四方面,公开所述磷硼杂链羟端基预聚物嵌段聚氨酯共聚物水性印染防火涂料的制备方法,包括:将所述颜料或染料、填料、磷硼杂链预聚物嵌段聚氨酯水性共聚物混合均匀,磨细后再以水复合溶剂调节粘度,即得。
在本发明的第五方面,公开所述硼杂链羟端基预聚物嵌段聚氨酯共聚物水性印染防火涂料在布料产品等的制备中的应用。
相较于现有技术,本发明具有以下有益效果:
(1)通过分子设计与合成,将磷硼阻燃元素和亲水基团以化学键形式键接于聚氨酯分子结构之中,得到磷硼杂链预聚物嵌段聚氨酯水性共聚物,因为磷硼元素在聚合物分子链中,只要聚合物分子链未降解为小分子,聚合物阻燃性能、防水特性长期有效;同时分子链中无卤素元素、高温分解过程氧化生成磷酸盐、硼酸盐乃至磷硼氧化物,具有低烟无卤的特点。
(2)本发明以所述硼杂链羟端基预聚物嵌段聚氨酯共聚物水性印染防火涂料制备适合布料染色的涂料,经过该涂料制备的布料具有低毒环保、低烟无卤、长效阻燃和防水防火的协效功能。
具体实施方式
下面结合具体实施例,进一步阐述本发明。应理解,这些实施例仅用于说明本发明而不用于限制本发明的范围。下列实施例中未注明具体条件的实验方法,通常按照常规条件或按照制造厂商所建议的条件。
除非另行定义,文中所使用的所有专业与科学用语与本领域熟练人员所熟悉的意义相同。本发明所使用的试剂或原料均可通过常规途径购买获得,如无特殊说明,本发明所使用的试剂或原料均按照本领域常规方式使用或者按照产品说明书使用。
此外,任何与所记载内容相似或均等的方法及材料皆可应用于本发明方法中。本发明中所述的较佳实施方法与材料仅作示范之用,现根据具体实施例对本发明进一步说明。
下列实施例中,所述磷硼杂链预聚物的数均分子量为1500~2000、分布指数为1.1~1.2。也可以采用其他现有的方法合成或者市售产品。
下列实施例中,磷硼杂链预聚物嵌段聚氨酯水性共聚物的合成路线如式(2)所示:
第一实施例
1、磷硼杂链预聚物嵌段聚氨酯水性共聚物的制备,包括如下步骤:
(1)在具有机械搅拌、氮气保护、冷凝回流、水浴加热和控温装置的四口烧瓶中,加入50ml二甲苯、75.9g PDCP-DGB、与TDI物质的量比为1:0.03的二月桂酸二丁基锡。
(2)开搅拌、通氮气,将步骤(1)的反应体系水浴加热至60±1℃,保温体系均匀后,30min内滴加17.3g TDI和6.8g DMPA,保持体系温度 75±1℃,保温2h,分离回收上层二甲苯。
(3)将步骤(2)的反应体系降温至45±1℃,然后加入一乙醇胺和 50ml水,继续搅拌1h,调整pH=9.0,停搅拌出料,即得磷硼杂链预聚物嵌段聚氨酯水性共聚物。
2、一种硼杂链羟端基预聚物嵌段聚氨酯共聚物水性印染防火涂料的制备,包括如下步骤:
S1、称取83.5g本实施例制备的磷硼杂链预聚物嵌段聚氨酯水性共聚物、13.5g水性大红染料、3.0g纳米碳酸钙,加入混合容器中搅拌混合,加入15.0ml水复合溶剂(水、乙醇和乙二醇二丁醚的体积比为3:1:2的混合物)搅匀,将得到的混合液倾入砂磨机中,启动砂磨机,保持转速 5000r/min、冷却水温≤30℃,研磨30min;
S2、以细度刮板仪检测研磨至细度≤40μm后,加入3.0g磷酸三丁脂和10.0ml水复合溶剂(水、乙醇和乙二醇二丁醚的体积比为3:1:2的混合物),继续研磨5min,将涂料的粘度调节至1500Cp(25℃),停砂磨机,过滤出料,得到磷硼杂链预聚物嵌段聚氨酯水性印染防火涂料。
第二实施例
1、磷硼杂链预聚物嵌段聚氨酯水性共聚物的制备,包括如下步骤:
(1)在具有机械搅拌、氮气保护、冷凝回流、水浴加热和控温装置的四口烧瓶中,加入50ml二甲苯、76.9g PDCP-DGB、与TDI物质的量比为1:0.02的二月桂酸二丁基锡。
(2)开搅拌、通氮气,将步骤(1)的反应体系水浴加热至65±1℃,保温体系均匀后,30min内滴加16.2g TDI和6.9g DMPA,保持体系温度 70±1℃,保温2h,分离回收上层二甲苯。
(3)将步骤(2)的反应体系降温至40±1℃,然后加入一乙醇胺和50ml水,继续搅拌1h,调整pH=8.0,停搅拌出料,即得磷硼杂链预聚物嵌段聚氨酯水性共聚物。
2、一种硼杂链羟端基预聚物嵌段聚氨酯共聚物水性印染防火涂料的制备,包括如下步骤:
S1、称取84.5g本实施例制备的磷硼杂链预聚物嵌段聚氨酯水性共聚物、11.5g水性白色染料、4.0g纳米凹凸棒土,加入混合容器中搅拌混合,加入15.0ml水复合溶剂(水、乙醇和乙二醇二丁醚的体积比为3:1:2的混合物)搅匀,将得到的混合液倾入砂磨机中,启动砂磨机,保持转速 5000r/min、冷却水温≤30℃,研磨30min;
S2、以细度刮板仪检测研磨至细度≤40μm后,加入3.0g磷酸三丁脂和10.0ml水复合溶剂(水、乙醇和乙二醇二丁醚的体积比为3:1:2的混合物),继续研磨5min,将涂料的粘度调节至1200Cp(25℃),停砂磨机,过滤出料,得到磷硼杂链预聚物嵌段聚氨酯水性印染防火涂料。
第三实施例
1、磷硼杂链预聚物嵌段聚氨酯水性共聚物的制备,包括如下步骤:
(1)在具有机械搅拌、氮气保护、冷凝回流、水浴加热和控温装置的四口烧瓶中,加入50ml二甲苯、76.0g PDCP-DGB、与TDI物质的量比为1:0.01的二月桂酸二丁基锡。
(2)开搅拌、通氮气,将步骤(1)的反应体系水浴加热至65±1℃,保温体系均匀后,30min内滴加17.0g TDI和6.8g DMPA,保持体系温度 75±1℃,保温1.5h,分离回收上层二甲苯。
(3)将步骤(2)的反应体系降温至40±1℃,然后加入一乙醇胺和 50ml水,继续搅拌1h,调整pH=7.5,停搅拌出料,即得磷硼杂链预聚物嵌段聚氨酯水性共聚物。
2、一种硼杂链羟端基预聚物嵌段聚氨酯共聚物水性印染防火涂料的制备,包括如下步骤:
S1、称取84.0g本实施例制备的磷硼杂链预聚物嵌段聚氨酯水性共聚物、12.5g水性黑色染料、3.5g滑石粉,加入混合容器中搅拌混合,加入 15.0ml水复合溶剂(水、乙醇和乙二醇二丁醚的体积比为3:1:2的混合物) 搅匀,将得到的混合液倾入砂磨机中,启动砂磨机,保持转速5000r/min、冷却水温≤30℃,研磨30min;
S2、以细度刮板仪检测研磨至细度≤40μm后,加入3.0g磷酸三丁脂和10.0ml水复合溶剂(水、乙醇和乙二醇二丁醚的体积比为3:1:2的混合物),继续研磨5min,将涂料的粘度调节至1000Cp(25℃),停砂磨机,过滤出料,得到磷硼杂链预聚物嵌段聚氨酯水性印染防火涂料。
性能测试
采用上述实施例所得磷硼杂链预聚物聚氨酯嵌段共聚物制备的防火涂料阻燃处理的涤纶织物性能进行测试,具体方法为GB/T3917.1-2009、 GB5454-1997、GB/T4744-1997,测得各项性能指标结果见表1。
表1
样品 | 撕破强力(N) | LOI | 渗水性(mm) |
市售未经防火涂料涂饰处理涤纶布 | 15 | 17.0 | 720 |
防火涂料涂饰处理涤纶布(第一实施例) | 18 | 27.0 | 100 |
防火涂料涂饰处理涤纶布(第二实施例) | 16 | 29.0 | 110 |
防火涂料涂饰处理涤纶布(第三实施例) | 18 | 28.0 | 120 |
由表1可见,经实施例制备防火涂料涂饰处理后,市售未经防火涂料涂饰处理涤纶布,撕破强力、阻燃氧指数与渗水性能得到很大提高。
以上所述仅为本发明的优选实施例而已,并不用于限制本发明,尽管参照前述实施例对本发明进行了详细的说明,对于本领域的技术人员来说,其依然可以对前述各实施例所记载的技术方案进行修改,或者对其中部分技术特征进行等同替换。凡在本发明的精神和原则之内,所作的任何修改、等同替换、改进等,均应包含在本发明的保护范围之内。
Claims (10)
1.一种硼杂链羟端基预聚物嵌段聚氨酯共聚物水性印染防火涂料,其特征在于,按质量百分数计,该涂料的原料组成包括:11.5~13.5%颜料或染料、3.0~4.0%填料,83.5~84.5%磷硼杂链预聚物嵌段聚氨酯水性共聚物;
所述磷硼杂链预聚物嵌段聚氨酯水性共聚物的制备方法包括步骤:
(1)将有机溶剂、磷硼杂链预聚物、二月桂酸二丁基锡混合后在保护气氛与加热条件下保温,待体系温度均匀后加入甲苯二异氰酸酯和二羟甲基丙酸,并将体系升温后保温,分离溶剂;
(2)将体系降温后加入中和剂和水,搅拌后调整pH值至合格,即得。
2.根据权利要求1所述的防火涂料,其特征在于,所述填料包括纳米碳酸钙、滑石粉、膨润土、纳米凹凸棒土中的至少一种;或者,所述涂料的细度≤40μm。
3.根据权利要求1所述的防火涂料,其特征在于,所述涂料的原料组成还包括助剂,优选地,所述助剂包括消泡剂,更优选为聚甲基硅油、磷酸三丁酯中的至少一种,优选地,所述消泡剂用量为涂料配方总质量的1~2%;
或者,所述涂料的原料组成还包括水复合溶剂;
优选地,所述水复合溶剂的添加量以25℃下,将涂料的粘度用水调节至1000~1500Cp为准;
优选地,所述水复合溶剂为水、乙醇和乙二醇二甲醚的混合体系,更优选地,所述水、乙醇和乙二醇二丁醚的体积比为3:1:2;
优选地,所述有机溶剂包括二甲苯、甲苯、环己酮中的任意一种。
4.根据权利要求1所述的防火涂料,其特征在于,步骤(1)中,按质量百分数计,所述磷硼杂链预聚物、甲苯二异氰酸酯、二羟甲基丙酸的添加比例依次序为:75.9~76.9%、16.2~17.3%、6.8~6.9%;
或者,步骤(1)中,所述二月桂酸二丁基锡与甲苯二异氰酸酯物质的量比为1:0.01~0.03;
或者,步骤(1)中,所述磷硼杂链预聚物的数均分子量为1500~2500、分布指数为1.1~1.2;
或者,步骤(1)中,所述保护气氛包括氮气或氩气等惰性气体。
5.根据权利要求1所述的防火涂料,其特征在于,步骤(1)中,所述加热温度为60~65℃,加热方式为水浴加热,保温时间为20~35min;
或者,步骤(1)中,所述体系升温后温度为70~75℃,保温时间为1.5~2.5h。
6.根据权利要求1所述的防火涂料,其特征在于,步骤(2)中,所述中和剂包括一乙醇胺、二乙醇胺、一乙胺、二乙胺中的至少一种;
或者,步骤(2)中,所述体系降温后温度为45~50℃;
或者,步骤(2)中,所述pH值保持在7.5~9.0范围内。
8.根据权利要求7所述的防火涂料,其特征在于,所述式(1)中,R包括-HCH2CH2OH、-(CH2CH2OH)2、-HCH2CH3、-(CH2CH3)2中的任意一种。
9.权利要求1-8任一项所述的磷硼杂链羟端基预聚物嵌段聚氨酯共聚物水性印染防火涂料的制备方法,其特征在于,包括:将所述颜料或染料、填料、磷硼杂链预聚物嵌段聚氨酯水性共聚物混合均匀,磨细后再以水复合溶剂调节粘度,即得。
10.权利要求1-8任一项所述的磷硼杂链羟端基预聚物嵌段聚氨酯共聚物水性印染防火涂料在布料产品的制备中的应用。
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