CN112342786A - 一种磷硼杂链预聚物嵌段聚氨酯织物阻燃水性上浆剂及其制备方法与应用 - Google Patents
一种磷硼杂链预聚物嵌段聚氨酯织物阻燃水性上浆剂及其制备方法与应用 Download PDFInfo
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Abstract
本发明涉及一种磷硼杂链预聚物嵌段聚氨酯织物阻燃水性上浆剂及其制备方法与应用,该水性上浆剂包括:11.0~15.0%聚乙醇、4.0~6.0%羧甲基纤维素、4.0~5.0%填料、75.0~80.0%磷硼杂链预聚物嵌段聚氨酯水性共聚物;所述水性共聚物的制备包括: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,将体系升温后保温,分离溶剂;2)将反应体系降温后加入中和剂和水,搅拌后调整pH值,即得。本发明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,得到适用于织物表面辊涂或喷涂的上浆剂。
Description
技术领域
本发明涉及纺织织物上浆剂技术领域,具体涉及一种磷硼杂链预聚物嵌段聚氨酯织物阻燃水性上浆剂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。
上浆剂是由成膜物质组成的浆状高分子分散体系,浆料浸轧整理织物附着于织物表面,经干燥成膜后包裹织物表面,从而赋予织物平滑厚实、丰满硬挺的手感,同时也因上浆剂组成体系中各种功能材料的应用,而赋予织物阻燃、防水和耐磨等特种功能。织物纤维(天然纤维和合成纤维)属于易燃物,遇明火容易燃烧,在使用过程中存在火灾隐患,织物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。
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公开了一种涤纶织物用阻燃抗熔滴整理剂及其阻燃抗熔滴整理方法,该阻燃抗熔滴整理剂能明显改善涤纶织物的阻燃性能,提高其极限氧指数,对涤纶织物的色度和强力影响小;经过阻燃整理的涤纶织物属于难燃材料,具有良好的耐洗性和耐久阻燃性,基本无熔滴现象,具有优异的阻燃抗熔滴性
文献2公开了一种阻燃织物及其制备方法,其利用层层自组装技术将带负电荷的纳米蒙脱土与带正电荷的高分子溶液或分散液交替沉积在织物表面制备具有阻燃功能的多层膜。
文献3公开了一种无溶剂制备阻燃棉织物的方法,该发明的阻燃整理剂不需要任何溶剂,工艺过程对环境和人体友好。在棉织物阻燃整理过程中及阻燃织物使用过程中均无甲醛释放,且在阻燃整理过程中,阻燃剂会和棉织物形成许多牢固的共价键,使得棉织物在获得高效阻燃的同时具有优异的耐水洗性。
文献4公开了一种棉用反应型硅磷氮协效阻燃拒水功能助剂的制备方法,该助剂可以用于棉织物的功能整理,赋予棉织物阻燃和拒水功能,是一种新型的染整助剂。
文献5公开了一种耐久阻燃织物整理液及耐久阻燃织物的制备方法,该发明提供的耐久阻燃织物整理液包括独立分装的DNA生物质阻燃整理液和金属盐整理液,制备的耐久阻燃织物具有较好的阻燃性能,且耐久性能优异。
目前,织物阻燃上浆剂技术具有以下特点:
①阻燃剂品种,无机物居多,有机物较少。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,因迁移造成环境的污染,发生火灾时因含卤高烟会造成更大的环境污染。
②阻燃剂形态,添加型居多,本征型较少。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201911396773.5,名称为一种涤纶织物用阻燃抗熔滴整理剂及其阻燃抗熔滴整理方法。
文献2:中国专利,申请号为201911378113.4,名称为一种阻燃织物及其制备方法。
文献3:中国专利,申请号为201910870314.X,名称为一种无溶剂制备阻燃棉织物的方法。
文献4:中国专利,申请号为201910449164.5,名称为一种棉用反应型硅磷氮协效阻燃拒水功能助剂的制备方法。
文献5:中国专利,申请号为201710806294.0,名称为一种耐久阻燃织物整理液及耐久阻燃织物的制备方法。
发明内容
本发明的目的是制备适合织物表面辊涂或喷涂的上浆剂,且经该上浆剂浸轧整理的织物具有低毒环保、低烟无卤、长效阻燃、爽滑耐磨和手感舒服等协效功能。
为此,本发明公开一种磷硼杂链预聚物嵌段聚氨酯织物阻燃水性上浆剂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,得到适用于织物表面辊涂或喷涂的上浆剂。
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)将分离去除了溶剂后的反应体系降温后加入中和剂和水,搅拌后调整体系pH值,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,步骤(1)中,所述磷硼杂链预聚物的粘度为1500~2000Cp(25℃),可选地,用水将所述磷硼杂链预聚物稀释成符合上述粘度要求的预聚物稀释液。
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:75.0~77.0%、16.0~17.0%、7.0~8.0%。
进一步地,步骤(1)中,所述二月桂酸二丁基锡用量为甲苯二异氰酸酯质量的3~5‰。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1500~2000、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、惰性气体等。
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℃,保温时间为1.5~2.5h,进一步提高缩聚反应的反应程度。
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。在本发明中,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。
在本发明的第三方面,公开一种磷硼杂链预聚物嵌段聚氨酯织物阻燃水性上浆剂,按质量百分数计,其原料组成包括:11.0~15.0%聚乙醇、4.0~6.0%羧甲基纤维素、4.0~5.0%填料、75.0~80.0%本发明所述磷硼杂链预聚物嵌段聚氨酯水性共聚物。
进一步地,所述填料包括碳酸钙、滑石粉、高岭土、膨润土中的至少一种。在本发明中,所述填料的主要作用是降低上浆剂干燥成膜后的收缩率,提高制品的表面光洁度、颜料的着色效果、降低成本,提高市场产品竞争力。
进一步地,所述水性上浆剂还包括助剂,包括消泡剂、分散剂等;可选地,所述消泡剂包括聚甲基硅油、磷酸三丁酯等中的至少一种,所述分散剂包括OP-10、聚乙二醇、十二烷基苯磺酸钠等中的至少一种;可选地,所述助剂的添加量为上浆剂总质量的3~5‰。
进一步地,所述上浆剂细度≤20μm,以便将上浆剂均匀涂在织物表面。
进一步地,所述上浆剂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调整上浆剂粘度在预设值为准。
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5:1:1。
在本发明的第四方面,公开所述硼杂链预聚物嵌段聚氨酯织物阻燃水性上浆剂的制备方法,包括:将所述聚乙醇、羧甲基纤维素、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,公开所述硼杂链预聚物嵌段聚氨酯织物阻燃水性上浆剂在织物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,本发明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,这种共聚物具有本征阻燃的特点。
(2)本发明以所述硼杂链羟端基预聚物嵌段聚氨酯共聚物为基料制备适用于织物表面辊涂或喷涂的上浆剂,经该上浆剂浸轧整理的织物具有低毒环保、低烟无卤、长效阻燃、爽滑耐磨和手感舒服等协效功能,这些效果是由于磷、硼元素在聚合物分子链中本征阻燃特点与聚氨酯弹性体耐磨柔韧性能相互协同作用导致的。
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采用申请号为201710836186.8的专利文献中方法合成,其数均分子量为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购买市售产品。
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、75g PDCP-DGB、占TDI质量3‰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,滴加17.0g TDI和8.0g DMPA,保持体系温度75±1℃,保温2h,分离回收上层二甲苯。
(3)将分离去除了二甲苯后的反应体系降温至45±1℃,然后加入一乙醇胺和50ml水,继续搅拌1h,调整pH=9.0,再以水将产物粘度调节至1500Cp(25℃),即得磷硼杂链预聚物嵌段聚氨酯水性共聚物稀释液。
2、一种磷硼杂链预聚物嵌段聚氨酯织物阻燃水性上浆剂的制备,包括如下步骤:
S1、称取75.0g本实施例制备的磷硼杂链预聚物嵌段聚氨酯水性共聚物稀释液、15.0g聚乙烯醇、6.0g纳米碳酸钙、4.0g羧甲基纤维素,2.0g OP-10,加入混合容器中搅拌混合,加入15ml水复合溶剂(水、乙醇和乙二醇二丁醚的体积比为5:1:1的混合物)搅匀,将得到的混合液胶体磨中,启动胶体磨,保持转速500r/min、冷却水温≤30℃,研磨10min;
S2、以细度刮板仪检测研磨至细度≤20μm,加入1.0g磷酸三丁脂和10.0ml水复合溶剂,继续研磨5min,测粘度合格,停胶体磨,过滤出料,得到磷硼杂链预聚物嵌段聚氨酯阻燃织物上浆剂。
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、77g PDCP-DGB、占TDI质量5‰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,滴加16.0g TDI和7.0g DMPA,保持体系温度75±1℃,保温1.5h,分离回收上层二甲苯。
(3)将分离去除了二甲苯后的反应体系降温至50±1℃,然后加入一乙醇胺和50ml水,继续搅拌1h,调整pH=8.0,再以水将产物粘度调节至1800Cp(25℃),即得磷硼杂链预聚物嵌段聚氨酯水性共聚物稀释液。
2、一种磷硼杂链预聚物嵌段聚氨酯织物阻燃水性上浆剂的制备,包括如下步骤:
S1、称取80.0g本实施例制备的磷硼杂链预聚物嵌段聚氨酯水性共聚物稀释液、11.0g聚乙烯醇、4.0g纳米碳酸钙、5.0g羧甲基纤维素,3.0g OP-10,加入混合容器中搅拌混合,加入15ml水复合溶剂(水、乙醇和乙二醇二丁醚的体积比为5:1:1的混合物)搅匀,将得到的混合液胶体磨中,启动胶体磨,保持转速500r/min、冷却水温≤30℃,研磨10min;
S2、以细度刮板仪检测研磨至细度≤20μm,加入2.0g磷酸三丁脂和10.0ml水复合溶剂,继续研磨5min,测粘度合格,停胶体磨,过滤出料,得到磷硼杂链预聚物嵌段聚氨酯阻燃织物上浆剂。
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、占TDI质量4‰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,滴加16.5g TDI和7.5g DMPA,保持体系温度70±1℃,保温2.5h,分离回收上层二甲苯。
(3)将分离去除了二甲苯后的反应体系降温至45±1℃,然后加入一乙胺和50ml水,继续搅拌1h,调整pH=7.5,再以水将产物粘度调节至2000Cp(25℃),即得磷硼杂链预聚物嵌段聚氨酯水性共聚物稀释液。
2、一种磷硼杂链预聚物嵌段聚氨酯织物阻燃水性上浆剂的制备,包括如下步骤:
S1、称取77.5g本实施例制备的磷硼杂链预聚物嵌段聚氨酯水性共聚物稀释液、12.0g聚乙烯醇、5.0g纳米碳酸钙、4.5g羧甲基纤维素,3.0g OP-10,加入混合容器中搅拌混合,加入15ml水复合溶剂(水、乙醇和乙二醇二丁醚的体积比为5:1:1的混合物)搅匀,将得到的混合液胶体磨中,启动胶体磨,保持转速500r/min、冷却水温≤30℃,研磨10min;
S2、以细度刮板仪检测研磨至细度≤20μm,加入2.0g磷酸三丁脂和10.0ml水复合溶剂,继续研磨5min,测粘度合格,停胶体磨,过滤出料,得到磷硼杂链预聚物嵌段聚氨酯阻燃织物上浆剂。
性能测试
对上述第一至第三实施例所得磷硼杂链预聚物聚氨酯嵌段共聚物制备的涂膜剂上浆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) |
市售未经上浆处理涤纶布 | 15 | 17.0 | 720 |
上浆处理涤纶布(第一实施例) | 18 | 27.0 | 100 |
上浆处理涤纶布(第二实施例) | 16 | 29.0 | 110 |
上浆处理涤纶布(第三实施例) | 18 | 28.0 | 120 |
由表1可见,经实施例制备施胶剂施胶处理后,市售未经上浆处理涤纶布的撕破强力、阻燃氧指数与渗水性能得到显著提高。
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)
1.一种磷硼杂链预聚物嵌段聚氨酯织物阻燃水性上浆剂,其特征在于,按质量百分数计,其原料组成包括:11.0~15.0%聚乙醇、4.0~6.0%羧甲基纤维素、4.0~5.0%填料、75.0~80.0%磷硼杂链预聚物嵌段聚氨酯水性共聚物;所述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)将分离去除了溶剂后的反应体系降温后加入中和剂和水,搅拌后调整体系pH值,即得。
2.根据权利要求1所述的水性上浆剂,其特征在于,所述填料包括碳酸钙、滑石粉、高岭土、膨润土中的至少一种。
3.根据权利要求1所述的水性上浆剂,其特征在于,所述水性上浆剂还包括助剂,优选为包括消泡剂、分散剂;
更优选地,所述消泡剂包括聚甲基硅油、磷酸三丁酯中的至少一种;
更优选地,所述分散剂包括OP-10、聚乙二醇、十二烷基苯磺酸黄中的至少一种;
更优选地,所述助剂的添加量为上浆剂总质量的3~5‰;
或者,所述上浆剂细度≤20μm,以便将上浆剂均匀涂在织物表面。
4.根据权利要求1所述的水性上浆剂,其特征在于,所述上浆剂的原料组成还包括水复合溶剂;
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5:1:1。
5.根据权利要求1所述的水性上浆剂,其特征在于,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、甲苯二异氰酸酯、二羟甲基丙酸的添加比例依次序为:75.0~77.0%、16.0~17.0%、7.0~8.0%;
或者,步骤(1)中,所述二月桂酸二丁基锡用量为甲苯二异氰酸酯质量的3~5‰。
6.根据权利要求1所述的水性上浆剂,其特征在于,步骤(1)中,所述有机溶剂包括二甲苯、甲苯、环己酮中的任意一种;
或者,步骤(1)中,所述磷硼杂链预聚物的粘度为25℃下1500~2000Cp,优选地,用水将所述磷硼杂链预聚物稀释成符合上述粘度要求的预聚物稀释液;
或者,步骤(1)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。
7.根据权利要求1所述的水性上浆剂,其特征在于,步骤(1)中,所述保护气氛包括氮气或惰性气体;
或者,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;
或者,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。
9.权利要求1-8任一项所述的硼杂链预聚物嵌段聚氨酯织物阻燃水性上浆剂的制备方法,其特征在于,包括:将所述聚乙醇、羧甲基纤维素、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任一项所述硼杂链预聚物嵌段聚氨酯织物阻燃水性上浆剂和/或权利要求9所述的制备方法得到的水性上浆剂在织物产品的制备中的应用。
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