CN106087427A - 一种防静电、阻燃安全作业服面料的制备方法 - Google Patents
一种防静电、阻燃安全作业服面料的制备方法 Download PDFInfo
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- CN106087427A CN106087427A CN201610415029.5A CN201610415029A CN106087427A CN 106087427 A CN106087427 A CN 106087427A CN 201610415029 A CN201610415029 A CN 201610415029A CN 106087427 A CN106087427 A CN 106087427A
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- antistatic
- fabric
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- retarding
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- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
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- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
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- D06M11/55—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with sulfur, selenium, tellurium, polonium or compounds thereof with sulfur trioxide; with sulfuric acid or thiosulfuric acid or their salts
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- Polymers & Plastics (AREA)
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- Health & Medical Sciences (AREA)
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- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
- Artificial Filaments (AREA)
Abstract
本发明涉及一种防静电、阻燃安全作业服面料的制备方法,包括:将阻燃共聚酯FR‑PET干燥切片,熔融纺丝,拉伸,得到阻燃涤纶纤维;然后将阻燃涤纶纤维与纤维素纤维按质量比为60~90:40~10进行混纺成纱线,得到阻燃面料;将含锌无机物A加入到防静电整理剂PEE中,搅拌溶解,30~100℃条件下边搅拌边加入季铵盐或吡啶鎓盐J,搅拌均匀,得到防静电剂PEEJ;将防静电剂PEEJ加入到60℃温水中,调节pH至4,得到浓度为1~10g/L的整理液;然后阻燃面料在整理液中两浸两轧,经过预烘和烘焙,即得。本发明的方法攻克了涤棉织物阻燃和抗静电功能难以复合的关键技术,且手感良好。
Description
技术领域
本发明属于安全作业服面料的制备领域,特别涉及一种防静电、阻燃安全作业服面料的制备方法。
背景技术
随着纺织品使用范围的扩展和用量的增加,由纺织品易燃性造成的火灾损失和人员伤亡,已引起世界各国的重视。据我国1994年统计,共发生火灾39120起,损失超过12.4亿元。其中煤矿10人以上事故共计78起,其中爆炸事故有51起,死亡人数占总死亡人数的70%,电火花占事故原因的60.42%。工作服的静电火花可成为燃烧爆炸事故的点火源,静电是物质的接触、分离或相互摩擦时产生静电的现象,例如在生产过程中的挤压、切割、搬运、搅拌和过滤,以及生活中的行走、起立、脱衣等,都会产生静电。大多数合成纤维都是低导电性的,它们会因为摩擦而产生静电,由这样的合成纤维织成的织物在使用时可带10kV以上的高电位,对人体和产品会产生影响和伤害;半合成纤维与天然纤维具有较高的吸湿性,与合成纤维相比,由摩擦引起的问题相对较少,但是它们在低湿度的条件下也会和合成纤维一样产生静电。随着我国经济快速发展和劳动安全防护意识的不断提高,化工、煤炭、石油、兵工等行业的一些易燃、易爆工作场所,对防护服及工业用布的防静电、阻燃性能提出了越来越高的要求。要消除一般工作服的这两个危险因素,劳动者必须穿着防静电阻燃服。而目前来看,我国的防静电阻燃安全作业服的产品合格率仍然不高,尤其缺乏双防护高性能的防静电阻燃服。因此,研究开发防静电阻燃双重功能工作服是防止易燃、易爆工作岗位重大事故的当务之急。
织物的防静电性能可以通过以下几种方式来赋予:(1)织物中嵌入导电纤维,导电纤维的防静电机理是利用逸散性,使导电纤维接近带电物体时,就会在其周围形成电场,由于电晕放电在空气中形成离子,使带电物体的电荷被极性相反的离子中和,而相同极性的离子被带电物体排斥,在空气中扩散向接地物体移动,带电物质与接地物体间形成通路,使带电物体的静电荷得到消除。但是目前采用的进口导电纤维价格较高,服装的生产成本远远高于使用传统助剂防静电的服装产品,所以现在仅仅限用于高档产品的生产,而国产导电纤维使用的面还并不广泛。(2)在合成纤维聚合物内部添加防静电剂,如磷酸酯、磺酸盐等表面活性剂,或是引入第三单体,如聚氧乙烯及其衍生物,以使纤维本身具有防静电效果。添加在聚合物内部的防静电剂大多数具有极性基团,这些极性基团在聚合体的外层形成导电层或通过氢键与空气中水分相结合,使聚合体的电阻减少,加速静电荷的散逸。防静电纤维的防静电机理是由于吸湿使静电泄漏,这种技术不仅能改善纤维及织物的防静电性,还能改善吸湿性、防污性等,具有多性能化的特征。但其防静电性主要是依靠吸收空气中的水分来实现,此防静电效果与环境的湿度密切相关,即在低湿度下几乎失去其防静电性,致使它的应用范围受到限制。(3)对织物进行防静电后整理,防静电剂整理是将防静电剂施加于织物表面,增加纤维的亲水性,防止静电在纤维上的积聚。防静电剂通常对纤维具有两种作用:①表面离子化:这类离子型整理剂受纤维表面层含水的作用,发生电离,变成导电,而能降低静电的积聚;②定向排列:按纤维不同,整理剂(表面活性剂)在织物表面排列不一。对棉而言,整理剂的亲水端吸附于棉表面,而疏水基却向外排列,所以反会增加静电。但对涤纶而言,恰恰相反,疏水基吸附于涤纶的表面,而亲水基却向外排列成一层吸水层,从而提高了导电性,具有防静电效果。这种防静电整理方法,与其他方法相比,其加工流程短,投资少,见效快。在当今市场上纺织品种日新月异的形势下,在增强市场竞争力的纺织新品种的开发中,后整理加工方法是极为有利的。
涤纶织物的阻燃的方法有很多种,按照生产过程和阻燃剂的引入方式,归类涤纶的阻燃方式有以下五种:(1)共聚法,在酯交换或缩聚阶段加入反应型阻燃剂进行共缩聚。它能够达到比较长久的阻燃效果,毒性低,且对织物的机械性能影响较小。(2)共混法,在融熔纺丝前向在熔体中加入添加型阻燃剂。共混法的优点是简单易行,操作费用低,缺点是耐久阻燃性比共聚法要差,不容易找到合适的添加型阻燃剂。(3)复合纺丝阻燃改性法,以普通聚酯与含阻燃成分的聚酯进行复合纺丝。对于那些耐水解性差,如部分磷共聚改性阻燃聚酯特别适合这种纺丝方法。但这种方法的成本较高,所以并未普遍应用到工业上。(4)接枝共聚法,反应型阻燃剂在涤纶或织物上进行接枝共聚。但接枝共聚要求技术条件和生产成本都高,因而不易被普遍采用,接枝法到目前还无工业化的先例。(5)后整理法,后处理法主要有浸轧焙烘法、涂层法、喷雾法等,使阻燃剂固着在织物上,获得阻燃效果。虽然后整理工艺较为简单,但是后整理法获得的阻燃效果通常不够耐久。
综观近年来国内外在防静电、阻燃织物研究中所采取的主要技术路线及其存在的问题,大致有以下几种:一是对棉或涤/棉等材料的织物采用防静电剂和阻燃剂进行后整理。由于并存于织物上的有机防静电剂和有机阻燃剂的相互作用,往往使其防静电、阻燃性能劣化,并使织物强度大为降低、手感粗糙发硬,同时这种织物的耐洗涤性能甚差,难以达到实用化的程度。二是对织物采用防静电、阻燃涂层处理,即在织物表面均匀地形成一层防静电与阻燃的膜状覆盖物。此法在一定程度上提高了织物双防性能的耐久性,强度也有所改善,但涂层易老化、防静电阻燃性能不佳。三是使导电纤维长丝嵌入普通织物中,再对织物进行阻燃后整理。这种方法是可获得比较好的防静电、阻燃性能的,但是阻燃的耐洗涤性差,特别是织物强度降低、增重大、粗糙厚硬的缺陷比较严重。四是使阻燃纤维制成织物后,再在织物中嵌织导电纤维长丝,来赋予织物双防功能.这种法避开了对织物的阻燃剂后处理,使双防织物的强度和手感均都有一定改善。但是制成的织物吸湿透气性能差、服用性能不够理想,而且工艺复杂、成本高。
发明内容
本发明所要解决的技术问题是提供一种防静电、阻燃安全作业服面料的制备方法,该方法在保证织物具有良好的防静电和阻燃性能的前提下,使织物同时具有质轻、轻柔的手感和充分的耐洗涤性。
本发明的一种防静电、阻燃安全作业服面料的制备方法,包括:
(1)将阻燃共聚酯FR-PET聚对苯二甲酸乙二醇干燥切片,熔融纺丝,拉伸,得到阻燃涤纶纤维;然后将阻燃涤纶纤维与纤维素纤维按质量比为60~90:40~10进行混纺成纱线,得到阻燃面料;
(2)将含锌无机物A加入到防静电整理剂聚对苯二甲酸乙二酯PEE中,搅拌溶解,30~100℃条件下边搅拌边加入物质J,搅拌均匀,得到防静电剂PEEJ;其中,物质J为季铵盐或吡啶鎓盐;
(3)将步骤(2)中的防静电剂PEEJ加入到60℃温水中,调节pH至4,得到浓度为1~10g/L的整理液;然后将步骤(1)阻燃面料在整理液中两浸两轧,然后经过预烘和烘焙,得到防静电、阻燃安全作业服面料。
所述步骤(1)中FR-PET的制备过程包括:2-羧乙基苯基次膦酸CEPPA的预酯化和阻燃PET共聚酯的合成;其中,阻燃PET共聚酯的合成包括酯化阶段和缩聚阶段。
所述2-羧乙基苯基次膦酸CEPPA的预酯化:称取1~5kg的2-羧乙基苯基次膦酸(CEPPA),按照乙二醇(EG):2-羧乙基苯基次膦酸(CEPPA)=1~5的摩尔比,称取一定量的EG,将物料放入已经洗好的反应釜内,内温保持100~400℃,反应1~5h。预酯化的产物为聚2-羧乙基苯基次膦酸乙二醇酯(CEPPA-EG),预酯化避免了阻燃剂在加工过程中因高温而造成分解。
所述阻燃PET共聚酯的合成:采用直接酯化—缩聚连续工艺路线,阻燃共聚酯聚合加工具体工艺流程如图1所示。
酯化阶段:预酯化完成后,于5L反应釜中的预酯化阻燃剂(CEPPA-EG)酯化液中加入对苯二甲酸PTA、稳定剂磷酸三甲酯TMP(0.1~1kg/kgPTA)、调色剂醋酸钴CoAc2·4H2O(0.1~1kg/kgPTA)、缩聚催化剂Sb2O3(0.1~1g/kgPTA)。打浆10~60min,升温至100~700℃,压力保持0.1Mp~1Mp,反应1~8h。酯化的产物为聚对苯二甲酸乙二醇及聚2-羧乙基苯基次膦酸乙二醇酯的嵌段共聚物。
缩聚阶段:酯化阶段结束后,升温至100~500℃,常压蒸过量的乙二醇EG约30min,然后进入抽真空阶段,此阶段分为低真空阶段和高真空阶段两个阶段。低真空阶段即釜内常压状态向高真空状态转变阶段,低真空至-0.08MPa。这个阶段完成后进入后真空度低于100Pa的高真空阶段,进行缩聚反应。缩聚阶段釜内温度控制在100~500℃。搅拌电机转速恒定,当达到一定值时充入氮气保护,停止反应,出料。
所述步骤(1)中丝速率:1000~5000m/min温度:一区150~300℃、二区200~400℃、三区200~400℃、联苯温度200~400℃、箱体温度200~400℃;拉伸的条件为:拉伸倍数1~2。
所述步骤(1)中纤维素纤维为棉或粘胶;阻燃面料为阻燃涤棉或涤粘面料。
所述步骤(2)中含锌无机物A为氧化锌、氯化锌、硫酸锌中的一种,A的加入量为PEE质量的5~30倍。
所述步骤(2)中防静电整理剂PEE的制备方法包括:(i)酯交换反应:在三口烧瓶中加入1~5kg对苯二甲酸二甲酯,1~5kg乙二醇和0.1~0.5kg对甲基苯磺酸,升温至有甲醇馏出,至酯交换结束(150~250℃,恒温反应2~5h);(ii)共缩聚反应:抽真空,向反应体系中加入1~5kg聚乙二醇和催化剂0.1~0.5kg,通入氮气并升温至100~500℃,减压蒸馏进行聚合反应,得防静电剂PEE。
所述防静电整理剂PEE对步骤(1)中得到的阻燃面料进行后整理:
整理液的配制方法:称取50~100g防静电剂PEE加入到烧杯内,加入一定量的温水(60℃),同时不停地搅拌,直至PEE完全溶解。然后加水并调节pH值至4,配制成浓度为1~10g/L的整理液。
防静电整理工艺:织物在整理液中两浸两轧(轧余率约为70~90%)→预烘(100℃)→高温焙烘(150~200℃,30~60s)。
结果证明,因为聚醚酯防静电剂PEE具有与涤纶相似的结构,可以与涤纶共熔共晶,具有良好的耐久性和防静电效果,但经整理的织物在手感上却有所下降。
所述步骤(2)中物质J为十六烷基三甲基氯化铵,十六烷基三甲基溴化铵,苯甲基氯吡啶鎓,鲸蜡基氯吡啶鎓中的一种。
所述步骤(2)中物质J与PEE的质量比为5~20:1~5。
所述步骤(2)中PEEJ的详细制备包括:称取一定量的防静电剂PEE加入到烧杯内,加入助剂A(自制),用量为PEE的5~30倍,不断搅拌,使PEE完全溶解,在溶液温度为30~100℃时,边搅拌边缓缓加入一定量的物质J,物质J的用量与PEE的质量比为5~20:1~5,搅拌均匀后停止,此即为防静电剂PEEJ。
所述步骤(3)中两浸两轧的轧余率为70~90%。
所述步骤(3)中预烘的温度为100~150℃,时间为5~15min。
所述步骤(3)中烘焙的温度为150~200℃,时间为30~60s。
经过防静电整理剂PEEJ整理后的阻燃涤棉面料的阻燃性能测试是根据GB8965.1《防护服装阻燃防护第1部分:阻燃服》的规定试验,热防护系数TPP达到A级标准;续燃时间、阴燃时间、损毁长度、熔融低落情况也达到A级标准;防静电性能根据GB12014-2009《防静电服》规定的方法测试,其防静电性能达A级标准;且手感优良。
本发明首先发明阻燃聚酯纤维,然后将阻燃聚酯纤维纱线、与棉混纺制成织物后,再对织物进行防静电后处理,在保证织物具有良好的防静电和阻燃性能的前提下,使双方织物同时具有质轻、轻柔的手感和充分的耐洗涤性。
有益效果
本发明制备阻燃共聚酯纤维,然后将阻燃聚酯纤维纱线、与棉混纺制成涤棉阻燃面料,合成防静电整理剂PEEJ后对涤棉阻燃面料进行防静电后处理,攻克了涤棉织物阻燃和抗静电功能难以复合的关键技术,且手感良好。
附图说明
图1为阻燃共聚酯聚合加工具体工艺流程图。
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。此外应理解,在阅读了本发明讲授的内容之后,本领域技术人员可以对本发明作各种改动或修改,这些等价形式同样落于本申请所附权利要求书所限定的范围。
实施例1
(1)阻燃共聚酯(FR-PET)的合成
(i)2-羧乙基苯基次膦酸(CEPPA)的预酯化
称取1kg的2-羧乙基苯基次膦酸(CEPPA),按照乙二醇(EG):2-羧乙基苯基次膦酸(CEPPA)=2:1的摩尔比,称取0.58kg的EG,将物料放入已经洗好的反应釜内,内温保持200℃,反应3h;预酯化的产物为聚2-羧乙基苯基次膦酸乙二醇酯(CEPPA-EG)。
(ii)阻燃PET共聚酯的合成
酯化阶段:预酯化完成后,按照乙二醇(EG):对苯二甲酸(PTA)=3:1的摩尔比,将0.52kg的对苯二甲酸PTA、和0.1kg稳定剂磷酸三甲酯TMP、0.1kg调色剂醋酸钴CoAc2·4H2O、0.1g缩聚催化剂Sb2O3加入5L反应釜;打浆60min,升温至300℃,压力保持0.4Mp,反应5h;酯化的产物为聚对苯二甲酸乙二醇及聚2-羧乙基苯基次膦酸乙二醇酯的嵌段共聚物。
缩聚阶段:酯化阶段结束后,升温至400℃,常压蒸过量的EG约30min,然后进入抽真空阶段,此阶段分为低真空阶段和高真空阶段两个阶段。低真空阶段即釜内常压状态向高真空状态转变阶段,低真空至-0.08MPa。这个阶段完成后进入后真空度低于100Pa的高真空阶段,进行缩聚反应。缩聚阶段釜内温度控制在300℃。搅拌电机转速恒定,充入氮气保护,停止反应,出料。
(2)将阻燃共聚酯(FR-PET)通过干燥切片、熔融纺丝(丝速率:2000m/min;温度:一区150℃、二区200℃、三区200℃、联苯温度300℃、箱体温度250℃)、拉伸变形(拉伸倍数1)等步骤,得到阻燃涤纶纤维,然后将阻燃涤纶与棉以65:35的质量比混纺成纱线,织成阻燃涤棉面料。
(3)防静电整理剂的合成
(i)酯交换反应:在三口烧瓶中加入1kg对苯二甲酸二甲酯,1kg乙二醇和0.1kg对甲基苯磺酸,升温至有甲醇馏出,150℃,恒温反应2h至酯交换结束;
(ii)共缩聚反应:抽真空,向反应体系中加入1kg聚乙二醇和催化剂0.1kg,通入氮气并升温至500℃,减压蒸馏进行聚合反应,得到防静电剂PEE。
(iii)称防静电剂PEE加入到烧杯内,加入氧化锌,用质量为PEE的10倍质量,不断搅拌,使PEE完全溶解,在溶液温度为100℃时,边搅拌边缓缓加入十六烷基三甲基氯化铵J,物质J的用量与PEE的质量比为2:1,搅拌均匀后停止,即为防静电剂PEEJ。
(4)防静电整理剂对阻燃涤棉织物进行后整理
(i)防静电整理剂液的配制:称取50g防静电剂PEEJ加入到烧杯内,加入60℃温水,同时不停地搅拌,直至PEEJ完全溶解,然后加水,并调节pH值至4,配制成浓度为5g/L的整理液。
(ii)防静电整理工艺:织物在整理液中两浸两轧(轧余率约为80%)→预烘(100℃,时间5min)→高温焙烘(160℃,30s)。
(iii)经过防静电整理剂PEEJ整理后的阻燃涤棉面料的阻燃性能测试、防静电性能测试、及手感评判。
实施例2
(1)阻燃共聚酯(FR-PET)的合成
(i)2-羧乙基苯基次膦酸(CEPPA)的预酯化
称取1kg的2-羧乙基苯基次膦酸(CEPPA),按照乙二醇(EG):2-羧乙基苯基次膦酸(CEPPA)=3:1的摩尔比,称取0.58kgEG,将物料放入已经洗好的反应釜内,内温保持200℃,反应3h。预酯化的产物为聚2-羧乙基苯基次膦酸乙二醇酯(CEPPA-EG)。
(ii)阻燃PET共聚酯的合成
酯化阶段:预酯化完成后,按照乙二醇(EG):对苯二甲酸(PTA)=2:1的摩尔比,将0.52kg的对苯二甲酸PTA、和0.1kg稳定剂磷酸三甲酯TMP、0.1kg调色剂醋酸钴CoAc2·4H2O、0.1g缩聚催化剂Sb2O3加入5L反应釜;打浆40min,升温至200℃,压力保持0.3Mp,反应5h;酯化的产物为聚对苯二甲酸乙二醇及聚2-羧乙基苯基次膦酸乙二醇酯的嵌段共聚物。
缩聚阶段:酯化阶段结束后,升温至300℃,常压蒸过量的EG约30min,然后进入抽真空阶段,此阶段分为低真空阶段和高真空阶段两个阶段。低真空阶段即釜内常压状态向高真空状态转变阶段,低真空至-0.08MPa。这个阶段完成后进入后真空度低于100Pa的高真空阶段,进行缩聚反应。缩聚阶段釜内温度控制在400℃。搅拌电机转速恒定,充入氮气保护,停止反应,出料。
(2)将阻燃共聚酯(FR-PET)通过干燥切片、熔融纺丝(丝速率:3000m/min;温度:一区250℃、二区200℃、三区400℃、联苯温度300℃、箱体温度350℃)、拉伸变形(拉伸倍数1)等步骤,得到阻燃涤纶纤维,然后将阻燃涤纶与粘胶以质量比67:33的比例混纺成纱线,织成阻燃涤粘面料。
(3)防静电整理剂的合成
(i)酯交换反应:在三口烧瓶中加入1kg对苯二甲酸二甲酯,0.8kg乙二醇和0.1kg对甲基苯磺酸,升温至有甲醇馏出,200℃,恒温反应2h至酯交换结束;
(ii)共缩聚反应:抽真空,向反应体系中加入1.5kg聚乙二醇和催化剂0.1kg,通入氮气并升温至300℃,减压蒸馏进行聚合反应,得到防静电剂PEE。
(iii)称防静电剂PEE加入到烧杯内,加入氯化锌,用质量为PEE的10倍的质量,不断搅拌,使PEE完全溶解,在溶液温度为100℃时,边搅拌边缓缓加入十六烷基三甲基溴化铵J,物质J的用量与PEE的质量比为4:1,搅拌均匀后停止,即为防静电剂PEEJ。
(4)防静电整理剂对阻燃涤粘织物进行后整理
(i)防静电整理剂液的配制:称取50g防静电剂PEEJ加入到烧杯内,加入60℃温水,同时不停地搅拌,直至PEEJ完全溶解,然后加水,并调节pH值至4,配制成浓度为10g/L的整理液。
(ii)防静电整理工艺:织物在整理液中两浸两轧(轧余率约为80%)→预烘(100℃,时间6min)→高温焙烘(160℃,60s)。
(iii)经过防静电整理剂PEEJ整理后的阻燃涤粘面料的阻燃性能测试、防静电性能测试、及手感评判。
实施例3
(1)阻燃共聚酯(FR-PET)的合成
(i)2-羧乙基苯基次膦酸(CEPPA)的预酯化
称取1kg的2-羧乙基苯基次膦酸(CEPPA),按照乙二醇(EG):2-羧乙基苯基次膦酸(CEPPA)=1.5:1的摩尔比,称取0.6kg的EG,将物料放入已经洗好的反应釜内,内温保持250℃,反应2h;预酯化的产物为聚2-羧乙基苯基次膦酸乙二醇酯(CEPPA-EG)。
(ii)阻燃PET共聚酯的合成
酯化阶段:预酯化完成后,按照乙二醇(EG):对苯二甲酸(PTA)=4:1的摩尔比,将0.52kg的对苯二甲酸PTA、和0.5kg稳定剂磷酸三甲酯TMP、0.3kg调色剂醋酸钴CoAc2·4H2O、0.4g缩聚催化剂Sb2O3加入5L反应釜;打浆30min,升温至300℃,压力保持0.3Mp,反应1h;酯化的产物为聚对苯二甲酸乙二醇及聚2-羧乙基苯基次膦酸乙二醇酯的嵌段共聚物。
缩聚阶段:酯化阶段结束后,升温至300℃,常压蒸过量的EG约30min,然后进入抽真空阶段,此阶段分为低真空阶段和高真空阶段两个阶段。低真空阶段即釜内常压状态向高真空状态转变阶段,低真空至-0.08MPa。这个阶段完成后进入后真空度低于100Pa的高真空阶段,进行缩聚反应。缩聚阶段釜内温度控制在200℃。搅拌电机转速恒定,充入氮气保护,停止反应,出料。
(2)将阻燃共聚酯(FR-PET)通过干燥切片、熔融纺丝(丝速率:4000m/min;温度:一区300℃、二区300℃、三区200℃、联苯温度200℃、箱体温度250℃)、拉伸变形(拉伸倍数2)等步骤,得到阻燃涤纶纤维,然后将阻燃涤纶与棉以70:30的质量比混纺成纱线,织成阻燃涤棉面料。
(3)防静电整理剂的合成
(i)酯交换反应:在三口烧瓶中加入2kg对苯二甲酸二甲酯,1.8kg乙二醇和0.5kg对甲基苯磺酸,升温至有甲醇馏出,200℃,恒温反应3h至酯交换结束;
(ii)共缩聚反应:抽真空,向反应体系中加入2kg聚乙二醇和催化剂0.1kg,通入氮气并升温至250℃,减压蒸馏进行聚合反应,得到防静电剂PEE。
(iii)称防静电剂PEE加入到烧杯内,加入硫酸锌,用质量为PEE的15倍的质量,不断搅拌,使PEE完全溶解,在溶液温度为100℃时,边搅拌边缓缓加入苯甲基氯吡啶鎓J,物质J的用量与PEE的质量比为10:1,搅拌均匀后停止,即为防静电剂PEEJ。
(4)防静电整理剂对阻燃涤棉织物进行后整理
(i)防静电整理剂液的配制:称取50g防静电剂PEEJ加入到烧杯内,加入60℃温水,同时不停地搅拌,直至PEEJ完全溶解,然后加水,并调节pH值至4,配制成浓度为5g/L的整理液。
(ii)防静电整理工艺:织物在整理液中两浸两轧(轧余率约为80%)→预烘(100℃,时间10min)→高温焙烘(160℃,40s)。
(iii)经过防静电整理剂PEEJ整理后的阻燃涤棉面料的阻燃性能测试、防静电性能测试、及手感评判。
实施例4
(1)阻燃共聚酯(FR-PET)的合成
(i)2-羧乙基苯基次膦酸(CEPPA)的预酯化
称取1kg的2-羧乙基苯基次膦酸(CEPPA),按照乙二醇(EG):2-羧乙基苯基次膦酸(CEPPA)=2:1的摩尔比,称取0.58kg的EG,将物料放入已经洗好的反应釜内,内温保持180℃,反应3h;预酯化的产物为聚2-羧乙基苯基次膦酸乙二醇酯(CEPPA-EG)。
(ii)阻燃PET共聚酯的合成
酯化阶段:预酯化完成后,按照乙二醇(EG):对苯二甲酸(PTA)=1:1的摩尔比,将0.52kg的对苯二甲酸PTA、和0.1kg稳定剂磷酸三甲酯TMP、0.2kg调色剂醋酸钴CoAc2·4H2O、0.4g缩聚催化剂Sb2O3加入5L反应釜;打浆30min,升温至250℃,压力保持0.3Mp,反应3h;酯化的产物为聚对苯二甲酸乙二醇及聚2-羧乙基苯基次膦酸乙二醇酯的嵌段共聚物。
缩聚阶段:酯化阶段结束后,升温至350℃,常压蒸过量的EG约30min,然后进入抽真空阶段,此阶段分为低真空阶段和高真空阶段两个阶段。低真空阶段即釜内常压状态向高真空状态转变阶段,低真空至-0.08MPa。这个阶段完成后进入后真空度低于100Pa的高真空阶段,进行缩聚反应。缩聚阶段釜内温度控制在400℃。搅拌电机转速恒定,充入氮气保护,停止反应,出料。
(2)将阻燃共聚酯(FR-PET)通过干燥切片、熔融纺丝(丝速率:5000m/min;温度:一区150℃、二区300℃、三区200℃、联苯温度400℃、箱体温度400℃)、拉伸变形(拉伸倍数2)等步骤,得到阻燃涤纶纤维,然后将阻燃涤纶与棉以65:35的质量比混纺成纱线,织成阻燃涤棉面料。
(3)防静电整理剂的合成
(i)酯交换反应:在三口烧瓶中加入1kg对苯二甲酸二甲酯,1.8kg乙二醇和0.1kg对甲基苯磺酸,升温至有甲醇馏出,300℃,恒温反应1h至酯交换结束;
(ii)共缩聚反应:抽真空,向反应体系中加入2kg聚乙二醇和催化剂0.2kg,通入氮气并升温至250℃,减压蒸馏进行聚合反应,得到防静电剂PEE。
(iii)称防静电剂PEE加入到烧杯内,加入氧化锌,用量为PEE的8倍质量,不断搅拌,使PEE完全溶解,在溶液温度为100℃时,边搅拌边缓缓加入鲸蜡基氯吡啶鎓J,物质J的用量与PEE的质量比为5:1,搅拌均匀后停止,即为防静电剂PEEJ。
(4)防静电整理剂对阻燃涤棉织物进行后整理
(i)防静电整理剂液的配制:称取50g防静电剂PEEJ加入到烧杯内,加入60℃温水,同时不停地搅拌,直至PEEJ完全溶解,然后加水,并调节pH值至4,配制成浓度为13g/L的整理液。
(ii)防静电整理工艺:织物在整理液中两浸两轧(轧余率约为80%)→预烘(100℃,时间10min)→高温焙烘(160℃,30s)。
(iii)经过防静电整理剂PEEJ整理后的阻燃涤棉面料的阻燃性能测试、防静电性能测试、及手感评判。
Claims (10)
1.一种防静电、阻燃安全作业服面料的制备方法,包括:
(1)将阻燃聚对苯二甲酸乙二醇共聚酯FR-PET干燥切片,熔融纺丝,拉伸,得到阻燃涤纶纤维;然后将阻燃涤纶纤维与纤维素纤维按质量比为60~90:40~10进行混纺成纱线,得到阻燃面料;
(2)将含锌无机物A加入到聚醚酯型防静电整理剂PEE中,搅拌溶解,30~100℃条件下边搅拌边加入物质J,搅拌均匀,得到防静电剂PEEJ;其中,物质J为季铵盐或吡啶鎓盐;
(3)将步骤(2)中的防静电剂PEEJ加入到60℃温水中,调节pH至4,得到浓度为1~10g/L的整理液;然后将步骤(1)阻燃面料在整理液中两浸两轧,然后经过预烘和烘焙,得到防静电、阻燃安全作业服面料。
2.根据权利要求1所述的一种防静电、阻燃安全作业服面料的制备方法,其特征在于,所述步骤(1)中FR-PET的制备过程包括:2-羧乙基苯基次膦酸CEPPA的预酯化和阻燃PET共聚酯的合成;其中,阻燃PET共聚酯的合成包括酯化阶段和缩聚阶段。
3.根据权利要求1所述的一种防静电、阻燃安全作业服面料的制备方法,其特征在于,所述步骤(1)中熔融纺丝的条件为:丝速率为1000~5000m/min;温度为:一区150~300℃、二区200~400℃、三区200~400℃、联苯温度200~400℃、箱体温度200~400℃;拉伸条件为:拉伸倍数1~2。
4.根据权利要求1所述的一种防静电、阻燃安全作业服面料的制备方法,其特征在于,所述步骤(1)中纤维素纤维为棉或粘胶;阻燃面料为阻燃涤棉或涤粘面料。
5.根据权利要求1所述的一种防静电、阻燃安全作业服面料的制备方法,其特征在于,所述步骤(2)中含锌无机物A为氧化锌、氯化锌或硫酸锌,加入量为PEE质量的5~30倍。
6.根据权利要求1所述的一种防静电、阻燃安全作业服面料的制备方法,其特征在于,所述步骤(2)中防静电整理剂PEE的制备方法包括:(i)酯交换反应:对苯二甲酸二甲酯、乙二醇和对甲基苯磺酸混合,升温至150~250℃,有甲醇馏出,恒温反应2~5h;(ii)共缩聚反应:抽真空,向反应体系中加入聚乙二醇和催化剂,通入氮气并升温至100~500℃,减压蒸馏进行聚合反应,得到防静电整理剂PEE。
7.根据权利要求1所述的一种防静电、阻燃安全作业服面料的制备方法,其特征在于,所述步骤(2)中物质J与PEE的质量比为5~20:1~5。
8.根据权利要求1所述的一种防静电、阻燃安全作业服面料的制备方法,其特征在于,所述步骤(2)中物质J为十六烷基三甲基氯化铵,十六烷基三甲基溴化铵,苯甲基氯吡啶鎓或鲸蜡基氯吡啶鎓。
9.根据权利要求1所述的一种防静电、阻燃安全作业服面料的制备方法,其特征在于,所述步骤(3)中两浸两轧的轧余率为70~90%。
10.根据权利要求1所述的一种防静电、阻燃安全作业服面料的制备方法,其特征在于,所述步骤(3)中预烘的温度为100~150℃,时间为5~15min;烘焙的温度为150~200℃,时间为30~60s。
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CN108976400A (zh) * | 2018-08-07 | 2018-12-11 | 日华化学(中国)有限公司 | 一种含锌聚酯聚醚高分子化合物的合成制备方法 |
CN108976400B (zh) * | 2018-08-07 | 2020-07-28 | 日华化学(中国)有限公司 | 一种含锌聚酯聚醚高分子化合物的合成制备方法 |
CN109137124A (zh) * | 2018-08-30 | 2019-01-04 | 盛世瑶兰(深圳)科技有限公司 | 一种阻燃面料的制备方法 |
CN109137124B (zh) * | 2018-08-30 | 2020-12-22 | 昱天(上海)新材料有限公司 | 一种阻燃面料的制备方法 |
CN113089330A (zh) * | 2021-05-13 | 2021-07-09 | 苏州联胜化学有限公司 | 一种涤纶耐久阻燃剂及其制备方法和应用 |
CN113089330B (zh) * | 2021-05-13 | 2022-10-25 | 苏州联胜化学有限公司 | 一种涤纶耐久阻燃剂及其制备方法和应用 |
CN115262030A (zh) * | 2022-08-24 | 2022-11-01 | 清源创新实验室 | 一种阻燃夜光纤维及其制备方法 |
CN115262030B (zh) * | 2022-08-24 | 2023-12-05 | 清源创新实验室 | 一种阻燃夜光纤维及其制备方法 |
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