CN114434909A - 一种高阻燃透气防护面料及其制备方法 - Google Patents
一种高阻燃透气防护面料及其制备方法 Download PDFInfo
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- CN114434909A CN114434909A CN202210168239.4A CN202210168239A CN114434909A CN 114434909 A CN114434909 A CN 114434909A CN 202210168239 A CN202210168239 A CN 202210168239A CN 114434909 A CN114434909 A CN 114434909A
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- retardant
- ramie fibers
- fibers
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Abstract
本发明涉及一种高阻燃透气防护面料及其制备方法,属于纺织面料技术领域。且所述高阻燃透气面料包括基布和基布表面粘合的阻燃层,所述基布以改性苎麻纤维和涤纶纤维纺织而成。本发明首先选用透气性能好的改性苎麻纤维为主要纤维,保证了基布的透气散热性能,且对苎麻纤维进行改性,提高了其弹性、抱合性和可纺性;其次,为了保证基布的透气性能,选择对基布的外层进行单侧改性,在基布外层接枝一层阻燃层;再次,所述阻燃层进行了单侧改性,提高阻燃层和基布之间的粘结性能;最后,阻燃层中含有阻燃剂,阻燃性能优异,且该阻燃剂含有含氟支链,赋予阻燃层高阻燃性能,耐水、耐化学试剂的性能。
Description
技术领域
本发明属于纺织面料技术领域,具体地,涉及一种高阻燃透气防护面料及其制备方法。
背景技术
普通的化纤合成纤维和天然纤维都比较容易燃烧,在消防、冶炼等高温行业,强大的辐射热能使普通服装迅速受热熔融、分解并燃烧,容易灼伤操作人员的肌肤,威胁其生命安全。阻燃服由于在面料中增加了阻燃纤维或者在面料上涂覆了阻燃剂,从而能够大大减慢燃烧速度,在移动后马上自行熄灭,而且燃烧部分迅速炭化而不产生熔融、滴落或穿洞,给人时间撤离燃烧现场或脱掉身燃烧的衣服,减少或避免烧伤烫伤,达到保护的目的。阻燃服因此成为高温作业人员的必要防护品之一。
一般的防火面料是采用阻燃材料或者在普通纤维中添加了阻燃成分制成,具有一定的防火性能,在装饰性防火墙布以及消防服中有所应用,但透气性欠佳,穿着舒适性差,消防等高温作业人员经常会暴露在火焰或高温中,他们需要的防护服或者防护制品除了能够耐高温以外,由于人体剧烈的运动使得人体的排汗量成倍排出,加之外部极高的环境温度,会使消防员产生极大的闷湿感,会严重影响消防员的作战效率。
如中国专利CN105113257A公开的一种防水透湿防火全涤纶PU防护面料,包括基布,所述基布的表面依次涂布有第一防水阻燃涂层、第二防水阻燃涂层、第三防水阻燃涂层和第四防水阻燃涂层。该发明中面料表面涂有多层阻燃涂层,其透气性必有所降低。
因此,本发明提供了一种阻燃性能好且透气性能好的防护面料及其制备方法。
发明内容
本发明的目的在于提供一种高阻燃透气防护面料及其制备方法。
本发明要解决的技术问题:现有防护面料中阻燃和透气性不能兼得的问题。
本发明的目的可以通过以下技术方案实现:
一种高阻燃透气防护面料,包括基布和基布表面粘合的阻燃层。
进一步地,所述基布以透气性能好的改性苎麻纤维和涤纶纤维纺织而成,利用苎麻纤维空隙大,透气好的特点,涤纶纤维模量高、强度高、弹性高、良好的保形性特点,使获得的基布具有透气渗湿和保型性好的特点;针对苎麻纤维素大分子取向度和结晶度较高,表面平直无卷曲,造成纤维刚性大、弹性小、抱合性能和可纺性能差的问题,本发明对苎麻纤维进行改性,得改性苎麻纤维。
进一步地,基布中改性苎麻纤维的含量为75-85%,涤纶纤维丝含量为15-25%,以苎麻纤维为主要纤维,保证了基布的透气散热性能,通过涤纶纤维的加入,提高基布的保形性。
进一步地,所述改性苎麻纤维通过以下步骤制成:
A1、将苎麻纤维置于质量分数18%氢氧化钠液中,室温下反应3h后,洗至中性,得碱处理苎麻纤维,其中,苎麻纤维和质量分数18%氢氧化钠液的质量比为1:30-40;
A2、将碱处理苎麻纤维置于混合溶液A中55℃下反应5h,依次水洗后经无水乙醇洗涤,再经水洗至中性,烘干,得醚化改性苎麻纤维,其中,碱处理苎麻纤维和混合溶液A的质量比为1:30-40;混合溶液A由环氧氯丙烷、质量分数5%的氢氧化钠溶液和无水乙醇按照3-4g:50g:3-5mL混合组成;
在上述反应中,利用苎麻纤维表面的羟基和环氧氯丙烷中的氯反应,将环氧基接枝到碱处理苎麻纤维表面;
A3、将醚化改性苎麻纤维置于混合溶液B中50℃下反应5h,经水洗、无水乙醇洗,再水洗至中性,得改性苎麻纤维,其中,醚化改性苎麻纤维和混合溶液B的质量比为1:30-40,混合溶液B由端氨基聚硅氧烷、碳酸氢钠和无水乙醇按照0.65-0.85mol:5-7g:100-120mL混合组成。
在上述反应中,利用醚化改性苎麻纤维表面的环氧基和端氨基聚硅氧烷中的氨基反应,将硅氧烷聚合链接入苎麻纤维表面,利用硅氧烷聚合链的柔软性,以及氨基,提高苎麻纤维的弹性、抱合性和可纺性。
进一步地,所述端氨基聚硅氧烷通过以下步骤制成:
在氮气气流的保护下,向四口烧瓶中,加入D4(八甲基环四硅氧烷)和催化剂苄基三甲基氢氧化胺甲醇溶液(0.5wt%),在磁力搅拌下,加热至50℃,加入封端剂,减压脱除体系中残余的水和甲醇,待体系粘度不变时,继续反应12h,继续升高温度至175℃破坏催化中心活性,后降温至150℃,负压脱除反应剩余的D4单体和低沸物小分子,得端氨基聚硅烷,其中,封端剂为1,3-双(3-氨基丙基)-1,1,3,3-四甲基二硅氧烷,D4、催化剂、封端剂的用量比为60g:0.6g:6-9g,端氨基聚硅氧烷的分子量为1000-1500。
进一步地,所述阻燃层通过以下步骤制成:
B1、将阻燃聚酯树脂粒和有机溶剂加入三口瓶中,在室温下持续搅拌至完全溶解,得阻燃聚酯溶液;将阻燃聚酯溶液经静电纺丝,待溶液纺丝完全后得阻燃聚酯膜,其中,阻燃聚酯树脂粒与有机溶剂的质量比为15-18:82-85,有机溶剂为丙酮和N,N-二甲基甲酰胺按照体积比为70-85:15-30进行混合的混合溶剂,其中,纺丝电压18kV,纺丝速率为0.6mL/h,纺丝接收距离为18cm,纺丝温度为28℃,纺丝湿度为35%;
B2、将阻燃聚酯膜的一侧用聚乙烯基胶带粘贴密封,对粘贴侧膜表面实施保护,并将单侧保护后的阻燃聚酯膜的未保护侧放入氧化剂溶液中,在95℃下对未保护侧进行7h氧化处理,得单侧氧化改性的阻燃层,其中氧化剂溶液为高锰酸钾粉末和质量分数68%的硝酸按照质量比1:1进行混合制成。
进一步地,所述阻燃聚酯树脂粒通过以下步骤制成:
C1、将甲基丙烯酸六氟丁酯、磷酸酯单体、1,1,1,3,3-四甲基硅烷和无水甲苯混合后,搅拌均匀,然后在氮气保护下,加热至96℃,然后加入氯铂酸异丙醇溶液,反应5h,反应结束后用活性炭吸附铂催化剂,过滤,旋蒸除去溶剂,得阻燃剂,其中,甲基丙烯酸六氟丁酯、磷酸酯单体、1,3,3-四甲基硅烷的摩尔比为1:1:1,氯铂酸异丙醇溶液的加入量为甲基丙烯酸六氟丁酯、磷酸酯单体和1,1,3,3-四甲基硅烷总质量的2-4%;
在C1反应中,利用烯烃类化合物和含氢硅烷的聚合反应,得阻燃剂,且该阻燃剂的分子结构式如下所示;
C2、将聚酯颗粒、阻燃剂和相容剂加入挤出机中,挤出造粒,得阻燃聚酯树脂粒,其中,挤出机的转速为200-400rpm,挤出温度为160-200℃,聚酯颗粒、阻燃剂、相容剂的质量比为100:15-30:1.5-4.5,相容剂为马来酸酐接枝聚乙烯、马来酸酐接枝聚丙烯中的一种,聚酯颗粒为PET颗粒。
在C2反应中,将C1反应得的阻燃剂加入聚酯颗粒中,经挤出造粒,得阻燃聚酯树脂粒,利用了阻燃剂与聚酯颗粒在相容剂的作用下混合挤出造粒,使得聚酯颗粒具有阻燃性能,首先,阻燃剂为线性聚合物,含有笼状磷酸酯结构和含氟支链,在相容剂和含氟支链的作用下该阻燃剂在聚酯体系中均匀分散,且因含有笼状磷酸酯结构、含氟支链和主链上的硅氧键,具有优异的阻燃性能。
进一步地,所述磷酸酯单体通过以下步骤制成:
D1、将季戊四醇、三氯氧磷和1,4-二氧六环加入带有机械搅拌、温度计、冷凝回流、干燥和氯化氢气体吸收装置的三口烧瓶中,升温至85℃,搅拌至无氯化氢气体产生,停止反应,冷却至室温,抽滤,沉淀用1,4-二氧六环和乙醇各洗涤两次,然后真空干燥至恒重,得笼状磷酸酯,其中,季戊四醇、三氯氧磷、1,4-二氧六环的用量比为0.11-0.13mol:0.1mol:40-60mL;
在上述反应中,利用季戊四醇中的醇羟基和三氯化磷中的氯反应,获得笼状磷酸酯,且其分子结构式如下所示;
D2、将笼状磷酸酯、乙腈、无水三氯化铝和三乙胺加入带有机械搅拌、冷凝回流、温度控制、氮气保护和恒压滴液漏斗的三口烧瓶中,加入烯丙基二甲基氯硅烷,在70℃下搅拌1.5h,再升温回流反应12h,停止反应,静置冷却至室温,抽滤,固体物质用乙腈洗涤数次,再用去离子水洗涤数次,最后真空干燥至恒重,得磷酸酯单体,其中,笼状磷酸酯、乙腈、无水三氯化铝、三乙胺、烯丙基二甲基氯硅烷的用量比为0.21-0.25mol:100-200mL:3-5g:0.35-0.55mol:0.1mol。
在上述反应中,利用笼状磷酸酯的羟基和烯丙基二甲基氯硅烷的氯反应,得磷酸酯单体,且其分子结构式如下所示。
一种高阻燃透气防护面料,通过以下步骤制成:
第一步、将改性苎麻纤维和涤纶纤维纺织成基布;
第二步、将基布进行漂白染色后,除皱,烘干,得处理后基布;
第三步、将阻燃层作为表层,其中,以阻燃层的单侧氧化改性的面作为粘结面,处理后的基布作为底层,用热压将阻燃层与基布粘合在一起,获得一种高阻燃透气防护面料。
本发明的有益效果:
本发明选用透气性能好的改性苎麻纤维为主要纤维,保证了基布的透气散热性能,通过涤纶纤维的加入,提高基布的保形性,且对苎麻纤维进行改性,提高了其弹性、抱合性和可纺性;其次,选择对基布的外层进行单侧改性,在基布外层接枝一层阻燃层,避免基布内层涂覆物质,造成面料透气性能的降低;再次,所述阻燃层进行了单侧改性,对阻燃层与基布的接触面进行了单侧氧化改性,使得该接触面具有更多的活性基团(阻燃层中的羟基被氧化成羰基或羧基),这些活性基团在阻燃层和基布的热压过程中可与基布上的基团(羟基)反应,使它们之间的粘结性更强;最后,阻燃层中含有阻燃剂,该阻燃剂为线性聚合物,相对分子量较大,迁移性小,阻燃性能优异且耐久,且含有含氟支链,因含氟支链的低表面能性能,赋予阻燃层耐水、耐化学试剂的性质,进而提高面料的防污性能,且在含氟支链迁移的作用下,阻燃剂中的笼状磷酸酯结构更易向复合材料的表面富集,形成一层致密的保护炭层,防止滴落或穿洞,进一步提高阻燃层的阻燃性能。
综上所述,本发明提供的面料具有高阻燃性能、良好的透气性能,以及耐污性能。
具体实施方式
下面将结合本发明实施例,对本发明实施例中的技术方案进行清楚、完整地描述,显然,所描述的实施例仅仅是本发明一部分实施例,而不是全部的实施例。基于本发明中的实施例,本领域普通技术人员在没有作出创造性劳动前提下所获得的所有其它实施例,都属于本发明保护的范围。
实施例1
磷酸酯单体通过以下步骤制成:
D1、将0.11mol季戊四醇、0.1mol三氯氧磷和40mL1,4-二氧六环加入带有机械搅拌、温度计、冷凝回流、干燥和氯化氢气体吸收装置的三口烧瓶中,升温至85℃,搅拌至无氯化氢气体产生,停止反应,冷却至室温,抽滤,沉淀用1,4-二氧六环和乙醇各洗涤两次,然后真空干燥至恒重,得笼状磷酸酯;
D2、将0.21mol笼状磷酸酯、100mL乙腈、3g无水三氯化铝和0.35mol三乙胺加入带有机械搅拌、冷凝回流、温度控制、氮气保护和恒压滴液漏斗的三口烧瓶中,加入0.1mol烯丙基二甲基氯硅烷,在70℃下搅拌1.5h,再升温回流反应12h,停止反应,静置冷却至室温,抽滤,固体物质用乙腈洗涤数次,再用去离子水洗涤3次,最后真空干燥至恒重,得磷酸酯单体。
实施例2
磷酸酯单体通过以下步骤制成:
D1、将0.13mol季戊四醇、0.1mol三氯氧磷和、60mL 1,4-二氧六环加入带有机械搅拌、温度计、冷凝回流、干燥和氯化氢气体吸收装置的三口烧瓶中,升温至85℃,搅拌至无氯化氢气体产生,停止反应,冷却至室温,抽滤,沉淀用1,4-二氧六环和乙醇各洗涤两次,然后真空干燥至恒重,得笼状磷酸酯;
D2、将0.25mol笼状磷酸酯、200mL乙腈、5g无水三氯化铝和0.55mol三乙胺加入带有机械搅拌、冷凝回流、温度控制、氮气保护和恒压滴液漏斗的三口烧瓶中,加入0.1mol烯丙基二甲基氯硅烷,在70℃下搅拌1.5h,再升温回流反应12h,停止反应,静置冷却至室温,抽滤,固体物质用乙腈洗涤数次,再用去离子水洗涤2次,最后真空干燥至恒重,得磷酸酯单体。
实施例3
阻燃聚酯树脂粒通过以下步骤制成:
C1、将0.1mol甲基丙烯酸六氟丁酯、0.1mol实施例1制备的磷酸酯单体、0.1mol 1,1,3,3-四甲基硅烷和无水甲苯混合后,搅拌均匀,然后在氮气保护下,加热至96℃,然后加入1.35g氯铂酸异丙醇溶液,反应5h,反应结束后用活性炭吸附铂催化剂,过滤,旋蒸除去溶剂,得阻燃剂;
C2、将100g聚酯颗粒、15g阻燃剂和1.5g相容剂加入挤出机中,挤出造粒,得阻燃聚酯树脂粒,其中,挤出机的转速为200rpm,挤出温度为160℃,相容剂为马来酸酐接枝聚乙烯,聚酯颗粒为PET颗粒。
实施例4
阻燃聚酯树脂粒通过以下步骤制成:
C1、将0.1mol甲基丙烯酸六氟丁酯、0.1mol实施例2制备的磷酸酯单体、0.1mol 1,1,3,3-四甲基硅烷和无水甲苯混合后,搅拌均匀,然后在氮气保护下,加热至96℃,然后加入2.7g氯铂酸异丙醇溶液,反应5h,反应结束后用活性炭吸附铂催化剂,过滤,旋蒸除去溶剂,得阻燃剂;
C2、将100g聚酯颗粒、30g阻燃剂和4.5g相容剂加入挤出机中,挤出造粒,得阻燃聚酯树脂粒,其中,挤出机的转速为400rpm,挤出温度为200℃,相容剂为马来酸酐接枝聚丙烯,聚酯颗粒为PET颗粒。
实施例5
阻燃层通过以下步骤制成:
B1、将15g实施例3制备的阻燃聚酯树脂粒和82g有机溶剂加入三口瓶中,在室温下持续搅拌至完全溶解,得阻燃聚酯溶液;将阻燃聚酯溶液经静电纺丝,待溶液纺丝完全后得阻燃聚酯膜,其中,有机溶剂为丙酮和N,N-二甲基甲酰胺按照体积比为70:30进行混合的混合溶剂,纺丝电压18kV,纺丝速率为0.6mL/h,纺丝接收距离为18cm,纺丝温度为28℃,纺丝湿度为35%;
B2、将阻燃聚酯膜的一侧用聚乙烯基胶带粘贴密封,对粘贴侧膜表面实施保护,并将单侧保护后的阻燃聚酯膜的未保护侧放入氧化剂溶液中,在95℃下对未保护侧进行7h氧化处理,得单侧氧化改性的阻燃层,其中氧化剂溶液为高锰酸钾粉末和质量分数68%的硝酸按照质量比1:1进行混合制成。
实施例6
阻燃层通过以下步骤制成:
B1、将18g实施例4制备的阻燃聚酯树脂粒和85g有机溶剂加入三口瓶中,在室温下持续搅拌至完全溶解,得阻燃聚酯溶液;将阻燃聚酯溶液经静电纺丝,待溶液纺丝完全后得阻燃聚酯膜,其中,有机溶剂为丙酮和N,N-二甲基甲酰胺按照体积比为85:15进行混合的混合溶剂,纺丝电压18kV,纺丝速率为0.6mL/h,纺丝接收距离为18cm,纺丝温度为28℃,纺丝湿度为35%;
B2、将阻燃聚酯膜的一侧用聚乙烯基胶带粘贴密封,对粘贴侧膜表面实施保护,并将单侧保护后的阻燃聚酯膜的未保护侧放入氧化剂溶液中,在95℃下对未保护侧进行7h氧化处理,得单侧氧化改性的阻燃层,其中氧化剂溶液为高锰酸钾粉末和质量分数68%的硝酸按照质量比1:1进行混合制成。
实施例7
端氨基聚硅氧烷通过以下步骤制成:
在氮气气流的保护下,向四口烧瓶中,加入60g D4和0.6g催化剂苄基三甲基氢氧化胺甲醇溶液(0.5wt%),在磁力搅拌下,加热至50℃,加入6g封端剂,减压脱除体系中残余的水和甲醇,待体系粘度不变时,继续反应12h,继续升高温度至175℃破坏催化中心活性,后降温至150℃,负压脱除反应剩余的D4单体和低沸物小分子,得端氨基聚硅烷,其中,端氨基聚硅氧烷的分子量为1000。
实施例8
端氨基聚硅氧烷通过以下步骤制成:
在氮气气流的保护下,向四口烧瓶中,加入60g D4和0.6g催化剂苄基三甲基氢氧化胺甲醇溶液(0.5wt%),在磁力搅拌下,加热至50℃,加入9g封端剂,减压脱除体系中残余的水和甲醇,待体系粘度不变时,继续反应12h,继续升高温度至175℃破坏催化中心活性,后降温至150℃,负压脱除反应剩余的D4单体和低沸物小分子,得端氨基聚硅烷,其中,端氨基聚硅氧烷的分子量为1500。
实施例9
改性苎麻纤维通过以下步骤制成:
A1、将苎麻纤维置于质量分数18%氢氧化钠液中,室温下反应3h后,洗至中性,得碱处理苎麻纤维,其中,苎麻纤维和质量分数18%氢氧化钠液的质量比为1:30;
A2、将碱处理苎麻纤维置于混合溶液A中55℃下反应5h,依次水洗后经无水乙醇洗涤,再经水洗至中性,烘干,得醚化改性苎麻纤维,其中,碱处理苎麻纤维和混合溶液A的质量比为1:30;混合溶液A由环氧氯丙烷、质量分数5%的氢氧化钠溶液和无水乙醇按照3g:50g:3mL混合组成;
A3、将醚化改性苎麻纤维置于混合溶液B中50℃下反应5h,经水洗、无水乙醇洗,再水洗至中性,得改性苎麻纤维,其中,醚化改性苎麻纤维和混合溶液B的质量比为1:30,混合溶液B由实施例7制备的端氨基聚硅氧烷、碳酸氢钠和无水乙醇按照0.65mol:5g:100mL混合组成。
实施例10
改性苎麻纤维通过以下步骤制成:
A1、将苎麻纤维置于质量分数18%氢氧化钠液中,室温下反应3h后,洗至中性,得碱处理苎麻纤维,其中,苎麻纤维和质量分数18%氢氧化钠液的质量比为1:40;
A2、将碱处理苎麻纤维置于混合溶液A中55℃下反应5h,依次水洗后经无水乙醇洗涤,再经水洗至中性,烘干,得醚化改性苎麻纤维,其中,碱处理苎麻纤维和混合溶液A的质量比为1:40;混合溶液A由环氧氯丙烷、质量分数5%的氢氧化钠溶液和无水乙醇按照4g:50g:5mL混合组成;
A3、将醚化改性苎麻纤维置于混合溶液B中50℃下反应5h,经水洗、无水乙醇洗,再水洗至中性,得改性苎麻纤维,其中,醚化改性苎麻纤维和混合溶液B的质量比为1:40,混合溶液B由实施例8制备的端氨基聚硅氧烷、碳酸氢钠和无水乙醇按照0.85mol:7g:120mL混合组成。
实施例11
一种高阻燃透气防护面料,通过以下步骤制成:
第一步、将实施例9制备的改性苎麻纤维和涤纶纤维纺织成基布,其中,改性苎麻纤维的含量为75%,涤纶纤维丝含量为25%;
第二步、将基布进行漂白染色后,除皱,烘干,得处理后基布;
第三步、将实施例5制备的阻燃层作为表层,其中,以阻燃层的单侧氧化改性的面作为粘结面,处理后的基布作为底层,用热压将阻燃层与基布粘合在一起,获得一种高阻燃透气防护面料。
实施例12
一种高阻燃透气防护面料,通过以下步骤制成:
第一步、将实施例10制备的改性苎麻纤维和涤纶纤维纺织成基布,其中,改性苎麻纤维的含量为80%,涤纶纤维丝含量为20%;
第二步、将基布进行漂白染色后,除皱,烘干,得处理后基布;
第三步、将实施例6制备的阻燃层作为表层,其中,以阻燃层的单侧氧化改性的面作为粘结面,处理后的基布作为底层,用热压将阻燃层与基布粘合在一起,获得一种高阻燃透气防护面料。
实施例13
一种高阻燃透气防护面料,通过以下步骤制成:
第一步、将实施例10制备的改性苎麻纤维和涤纶纤维纺织成基布,其中,改性苎麻纤维的含量为85%,涤纶纤维丝含量为15%;
第二步、将基布进行漂白染色后,除皱,烘干,得处理后基布;
第三步、将实施例5制备的阻燃层作为表层,其中,以阻燃层的单侧氧化改性的面作为粘结面,处理后的基布作为底层,用热压将阻燃层与基布粘合在一起,获得一种高阻燃透气防护面料。
对比例1
阻燃聚酯树脂粒的制备:
C1、将0.1mol甲基丙烯酸六氟丁酯、0.1mol 1,1,3,3-四甲基硅烷和无水甲苯混合后,搅拌均匀,然后在氮气保护下,加热至96℃,然后加入1g氯铂酸异丙醇溶液,反应5h,反应结束后用活性炭吸附铂催化剂,过滤,旋蒸除去溶剂,得阻燃剂;
C2、将100g聚酯颗粒、15g阻燃剂和1.5g相容剂加入挤出机中,挤出造粒,得阻燃聚酯树脂粒,其中,挤出机的转速为200rpm,挤出温度为160℃,相容剂为马来酸酐接枝聚乙烯,聚酯颗粒为PET颗粒。
阻燃层的制备:与相比实施例5,将阻燃树脂粒替换成上述制备的阻燃聚酯树脂粒,其余相同。
对比例2
阻燃聚酯树脂粒的制备:
C1、将0.1mol甲基丙烯酸六氟丁酯、0.1mol实施例2制备的磷酸酯单体和无水甲苯混合后,搅拌均匀,然后在氮气保护下,加热至96℃,然后加入2g氯铂酸异丙醇溶液,反应5h,反应结束后用活性炭吸附铂催化剂,过滤,旋蒸除去溶剂,得阻燃剂;
C2、将100g聚酯颗粒、30g阻燃剂和4.5g相容剂加入挤出机中,挤出造粒,得阻燃聚酯树脂粒,其中,挤出机的转速为400rpm,挤出温度为200℃,相容剂为马来酸酐接枝聚丙烯,聚酯颗粒为PET颗粒。
阻燃层的制备:与相比实施例6,将阻燃树脂粒替换成上述制备的阻燃聚酯树脂粒,其余相同。
对比例3
阻燃聚酯树脂粒通过以下步骤制成:
C1、将0.1mol甲基丙烯酸六氟丁酯、0.1mol实施例2制备的磷酸酯单体和无水甲苯混合后,搅拌均匀,然后在氮气保护下,加热至96℃,然后加入1.9g氯铂酸异丙醇溶液,反应5h,反应结束后用活性炭吸附铂催化剂,过滤,旋蒸除去溶剂,得阻燃剂;
C2、将100g聚酯颗粒、30g阻燃剂和4.5g相容剂加入挤出机中,挤出造粒,得阻燃聚酯树脂粒,其中,挤出机的转速为400rpm,挤出温度为200℃,相容剂为马来酸酐接枝聚丙烯,聚酯颗粒为PET颗粒。
阻燃层的制备:与相比实施例5,将阻燃树脂粒替换成上述制备的阻燃聚酯树脂粒,其余相同。
对比例4
阻燃层通过以下步骤制成:
将15g实施例3制备的阻燃聚酯树脂粒和82g有机溶剂加入三口瓶中,在室温下持续搅拌至完全溶解,得阻燃聚酯溶液;将阻燃聚酯溶液经静电纺丝,待溶液纺丝完全后得阻燃层,其中,有机溶剂为丙酮和N,N-二甲基甲酰胺按照体积比为70:30进行混合的混合溶剂,纺丝电压18kV,纺丝速率为0.6mL/h,纺丝接收距离为18cm,纺丝温度为28℃,纺丝湿度为35%;
对比例5
一种高阻燃透气防护面料,通过以下步骤制成:
与实施例11相比,将步骤三中的阻燃层替换成对比例1制备的阻燃层。
对比例6
一种高阻燃透气防护面料,通过以下步骤制成:
与实施例12相比,将步骤三中的阻燃层替换成对比例2制备的阻燃层。
对比例7
一种高阻燃透气防护面料,通过以下步骤制成:
与实施例12相比,将步骤三中的阻燃层替换成对比例3制备的阻燃层。
对比例8
一种高阻燃透气防护面料,通过以下步骤制成:
与实施例13相比,将步骤三中的阻燃层替换成对比例4制备的阻燃层。
对比例9
一种面料,通过以下步骤制成:
第一步、将实施例10制备的改性苎麻纤维和涤纶纤维纺织成基布,其中,改性苎麻纤维的含量为75%,涤纶纤维丝含量为25%;
第二步、将基布进行漂白染色后,除皱,烘干,得处理后基布;
第三步、将处理后的基布双侧通过热压粘合两层实施例5制备的阻燃层,以阻燃层的单侧氧化改性的面作为粘结面,获得一种面料。
对比例10
实施例13中的基布。
实施例14
将实施例11-13和对比例5-10获得的面料进行以下性能测试:
接触角:采用将待测样品粘贴在载玻片上,每个样品各取5个不同位置,将去离子水滴于样品表面5s后保存图片,计算其度数;
透气性能:透气性能采用裁剪所需样品,设定测试压力为0.1MPa,测定每分钟内氮气透过面积样品面料的体积;
阻燃性能:将实施例或对比例提供的面料分别取出2cm×2cm的小样作为测试样品,标记为样品1-8,用镊子夹持测试样品,垂直放入透明燃烧筒中,筒内有向上的移动氧氮气流,点燃试样上端,随即观察燃烧现象,并与规定的极限比较其持续燃烧时间或燃烧的距离。通过不同氧浓度中一系列试样的实验,可以测得最低氧浓度,即极限氧指数,极限氧指数越高,表示材料的阻燃性能越好;
阻燃层的剥离强度:用BLD-200H剥离强度测试仪测试层间剥离强度;
上述测试数据如表1所示。
表1
从表1中的数据可以看出,实施例11-13获得的面料的接触角、阻燃性能均优于对比例10中的基布,且透气性能与对比例10相似,具有良好的透气性,实施例11-13获得面料的阻燃性要优于对比例5-7获得的面料的对应性能,实施例11-13获得面料的阻然层的剥离强度优于对比例8获得面料的对应性能,实施例11-13获得面料的接触角优于对比例8获得面料的对应性能。
在说明书的描述中,参考术语“一个实施例”、“示例”、“具体示例”等的描述意指结合该实施例或示例描述的具体特征、结构、材料或者特点包含于本发明的至少一个实施例或示例中。在本说明书中,对上述术语的示意性表述不一定指的是相同的实施例或示例。而且,描述的具体特征、结构、材料或者特点可以在任何的一个或多个实施例或示例中以合适的方式结合。
以上内容仅仅是对本发明所作的举例和说明,所属本技术领域的技术人员对所描述的具体实施例做各种各样的修改或补充或采用类似的方式替代,只要不偏离发明或者超越本权利要求书所定义的范围,均应属于本发明的保护范围。
Claims (8)
1.一种高阻燃透气防护面料,其特征在于:包括基布和基布表面粘合的阻燃层,所述基布以改性苎麻纤维和涤纶纤维纺织而成;
所述阻燃层包括以下步骤制成:
将阻燃聚酯膜的一侧用聚乙烯基胶带粘贴密封,并将单侧保护后的阻燃聚酯膜的未保护侧放入氧化剂溶液中,在95℃下对未保护侧进行7h氧化处理,得单侧氧化改性的阻燃层。
2.根据权利要求1所述的一种高阻燃透气防护面料,其特征在于:基布中改性苎麻纤维的含量为75-85%,涤纶纤维丝含量为15-25%。
3.根据权利要求1所述的一种高阻燃透气防护面料,其特征在于:所述改性苎麻纤维包括以下步骤制成:
A1、将苎麻纤维置于质量分数18%氢氧化钠液中,室温下反应3h后,洗至中性,得碱处理苎麻纤维;
A2、将碱处理苎麻纤维置于混合溶液A中55℃下反应5h,依次水洗后经无水乙醇洗涤,再经水洗至中性,烘干,得醚化改性苎麻纤维,其中,混合溶液A由环氧氯丙烷、质量分数5%的氢氧化钠溶液和无水乙醇按照3-4g:50g:3-5mL混合组成;
A3、将醚化改性苎麻纤维置于混合溶液B中50℃下反应5h,经水洗、无水乙醇洗,再水洗至中性,得改性苎麻纤维,其中,混合溶液B由端氨基聚硅氧烷、碳酸氢钠和无水乙醇按照0.65-0.85mol:5-7g:100-120mL混合组成。
4.根据权利要求1所述的一种高阻燃透气防护面料,其特征在于:所述阻燃聚酯膜包括以下步骤制成:
将阻燃聚酯树脂粒和有机溶剂混合均匀后,得阻燃聚酯溶液;将阻燃聚酯溶液经静电纺丝,待溶液纺丝完全后得阻燃聚酯膜。
5.根据权利要求4所述的一种高阻燃透气防护面料,其特征在于:所述阻燃聚酯树脂粒包括以下步骤制成:
C1、将甲基丙烯酸六氟丁酯、磷酸酯单体、1,1,3,3-四甲基硅烷和无水甲苯混合后,搅拌均匀,然后在氮气保护下,加热至96℃,然后加入氯铂酸异丙醇溶液,反应5h,经后处理,得阻燃剂;
C2、将聚酯颗粒、阻燃剂和相容剂加入挤出机中挤出造粒,得阻燃聚酯树脂粒。
6.根据权利要求5所述的一种高阻燃透气防护面料,其特征在于:所述磷酸酯单体包括以下步骤制成:
将笼状磷酸酯、乙腈、无水三氯化铝和三乙胺混合后,加入烯丙基二甲基氯硅烷,在70℃下搅拌1.5h,再升温回流反应12h,停止反应,经后处理,得磷酸酯单体。
7.根据权利要求6所述的一种高阻燃透气防护面料,其特征在于:所述笼状磷酸酯、乙腈、无水三氯化铝、三乙胺、烯丙基二甲基氯硅烷的用量比为0.21-0.25mol:100-200mL:3-5g:0.35-0.55mol:0.1mol。
8.根据权利要求1所述的一种高阻燃透气防护面料的制备方法,其特征在于:包括以下步骤:
第一步、将改性苎麻纤维和涤纶纤维纺织成基布;
第二步、将基布进行漂白染色后,除皱,烘干,得处理后基布;
第三步、将阻燃层作为表层,其中,以阻燃层的单侧氧化改性的面作为粘结面,处理后的基布作为底层,用热压将阻燃层与基布粘合在一起,获得一种高阻燃透气防护面料。
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