CN111516332B - 一种高牢度弹力牛仔贴合面料及其制备方法 - Google Patents
一种高牢度弹力牛仔贴合面料及其制备方法 Download PDFInfo
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- CN111516332B CN111516332B CN202010446917.XA CN202010446917A CN111516332B CN 111516332 B CN111516332 B CN 111516332B CN 202010446917 A CN202010446917 A CN 202010446917A CN 111516332 B CN111516332 B CN 111516332B
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Classifications
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- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- 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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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
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- D06M11/45—Oxides or hydroxides of elements of Groups 3 or 13 of the Periodic Table; Aluminates
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- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
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- D06M11/51—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
- D06M11/52—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 selenium, tellurium, polonium or their compounds; with sulfur, dithionites or compounds containing sulfur and halogens, with or without oxygen; by sulfohalogenation with chlorosulfonic acid; by sulfohalogenation with a mixture of sulfur dioxide and free halogens
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- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
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Abstract
本发明公开了一种高牢度弹力牛仔贴合面料及其制备方法,所述贴合面料包括预处理底布、面布和TPE膜,所述面布通过热熔胶贴合在预处理底布上,所述TPE膜通过热熔胶贴合在面布上;所述预处理底布由底布、表面改性剂改性制得;所述表面改性剂各组分原料包括:以重量计,阻燃剂5‑7份、吸水微球10‑12份、六水合氯化铝8‑10份、无水乙醇25‑30份、甲酰胺4‑6份、正硅酸四乙酯4‑6份、1,2‑环氧丙烷10‑14份。本发明公开了一种高牢度弹力牛仔贴合面料及其制备方法,工艺设计合理,操作简单,制备得到具有优异阻燃性能的三层贴合面料,该贴合面料挺括性好,可广泛应用于服装领域,实用性较高。
Description
技术领域
本发明涉及面料制备技术领域,具体是一种高牢度弹力牛仔贴合面料及其制备方法。
背景技术
牛仔面料(Denim),又叫牛仔布,这是一种较粗厚的色织经面斜纹棉布,经纱颜色深,一般为靛蓝色,纬纱颜色浅,一般为浅灰或煮练后的本白纱。牛仔布始于美国西部,放牧人员用以制作衣裤而得名,缩质地紧密,厚实,色泽鲜艳,织纹清晰;适用于男女式牛仔裤,牛仔上装,牛仔背心,牛仔裙等。
现如今,牛仔面料因其实用耐穿的特点广泛应用于我们的生活中,但现有的牛仔面料的功能比较单一,单层面料的质感、手感都比较差,其阻燃性能也无法满足我们的需求。
针对该问题,我们设计了一种高牢度弹力牛仔贴合面料及其制备方法,这是我们亟待解决的技术问题之一。
发明内容
本发明的目的在于提供一种高牢度弹力牛仔贴合面料及其制备方法,以解决现有技术中的问题。
为实现上述目的,本发明提供如下技术方案:
一种高牢度弹力牛仔贴合面料,所述贴合面料包括预处理底布、面布和TPE膜,所述面布通过热熔胶贴合在预处理底布上,所述TPE膜通过热熔胶贴合在面布上;所述预处理底布由底布、表面改性剂改性制得;
所述表面改性剂各组分原料包括:以重量计,阻燃剂5-7份、吸水微球10-12份、六水合氯化铝8-10份、无水乙醇25-30份、甲酰胺4-6份、正硅酸四乙酯4-6份、1,2-环氧丙烷10-14份。
较优化的方案,所述吸水微球由改性微球、改性吸水料、无水乙醇制备得到;所述阻燃剂由磷酸、冰乙酸、无水哌嗪制备得到。
较优化的方案,所述改性吸水料由吸水料、3-氨丙基三甲氧基硅氧烷、无水乙醇制得,所述吸水料各组分原料包括:以重量计,丁腈橡胶90-100份、改性橡胶30-40份、硅橡胶20-30份、氧化石墨烯6-8份、氧化锌4-5份、硬脂酸1-2份、防老剂2-3份、促进剂3-4份、炭黑8-10份、聚丙烯酸钠30-35份、硫磺2-3份。
较优化的方案,所述改性橡胶由叔丁基过氧化氢、三氧化钼、丁腈橡胶制备得到;所述硅橡胶由乙烯基硅油、白炭黑、氢氧化铝、铂金催化剂、含氢硅油制备得到。
较优化的方案,所述改性微球由邻苯二酚、己二胺、二氧化硅微球制备得到。
较优化的方案,所述面布为95%-98%棉和2%-5%氨纶牛仔混合而成;所述底布为尼龙网眼布。
较优化的方案,所述二氧化硅微球的粒径为0.08-0.1mm。
较优化的方案,一种高牢度弹力牛仔贴合面料的制备方法,包括以下步骤:
1)准备物料;
2)改性吸水料的制备:
a)取叔丁基过氧化氢和三氧化钼,混合搅拌,加热升温至70-75℃,搅拌反应,反应后加入丁腈橡胶,60-80℃下搅拌反应,洗涤,真空干燥,得到改性橡胶;
b)取乙烯基硅油、白炭黑和氢氧化铝,混合搅拌,真空条件下继续加热至200-210℃,搅拌,再加入铂金催化剂和含氢硅油,继续搅拌,140-145℃下模压成型,得到硅橡胶;
c)取丁腈橡胶、改性橡胶,塑炼,加入硅橡胶和氧化石墨烯,混炼,再依次加入氧化锌、硬脂酸、防老剂、促进剂、炭黑、聚丙烯酸钠和硫磺,混炼,薄通,置于平板硫化机上硫化,得到吸水料;
d)取吸水料,无水乙醇溶解,超声分散,加入3-氨丙基三甲氧基硅氧烷,反应,冷却至室温,醇洗,水洗,冷冻干燥,研磨粉碎,过200目筛,得到改性吸水料;
3)吸水微球的制备:
a)取邻苯二酚、己二胺,去离子水溶解,搅拌,加入二氧化硅微球,继续搅拌,室温下反应,离心分离,洗涤后置于刻蚀液中,搅拌,离心分离,洗涤,真空干燥,得到改性微球;
b)取改性吸水料,盐酸溶解,搅拌,过滤,洗涤,得到物料A;取改性微球,氢氧化钠溶液溶解,搅拌,过滤,洗涤,得到物料B;取物料B,无水乙醇溶解,再加入物料A,搅拌,过滤,洗涤,真空干燥,得到吸水微球;
4)表面改性剂的制备:
a)取磷酸,加热升温至200-220℃,反应,加入冰乙酸和无水哌嗪,调温至110-115℃,继续反应,抽滤,真空干燥,得到阻燃剂;
b)取六水合氯化铝、无水乙醇、去离子水和甲酰胺,搅拌,加入正硅酸四乙酯,搅拌,再加入阻燃剂和吸水微球,继续搅拌,接着添加1,2-环氧丙烷,搅拌,得到表面改性剂;
5)取底布,清洗,干燥后置于氢氧化钠溶液中浸泡,去离子水洗涤,烘干,再置于表面改性剂中浸泡,取出底布,室温下静置,老化干燥,得到预处理底布;
6)取面布,表面通过热熔胶贴合TPE膜,橡胶压辊压紧,蒸发固化,得到预处理面布;再取预处理底布,将预处理面布贴合至预处理底布表面,橡胶压辊压紧贴合,蒸发固化,再置于100-120℃下烘干,升温至140-160℃,烘焙,得到贴合面料。
较优化的方案,包括以下步骤:
1)准备物料;
2)改性吸水料的制备:
a)取叔丁基过氧化氢和三氧化钼,混合搅拌10-20min,加热升温至70-75℃,搅拌反应2-2.5h,反应后加入丁腈橡胶,60-80℃下搅拌反应30-80min,无水乙醇洗涤,40℃下真空干燥,得到改性橡胶;
b)取乙烯基硅油、白炭黑和氢氧化铝,混合搅拌3-3.5h,真空条件下继续加热至200-210℃,搅拌2-2.2h,再加入铂金催化剂和含氢硅油,继续搅拌20-30min,140-145℃下模压成型,模压时间为15-20min,得到硅橡胶;
c)取丁腈橡胶、改性橡胶,塑炼5-7min,加入硅橡胶和氧化石墨烯,混炼5-7min,再依次加入氧化锌、硬脂酸、防老剂、促进剂、炭黑、聚丙烯酸钠和硫磺,混炼15-25min,薄通,置于平板硫化机上硫化,160-165℃温度下硫化2-3min,得到吸水料;
d)取吸水料,无水乙醇溶解,超声分散30-40min,加入3-氨丙基三甲氧基硅氧烷,反应6-6.2h,冷却至室温,醇洗2-3次,水洗2-3次,冷冻干燥,研磨粉碎,过200目筛,得到改性吸水料;
3)吸水微球的制备:
a)取邻苯二酚、己二胺,去离子水溶解,搅拌20-30min,加入二氧化硅微球,继续搅拌10-20min,室温下反应36-38h,离心分离,洗涤后置于刻蚀液中,搅拌25-35min,离心分离,洗涤,40℃下真空干燥24h,得到改性微球;
b)取改性吸水料,盐酸溶解,搅拌5-10min,过滤,洗涤,得到物料A;取改性微球,氢氧化钠溶液溶解,搅拌5-10min,过滤,洗涤,得到物料B;取物料B,无水乙醇溶解,再加入物料A,搅拌10-20min,过滤,洗涤,40℃下真空干燥,得到吸水微球;
4)表面改性剂的制备:
a)取磷酸,加热升温至200-220℃,反应25-35min,加入冰乙酸和无水哌嗪,调温至110-115℃,反应3-3.2h,抽滤,真空干燥,得到阻燃剂;
b)取六水合氯化铝、无水乙醇、去离子水和甲酰胺,搅拌15-18min,加入正硅酸四乙酯,搅拌24-26h,再加入阻燃剂和吸水微球,继续搅拌10-15min,接着添加1,2-环氧丙烷,搅拌4-5min,得到表面改性剂;
5)取底布,无水***清洗5-6h,去离子水清洗,干燥后置于氢氧化钠溶液中,浸泡0.8-1h,去离子水洗涤,烘干,再置于表面改性剂中浸泡3-5min,取出底布,室温下静置20-24h,老化干燥,得到预处理底布;
6)取面布,表面通过热熔胶贴合TPE膜,橡胶压辊压紧,蒸发固化40-45h,得到预处理面布;再取预处理底布,将预处理面布贴合至预处理底布表面,橡胶压辊压紧贴合,蒸发固化40-45h,再置于100-120℃下烘干30-40s,升温至140-160℃,烘焙2-3min,得到贴合面料。
较优化的方案,步骤3)的a)步骤中,所述刻蚀液包括氢氟酸和氟化铵,所述氢氟酸和氟化铵的体积比为1:1。
与现有技术相比,本发明的有益效果是:
本发明在制备时,步骤2)先进行改性吸水料的制备,制备时以叔丁基过氧化氢为氧化剂,以三氧化钼为催化剂对丁腈橡胶进行环氧化反应,制备得到改性橡胶(环氧化丁腈橡胶),接着再利用铂金催化剂、氢氧化铝和乙烯基硅油等组分,制备得到具有优异阻燃效果的硅橡胶,在该制备过程中氢氧化铝作为阻燃剂以提高硅橡胶的阻燃性能,该硅橡胶的添加有助于提高吸水料的阻燃性能;接着本发明再以丁腈橡胶、改性橡胶、硅橡胶为主要胶料,添加氧化石墨烯、炭黑等组分,制备得到吸水膨胀橡胶料(即吸水料),由于硅橡胶和吸水树脂(聚丙烯酸钠)的存在,该吸水料具有优异的阻燃性能和吸水性能,且制备过程中对丁腈橡胶进行了环氧化改性,可提高吸水树脂和丁腈橡胶之间的相容性,进一步提高吸水料的力学性能。
本发明制备得到吸水料之后,又利用无水乙醇、3-氨丙基三甲氧基硅氧烷对其进行氨基化处理,3-氨丙基三甲氧基硅氧烷可与氧化石墨烯表面的环氧键发生亲核反应并接枝有氨基,得到改性吸水料,该改性吸水料可在酸性环境下发生氨基质子化反应,生成带有正电荷的改性吸水料。
接着本发明步骤3)进行吸水微球的制备,在制备过程中选用粒径为0.08-0.1mm大小的二氧化硅微球,以该二氧化硅微球为模板,通过邻苯二酚和己二胺反应聚合并包覆在二氧化硅微球表面,形成聚酚胺核壳结构,再将该聚酚胺核壳结构置于刻蚀液中刻蚀,去除胶囊内部的二氧化硅微球,离心分离后得到改性微球,该改性微球中含有大量的氨基和酚羟基,在酸性环境下发生氨基质子化,使得改性微球带有正电荷,在碱性环境下,酚羟基发生去质子作用,可使改性微球带有负电荷。
基于该性质,本发明制备得到改性微球后,将改性微球置于氢氧化钠溶液中,使其因为酚羟基的去质子作用而带有负电荷,再将改性吸水料置于盐酸溶液中,使其带有正电荷,并在静电作用下将改性吸水料吸附至改性微球中,得到具有优异吸水效果的吸水微球;在制备过程中,本申请将改性吸水料研磨过200目筛,使其粒径小于0.07mm,而改性微球内部空腔大小为0.08-0.1mm,使得改性吸水料可有效吸附至改性微球中,保证吸水微球的顺利制备。
本发明步骤4)进行表面改性剂的制备,以磷酸和无水哌嗪为原料,磷酸在高温环境下脱水并生成焦磷酸,焦磷酸与无水哌嗪反应制备焦磷酸哌嗪(阻燃剂);阻燃剂制备后,本申请再采用溶胶-凝胶法,以六水合氯化铝为铝源,以正硅酸四乙酯为硅源,1,2-环氧丙烷作为凝胶网络诱导剂,生成二氧化硅凝胶,在制备过程中,由于底布选为尼龙22D网眼布,其表面含有大量的酰胺键,在经过氢氧化钠处理后,底布表面的酰胺键被破坏,并带有负电荷,而二氧化硅凝胶体系中的胶粒带有正电荷,不仅可以将吸收微球吸附在凝胶体系中,还能够通过静电作用将带正电荷的胶粒牢固的吸附在底布表面,在1,2-环氧丙烷的作用下进一步缩聚,使得底布表面形成均匀包覆的凝胶膜层,老化干燥步骤处理后,底布表面形成气凝胶层,得到预处理底布,该气凝胶层中吸附有吸收微球和阻燃剂。
本发明制备得到预处理底布后,再进行面布、TPE膜的热熔贴合,得到贴合面料;燃烧时随着温度的升高,预处理底布中的焦磷酸哌嗪开始分解,产生大量不燃性气体,可稀释氧气的浓度,抑制氧气传输和热量传递;分解时还生成磷酸、偏磷酸或多聚磷酸等酸性物质,该酸洗物质具有优异脱水效果,可以脱水促进成炭,同时还使整个预处理底布处于酸性环境下,在该环境下,改性微球氨基质子化从而带正电荷,在静电作用下改性吸水料脱离改性微球,改性吸水料吸水膨胀,不仅可以提高体系脱水成炭效率,而且吸水膨胀后的粒子可对炭层进行填充,有效提高炭层的致密性,隔热隔氧;同时在该过程中,预处理底布表面的氢氧化铝可吸热分解生成氧化铝,增加预处理底布自身的热损耗和传热阻力,隔热阻燃性能得到进一步提高。
本发明公开了一种高牢度弹力牛仔贴合面料及其制备方法,工艺设计合理,操作简单,制备得到具有优异阻燃性能的三层贴合面料,该贴合面料挺括性好,可广泛应用于服装领域,实用性较高。
具体实施方式
下面将对本发明实例中的技术方案进行清楚、完整地描述,显然,所描述的实例仅仅是本发明一部分实例,而不是全部的实例。基于本发明中的实例,本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实例,都属于本发明保护的范围。
实例1:
S1:准备物料;
S2:改性吸水料的制备:
取叔丁基过氧化氢和三氧化钼,混合搅拌10min,加热升温至70℃,搅拌反应2h,反应后加入丁腈橡胶,60℃下搅拌反应30min,无水乙醇洗涤,40℃下真空干燥,得到改性橡胶;
取乙烯基硅油、白炭黑和氢氧化铝,混合搅拌3h,真空条件下继续加热至200℃,搅拌2h,再加入铂金催化剂和含氢硅油,继续搅拌20min,140℃下模压成型,模压时间为15min,得到硅橡胶;
取丁腈橡胶、改性橡胶,塑炼5min,加入硅橡胶和氧化石墨烯,混炼5min,再依次加入氧化锌、硬脂酸、防老剂、促进剂、炭黑、聚丙烯酸钠和硫磺,混炼15min,薄通,置于平板硫化机上硫化,160℃温度下硫化2min,得到吸水料;
取吸水料,无水乙醇溶解,超声分散30min,加入3-氨丙基三甲氧基硅氧烷,反应6h,冷却至室温,醇洗2次,水洗2次,冷冻干燥,研磨粉碎,过200目筛,得到改性吸水料;
S3:吸水微球的制备:
取邻苯二酚、己二胺,去离子水溶解,搅拌20min,加入二氧化硅微球,继续搅拌10min,室温下反应36h,离心分离,洗涤后置于刻蚀液中,搅拌25min,离心分离,洗涤,40℃下真空干燥24h,得到改性微球;其中刻蚀液包括氢氟酸和氟化铵,所述氢氟酸和氟化铵的体积比为1:1;
取改性吸水料,盐酸溶解,搅拌5min,过滤,洗涤,得到物料A;取改性微球,氢氧化钠溶液溶解,搅拌5min,过滤,洗涤,得到物料B;取物料B,无水乙醇溶解,再加入物料A,搅拌10min,过滤,洗涤,40℃下真空干燥,得到吸水微球;
S4:表面改性剂的制备:
取磷酸,加热升温至200℃,反应25min,加入冰乙酸和无水哌嗪,调温至110℃,反应3h,抽滤,真空干燥,得到阻燃剂;
取六水合氯化铝、无水乙醇、去离子水和甲酰胺,搅拌15min,加入正硅酸四乙酯,搅拌24h,再加入阻燃剂和吸水微球,继续搅拌10min,接着添加1,2-环氧丙烷,搅拌4min,得到表面改性剂;
S5:取底布,无水***清洗5h,去离子水清洗,干燥后置于氢氧化钠溶液中,浸泡0.8h,去离子水洗涤,烘干,再置于表面改性剂中浸泡3min,取出底布,室温下静置20h,老化干燥,得到预处理底布;
S6:取面布,表面通过热熔胶贴合TPE膜,橡胶压辊压紧,蒸发固化40h,得到预处理面布;再取预处理底布,将预处理面布贴合至预处理底布表面,橡胶压辊压紧贴合,蒸发固化40h,再置于100℃下烘干30s,升温至140℃,烘焙2min,得到贴合面料。
本实例中,表面改性剂各组分原料包括:以重量计,阻燃剂5份、吸水微球10份、六水合氯化铝8份、无水乙醇25份、甲酰胺4份、正硅酸四乙酯4份、1,2-环氧丙烷10份。
吸水料各组分原料包括:以重量计,丁腈橡胶90份、改性橡胶30份、硅橡胶20份、氧化石墨烯6份、氧化锌4份、硬脂酸1份、防老剂2份、促进剂3份、炭黑8份、聚丙烯酸钠30份、硫磺2份;二氧化硅微球的粒径为0.08mm。
实例2:
S1:准备物料;
S2:改性吸水料的制备:
取叔丁基过氧化氢和三氧化钼,混合搅拌15min,加热升温至72℃,搅拌反应2.3h,反应后加入丁腈橡胶,70℃下搅拌反应60min,无水乙醇洗涤,40℃下真空干燥,得到改性橡胶;
取乙烯基硅油、白炭黑和氢氧化铝,混合搅拌3.2h,真空条件下继续加热至205℃,搅拌2.1h,再加入铂金催化剂和含氢硅油,继续搅拌25min,143℃下模压成型,模压时间为18min,得到硅橡胶;
取丁腈橡胶、改性橡胶,塑炼6min,加入硅橡胶和氧化石墨烯,混炼6min,再依次加入氧化锌、硬脂酸、防老剂、促进剂、炭黑、聚丙烯酸钠和硫磺,混炼20min,薄通,置于平板硫化机上硫化,163℃温度下硫化2.5min,得到吸水料;
取吸水料,无水乙醇溶解,超声分散35min,加入3-氨丙基三甲氧基硅氧烷,反应6.1h,冷却至室温,醇洗2次,水洗2次,冷冻干燥,研磨粉碎,过200目筛,得到改性吸水料;
S3:吸水微球的制备:
取邻苯二酚、己二胺,去离子水溶解,搅拌25min,加入二氧化硅微球,继续搅拌15min,室温下反应37h,离心分离,洗涤后置于刻蚀液中,搅拌30min,离心分离,洗涤,40℃下真空干燥24h,得到改性微球;其中刻蚀液包括氢氟酸和氟化铵,所述氢氟酸和氟化铵的体积比为1:1;
取改性吸水料,盐酸溶解,搅拌8min,过滤,洗涤,得到物料A;取改性微球,氢氧化钠溶液溶解,搅拌8min,过滤,洗涤,得到物料B;取物料B,无水乙醇溶解,再加入物料A,搅拌15min,过滤,洗涤,40℃下真空干燥,得到吸水微球;
S4:表面改性剂的制备:
取磷酸,加热升温至210℃,反应30min,加入冰乙酸和无水哌嗪,调温至113℃,反应3.1h,抽滤,真空干燥,得到阻燃剂;
取六水合氯化铝、无水乙醇、去离子水和甲酰胺,搅拌16min,加入正硅酸四乙酯,搅拌25h,再加入阻燃剂和吸水微球,继续搅拌12min,接着添加1,2-环氧丙烷,搅拌4.5min,得到表面改性剂;
S5:取底布,无水***清洗5.5h,去离子水清洗,干燥后置于氢氧化钠溶液中,浸泡0.9h,去离子水洗涤,烘干,再置于表面改性剂中浸泡4min,取出底布,室温下静置22h,老化干燥,得到预处理底布;
S6:取面布,表面通过热熔胶贴合TPE膜,橡胶压辊压紧,蒸发固化43h,得到预处理面布;再取预处理底布,将预处理面布贴合至预处理底布表面,橡胶压辊压紧贴合,蒸发固化42h,再置于110℃下烘干35s,升温至150℃,烘焙2.5min,得到贴合面料。
本实例中,表面改性剂各组分原料包括:以重量计,阻燃剂6份、吸水微球11份、六水合氯化铝9份、无水乙醇28份、甲酰胺5份、正硅酸四乙酯5份、1,2-环氧丙烷12份。
吸水料各组分原料包括:以重量计,丁腈橡胶95份、改性橡胶35份、硅橡胶25份、氧化石墨烯7份、氧化锌4.5份、硬脂酸1.5份、防老剂2.5份、促进剂3.5份、炭黑9份、聚丙烯酸钠32份、硫磺2.5份;二氧化硅微球的粒径为0.09mm。
实例3:
S1:准备物料;
S2:改性吸水料的制备:
取叔丁基过氧化氢和三氧化钼,混合搅拌20min,加热升温至75℃,搅拌反应2.5h,反应后加入丁腈橡胶,80℃下搅拌反应80min,无水乙醇洗涤,40℃下真空干燥,得到改性橡胶;
取乙烯基硅油、白炭黑和氢氧化铝,混合搅拌3.5h,真空条件下继续加热至210℃,搅拌2.2h,再加入铂金催化剂和含氢硅油,继续搅拌30min,145℃下模压成型,模压时间为20min,得到硅橡胶;
取丁腈橡胶、改性橡胶,塑炼7min,加入硅橡胶和氧化石墨烯,混炼7min,再依次加入氧化锌、硬脂酸、防老剂、促进剂、炭黑、聚丙烯酸钠和硫磺,混炼25min,薄通,置于平板硫化机上硫化,165℃温度下硫化3min,得到吸水料;
取吸水料,无水乙醇溶解,超声分散40min,加入3-氨丙基三甲氧基硅氧烷,反应6.2h,冷却至室温,醇洗3次,水洗3次,冷冻干燥,研磨粉碎,过200目筛,得到改性吸水料;
S3:吸水微球的制备:
取邻苯二酚、己二胺,去离子水溶解,搅拌30min,加入二氧化硅微球,继续搅拌20min,室温下反应38h,离心分离,洗涤后置于刻蚀液中,搅拌35min,离心分离,洗涤,40℃下真空干燥24h,得到改性微球;其中刻蚀液包括氢氟酸和氟化铵,所述氢氟酸和氟化铵的体积比为1:1;
取改性吸水料,盐酸溶解,搅拌10min,过滤,洗涤,得到物料A;取改性微球,氢氧化钠溶液溶解,搅拌10min,过滤,洗涤,得到物料B;取物料B,无水乙醇溶解,再加入物料A,搅拌20min,过滤,洗涤,40℃下真空干燥,得到吸水微球;
S4:表面改性剂的制备:
取磷酸,加热升温至220℃,反应35min,加入冰乙酸和无水哌嗪,调温至115℃,反应3.2h,抽滤,真空干燥,得到阻燃剂;
取六水合氯化铝、无水乙醇、去离子水和甲酰胺,搅拌18min,加入正硅酸四乙酯,搅拌26h,再加入阻燃剂和吸水微球,继续搅拌15min,接着添加1,2-环氧丙烷,搅拌5min,得到表面改性剂;
S5:取底布,无水***清洗6h,去离子水清洗,干燥后置于氢氧化钠溶液中,浸泡1h,去离子水洗涤,烘干,再置于表面改性剂中浸泡5min,取出底布,室温下静置24h,老化干燥,得到预处理底布;
S6:取面布,表面通过热熔胶贴合TPE膜,橡胶压辊压紧,蒸发固化45h,得到预处理面布;再取预处理底布,将预处理面布贴合至预处理底布表面,橡胶压辊压紧贴合,蒸发固化45h,再置于120℃下烘干40s,升温至160℃,烘焙3min,得到贴合面料。
本实例中,表面改性剂各组分原料包括:以重量计,阻燃剂7份、吸水微球12份、六水合氯化铝10份、无水乙醇30份、甲酰胺6份、正硅酸四乙酯6份、1,2-环氧丙烷14份。
吸水料各组分原料包括:以重量计,丁腈橡胶100份、改性橡胶40份、硅橡胶30份、氧化石墨烯8份、氧化锌5份、硬脂酸2份、防老剂3份、促进剂4份、炭黑10份、聚丙烯酸钠35份、硫磺3份;二氧化硅微球的粒径为0.1mm。
对比例1:(缺少吸水微球)
S1:准备物料;
S2:表面改性剂的制备:
取磷酸,加热升温至210℃,反应30min,加入冰乙酸和无水哌嗪,调温至113℃,反应3.1h,抽滤,真空干燥,得到阻燃剂;
取六水合氯化铝、无水乙醇、去离子水和甲酰胺,搅拌16min,加入正硅酸四乙酯,搅拌25h,再加入阻燃剂,继续搅拌12min,接着添加1,2-环氧丙烷,搅拌4.5min,得到表面改性剂;
S3:取底布,无水***清洗5.5h,去离子水清洗,干燥后置于氢氧化钠溶液中,浸泡0.9h,去离子水洗涤,烘干,再置于表面改性剂中浸泡4min,取出底布,室温下静置22h,老化干燥,得到预处理底布;
S4:取面布,表面通过热熔胶贴合TPE膜,橡胶压辊压紧,蒸发固化43h,得到预处理面布;再取预处理底布,将预处理面布贴合至预处理底布表面,橡胶压辊压紧贴合,蒸发固化42h,再置于110℃下烘干35s,升温至150℃,烘焙2.5min,得到贴合面料。
本实例中,表面改性剂各组分原料包括:以重量计,阻燃剂6份、六水合氯化铝9份、无水乙醇28份、甲酰胺5份、正硅酸四乙酯5份、1,2-环氧丙烷12份。
对比例2:(缺少吸水微球、阻燃剂)
S1:准备物料;
S2:表面改性剂的制备:
取六水合氯化铝、无水乙醇、去离子水和甲酰胺,搅拌16min,加入正硅酸四乙酯,搅拌25h,再添加1,2-环氧丙烷,搅拌4.5min,得到表面改性剂;
S3:取底布,无水***清洗5.5h,去离子水清洗,干燥后置于氢氧化钠溶液中,浸泡0.9h,去离子水洗涤,烘干,再置于表面改性剂中浸泡4min,取出底布,室温下静置22h,老化干燥,得到预处理底布;
S4:取面布,表面通过热熔胶贴合TPE膜,橡胶压辊压紧,蒸发固化43h,得到预处理面布;再取预处理底布,将预处理面布贴合至预处理底布表面,橡胶压辊压紧贴合,蒸发固化42h,再置于110℃下烘干35s,升温至150℃,烘焙2.5min,得到贴合面料。
本实例中,表面改性剂各组分原料包括:以重量计,六水合氯化铝9份、无水乙醇28份、甲酰胺5份、正硅酸四乙酯5份、1,2-环氧丙烷12份。
对比例3:(缺少吸水微球、阻燃剂、表面改性剂)
S1:准备物料;
S2:取底布,无水***清洗5.5h,去离子水清洗,干燥后置于氢氧化钠溶液中,浸泡0.9h,去离子水洗涤,烘干,得到预处理底布;
S3:取面布,表面通过热熔胶贴合TPE膜,橡胶压辊压紧,蒸发固化43h,得到预处理面布;再取预处理底布,将预处理面布贴合至预处理底布表面,橡胶压辊压紧贴合,蒸发固化42h,再置于110℃下烘干35s,升温至150℃,烘焙2.5min,得到贴合面料。
实验:
分别取实例1-3、对比例1-3中制备的贴合面料,分别依据GB/T5455-1997《纺织品燃烧性能试验垂直法》测定阻燃性能,检测数据如下表所示:
由上表可知,实例1-3分别与对比例1-3形成对照实验,实验可证明,阻燃剂、吸水微球的添加均可有效提高贴合面料的阻燃性能。
结论:本发明工艺设计合理,操作简单,制备得到具有优异阻燃性能的三层贴合面料,该贴合面料挺括性好,可广泛应用于服装领域,实用性较高。
对于本领域技术人员而言,显然本发明不限于上述示范性实例的细节,而且在不背离本发明的精神或基本特征的情况下,能够以其他的具体形式实现本发明。因此,无论从哪一点来看,均应将实例看作是示范性的,而且是非限制性的,本发明的范围由所附权利要求而不是上述说明限定,因此旨在将落在权利要求的等同要件的含义和范围内的所有变化囊括在本发明内。
Claims (6)
1.一种高牢度弹力牛仔贴合面料,其特征在于:所述贴合面料包括预处理底布、面布和TPE膜,所述面布通过热熔胶贴合在预处理底布上,所述TPE膜通过热熔胶贴合在面布上;所述预处理底布由底布、表面改性剂改性制得;
所述表面改性剂各组分原料包括:以重量计,阻燃剂5-7份、吸水微球10-12份、六水合氯化铝8-10份、无水乙醇25-30份、甲酰胺4-6份、正硅酸四乙酯4-6份、1,2-环氧丙烷10-14份;
所述吸水微球由改性微球、改性吸水料、无水乙醇制备得到;所述阻燃剂由磷酸、冰乙酸、无水哌嗪制备得到;
所述改性吸水料由吸水料、3-氨丙基三甲氧基硅氧烷、无水乙醇制得,所述吸水料各组分原料包括:以重量计,丁腈橡胶90-100份、改性橡胶30-40份、硅橡胶20-30份、氧化石墨烯6-8份、氧化锌4-5份、硬脂酸1-2份、防老剂2-3份、促进剂3-4份、炭黑8-10份、聚丙烯酸钠30-35份、硫磺2-3份;
所述改性橡胶由叔丁基过氧化氢、三氧化钼、丁腈橡胶制备得到;所述硅橡胶由乙烯基硅油、白炭黑、氢氧化铝、铂金催化剂、含氢硅油制备得到;
所述改性微球由邻苯二酚、己二胺、二氧化硅微球制备得到。
2.根据权利要求1所述的一种高牢度弹力牛仔贴合面料,其特征在于:所述面布为95%-98%棉和2%-5%氨纶牛仔混合而成;所述底布为尼龙网眼布。
3.根据权利要求1所述的一种高牢度弹力牛仔贴合面料,其特征在于:所述二氧化硅微球的粒径为0.08-0.1mm。
4.一种根据权利要求1所述的高牢度弹力牛仔贴合面料的制备方法,其特征在于:包括以下步骤:
1)准备物料;
2)改性吸水料的制备:
a)取叔丁基过氧化氢和三氧化钼,混合搅拌,加热升温至70-75℃,搅拌反应,反应后加入丁腈橡胶,60-80℃下搅拌反应,洗涤,真空干燥,得到改性橡胶;
b)取乙烯基硅油、白炭黑和氢氧化铝,混合搅拌,真空条件下继续加热至200-210℃,搅拌,再加入铂金催化剂和含氢硅油,继续搅拌,140-145℃下模压成型,得到硅橡胶;
c)取丁腈橡胶、改性橡胶,塑炼,加入硅橡胶和氧化石墨烯,混炼,再依次加入氧化锌、硬脂酸、防老剂、促进剂、炭黑、聚丙烯酸钠和硫磺,混炼,薄通,置于平板硫化机上硫化,得到吸水料;
d)取吸水料,无水乙醇溶解,超声分散,加入3-氨丙基三甲氧基硅氧烷,反应,冷却至室温,醇洗,水洗,冷冻干燥,研磨粉碎,过200目筛,得到改性吸水料;
3)吸水微球的制备:
a)取邻苯二酚、己二胺,去离子水溶解,搅拌,加入二氧化硅微球,继续搅拌,室温下反应,离心分离,洗涤后置于刻蚀液中,搅拌,离心分离,洗涤,真空干燥,得到改性微球;
b)取改性吸水料,盐酸溶解,搅拌,过滤,洗涤,得到物料A;取改性微球,氢氧化钠溶液溶解,搅拌,过滤,洗涤,得到物料B;取物料B,无水乙醇溶解,再加入物料A,搅拌,过滤,洗涤,真空干燥,得到吸水微球;
4)表面改性剂的制备:
a)取磷酸,加热升温至200-220℃,反应,加入冰乙酸和无水哌嗪,调温至110-115℃,继续反应,抽滤,真空干燥,得到阻燃剂;
b)取六水合氯化铝、无水乙醇、去离子水和甲酰胺,搅拌,加入正硅酸四乙酯,搅拌,再加入阻燃剂和吸水微球,继续搅拌,接着添加1,2-环氧丙烷,搅拌,得到表面改性剂;
5)取底布,清洗,干燥后置于氢氧化钠溶液中浸泡,去离子水洗涤,烘干,再置于表面改性剂中浸泡,取出底布,室温下静置,老化干燥,得到预处理底布;
6)取面布,表面通过热熔胶贴合TPE膜,橡胶压辊压紧,蒸发固化,得到预处理面布;再取预处理底布,将预处理面布贴合至预处理底布表面,橡胶压辊压紧贴合,蒸发固化,再置于100-120℃下烘干,升温至140-160℃,烘焙,得到贴合面料。
5.根据权利要求4所述的一种高牢度弹力牛仔贴合面料的制备方法,其特征在于:包括以下步骤:
1)准备物料;
2)改性吸水料的制备:
a)取叔丁基过氧化氢和三氧化钼,混合搅拌10-20min,加热升温至70-75℃,搅拌反应2-2.5h,反应后加入丁腈橡胶,60-80℃下搅拌反应30-80min,无水乙醇洗涤,40℃下真空干燥,得到改性橡胶;
b)取乙烯基硅油、白炭黑和氢氧化铝,混合搅拌3-3.5h,真空条件下继续加热至200-210℃,搅拌2-2.2h,再加入铂金催化剂和含氢硅油,继续搅拌20-30min,140-145℃下模压成型,模压时间为15-20min,得到硅橡胶;
c)取丁腈橡胶、改性橡胶,塑炼5-7min,加入硅橡胶和氧化石墨烯,混炼5-7min,再依次加入氧化锌、硬脂酸、防老剂、促进剂、炭黑、聚丙烯酸钠和硫磺,混炼15-25min,薄通,置于平板硫化机上硫化,160-165℃温度下硫化2-3min,得到吸水料;
d)取吸水料,无水乙醇溶解,超声分散30-40min,加入3-氨丙基三甲氧基硅氧烷,反应6-6.2h,冷却至室温,醇洗2-3次,水洗2-3次,冷冻干燥,研磨粉碎,过200目筛,得到改性吸水料;
3)吸水微球的制备:
a)取邻苯二酚、己二胺,去离子水溶解,搅拌20-30min,加入二氧化硅微球,继续搅拌10-20min,室温下反应36-38h,离心分离,洗涤后置于刻蚀液中,搅拌25-35min,离心分离,洗涤,40℃下真空干燥24h,得到改性微球;
b)取改性吸水料,盐酸溶解,搅拌5-10min,过滤,洗涤,得到物料A;取改性微球,氢氧化钠溶液溶解,搅拌5-10min,过滤,洗涤,得到物料B;取物料B,无水乙醇溶解,再加入物料A,搅拌10-20min,过滤,洗涤,40℃下真空干燥,得到吸水微球;
4)表面改性剂的制备:
a)取磷酸,加热升温至200-220℃,反应25-35min,加入冰乙酸和无水哌嗪,调温至110-115℃,反应3-3.2h,抽滤,真空干燥,得到阻燃剂;
b)取六水合氯化铝、无水乙醇、去离子水和甲酰胺,搅拌15-18min,加入正硅酸四乙酯,搅拌24-26h,再加入阻燃剂和吸水微球,继续搅拌10-15min,接着添加1,2-环氧丙烷,搅拌4-5min,得到表面改性剂;
5)取底布,无水***清洗5-6h,去离子水清洗,干燥后置于氢氧化钠溶液中,浸泡0.8-1h,去离子水洗涤,烘干,再置于表面改性剂中浸泡3-5min,取出底布,室温下静置20-24h,老化干燥,得到预处理底布;
6)取面布,表面通过热熔胶贴合TPE膜,橡胶压辊压紧,蒸发固化40-45h,得到预处理面布;再取预处理底布,将预处理面布贴合至预处理底布表面,橡胶压辊压紧贴合,蒸发固化40-45h,再置于100-120℃下烘干30-40s,升温至140-160℃,烘焙2-3min,得到贴合面料。
6.根据权利要求5所述的一种高牢度弹力牛仔贴合面料的制备方法,其特征在于:步骤3)的a)步骤中,所述刻蚀液包括氢氟酸和氟化铵,所述氢氟酸和氟化铵的体积比为1:1。
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