CN112853619B - 一种环保的空气过滤无纺布及其生产工艺和应用 - Google Patents
一种环保的空气过滤无纺布及其生产工艺和应用 Download PDFInfo
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- CN112853619B CN112853619B CN202011640341.7A CN202011640341A CN112853619B CN 112853619 B CN112853619 B CN 112853619B CN 202011640341 A CN202011640341 A CN 202011640341A CN 112853619 B CN112853619 B CN 112853619B
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Classifications
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- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
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- D04H1/56—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties by welding together the fibres, e.g. by partially melting or dissolving in association with fibre formation, e.g. immediately following extrusion of staple fibres
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B01D39/00—Filtering material for liquid or gaseous fluids
- B01D39/08—Filter cloth, i.e. woven, knitted or interlaced material
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- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
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- D—TEXTILES; PAPER
- 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
- D06M10/00—Physical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. ultrasonic, corona discharge, irradiation, electric currents, or magnetic fields; Physical treatment combined with treatment with chemical compounds or elements
- D06M10/02—Physical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. ultrasonic, corona discharge, irradiation, electric currents, or magnetic fields; Physical treatment combined with treatment with chemical compounds or elements ultrasonic or sonic; Corona discharge
- D06M10/025—Corona discharge or low temperature plasma
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- D—TEXTILES; PAPER
- 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
- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/322—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing nitrogen
- D06M13/325—Amines
- D06M13/328—Amines the amino group being bound to an acyclic or cycloaliphatic carbon atom
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- D—TEXTILES; PAPER
- 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
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
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Abstract
本发明提供一种环保的空气过滤无纺布的生产工艺,属于空气过滤技术领域,将聚丙烯、驻极母粒和高分子驻极体混合均匀,将制得的混合料喂入螺杆挤出机,经所述螺杆挤出机熔融挤出形成熔体,熔体通过喷丝板喷出形成纤维,所述纤维经过恒温恒压的热风牵伸,在网帘上形成熔喷布,再依次经过红外辐射热处理、高压驻极处理和冷却处理后收卷得到所述空气过滤无纺布,所述驻极母粒由聚丙烯、少层石墨烯纳米片、抗氧化剂、相容剂、成核剂组成;所述少层石墨烯纳米片以具有面心立方结构的氧化镁微晶作为基底和模板,通过化学气相沉积法制备得到,所述驻极母粒提高了纤维的驻极化程度,同时提高电荷的储存稳定性,进而提高过滤性能。
Description
技术领域
本发明涉及空气过滤技术领域,具体涉及一种环保的空气过滤无纺布及其生产工艺和应用。
背景技术
现有研究显示,空气中由污染造成的颗粒物尤其是空气动力学当量小于等于2.5微米的颗粒物,其粒径小,且富含有毒有害物质,这些颗粒物在空气中能长时间停留,极易被人吸收进入身体从而引起引发呼吸系统疾病、伤肺、致癌、心血管疾病、生殖系统、胎儿发育等疾病。
常用的纤维过滤材料捕尘主要依靠布朗扩散、截留、惯性碰撞以及直接拦截等机阻挡过程,过滤材料和粒子之间的静电吸附作用甚微,对于小粒径的粒子过滤效率很差,采用更小的过滤孔道提高过滤效率时过滤阻力也很高,如果过滤材料在空气过滤的过程中增强静电吸附,除原有的机械阻挡作用外,依靠库仑力直接吸引气相中的带电微粒并将其捕获,或诱导中性微粒产生极性再将其捕获,从而更有效地过滤气体载体相中的亚微粒子,过滤效率大大增强,而空气阻力却不会增加。
通过熔喷技术生产的聚丙烯熔纤维很细,而且得到的熔喷布具有很大的比表面积,孔隙小而孔隙率大,因此过滤性、屏蔽性、绝热性和吸油性等应用特性是其它工艺生产的无纺布所难以实现的。一般来说,聚丙烯熔喷布广泛用于过滤材料、医疗卫生材料、吸油材料、擦拭布、保暖材料、电池隔膜材料及隔音材料等领域。因此聚丙烯熔喷布已大量应用于空气净化及医疗卫生行业,如用作空调滤网、医用防护口罩和防尘口罩等。
现有技术直接对熔喷聚丙烯材料进行驻极处理后,通过荷电纤维的库仑力实现对亚微粒子的捕获,但驻极处理后的熔喷聚丙烯纤维的电荷稳定性较低,难以保持良好的高效低阻性能。
发明内容
针对上述问题,本发明提供一种环保的空气过滤无纺布及其生产工艺和应用。
本发明的目的采用以下技术方案来实现:
一种环保的空气过滤无纺布的生产工艺,包括以下步骤:
S1、将聚丙烯、驻极母粒和高分子驻极体混合均匀,制得混合料;其中,所述聚丙烯、所述驻极母粒和所述高分子驻极体的重量比为100:(4-8):(0.1-1);
S2、将所述混合料喂入螺杆挤出机,经所述螺杆挤出机熔融挤出形成熔体;
S3、所述熔体恒温保温在管道中,经计量泵计量后通过喷丝板喷出形成纤维,所述纤维经过恒温恒压的热风牵伸,在网帘上形成熔喷布;
S4、将S3制得的熔喷布依次进行恒温红外辐射热处理、5-6万伏的高压驻极处理和冷却处理后收卷得到所述空气过滤无纺布;
所述驻极母粒由聚丙烯、少层石墨烯纳米片、抗氧化剂、相容剂、成核剂组成;所述驻极母粒的制备方法包括以下步骤:
a1、称取5g的的氧化镁微晶粉末并置于氧化铝陶瓷舟中,将装有氧化镁微晶粉末的陶瓷舟移入管式炉中部,封闭管式炉,以氩气置换管内空气,调节氩气流量恒定在100-120ml/min,管式炉逐渐加热升温至920-1000℃,升温速率8-10℃/min,待升温至目标温度后保温10-30min,气氛切转为甲烷和氢气的混合气体,所述混合气体的流量恒定为60-72ml/min,开始在所述氧化镁微晶表面沉积少层石墨烯,沉积时间90-100min,沉积完成后将气氛切换为氩气,待管式炉自然冷却至室温,得到黑灰色的粉末状产物,将所述黑灰色粉末状产物转移至盐酸溶液中,缓慢搅拌12h以上,滤出不溶物,以去离子水洗涤至洗涤液中无金属离子检出,得到黑色粉末,将所述黑色粉末超声分散在质量分数15%的聚乙二醇水溶液中,再次过滤,得到所述少层石墨烯纳米片;
其中,所述氧化镁微晶粉末的纯度不小于99.9%;所述混合气体中甲烷和氢气的体积比为1:5,所述超声分散功率为200W,超声时间10-30min;
a2、按设定比例称取所述驻极母粒的各组成组分,加入到高速混合机中混合1-3min,混合转速1000-2000rpm,得到预混料;所述预混料经双螺杆挤出机熔融挤出,螺杆各区温度为190~230℃,真空造粒制得所述驻极母粒。
优选的,所述高分子驻极体为聚碳酸酯、聚甲基丙烯酸甲酯、聚偏氟乙烯中的一种或多种。
优选的,所述聚丙烯、所述少层石墨烯纳米片、所述抗氧化剂、所述相容剂和所述成核剂的重量比例为100:(8-18):(2-5):(1-2):(1-2)。
优选的,所述抗氧化剂为四[β-(3,5-二叔丁基-4-羟基苯基)丙酸]季戊四醇酯、β-(3,5-二叔丁基-4-羟基苯基)丙酸正十八碳醇酯或二缩三乙二醇双[β-(3-叔丁基-4-羟基-5-甲基苯基)丙酸酯]。
优选的,所述相容剂为马来酸酐接枝聚丙烯、马来酸酐接枝丙烯基弹性体、甲基丙烯酸甲酯接枝聚丙烯、甲基丙烯酸甲酯接枝丙烯基弹性体、甲基丙烯酸缩水甘油酯接枝聚丙烯、甲基丙烯酸缩水甘油酯接枝丙烯基弹性体中的一种或多种。
优选的,所述成核剂为硬脂酸盐,所述硬脂酸盐为硬脂酸锂、硬脂酸钠、硬脂酸镁、硬脂酸钙、硬脂酸钡、硬脂酸锌、二硬脂酸铝中的一种或多种。
优选的,步骤S3中所述熔喷布的制备还包括表面改性处理,所述表面改性处理包括以下步骤:
b1、保护气氛下,在10ml的甲基丙烯酸中加入0.65g的十二烷基三硫代碳酸酯和20ml的二甲酰胺溶液,充分搅拌均匀后加入0.07g的偶氮引发剂,再次搅拌后除氧,在保护气氛下,将混合溶液升温至70-75℃,保温反应8-10h,反应结束后自然冷却至室温,加入质量分数50%的乙醇溶液稀释,再加入乙醚析出聚合物沉淀,将沉淀分离并真空干燥,加入至50ml的去离子水中溶解,经吹氮除氧后加入12-14ml的乙醇胺,在保护气氛下搅拌反应20h,得到白色悬液,调节所述白色悬液的pH为3-4,过滤,滤液经透析后冻干,得到端巯基修饰的聚甲基丙烯酸;
b2、称取10g的干燥短绒棉纤维,加入至200ml的二甲酰胺溶液中,搅拌并升温至100℃,保温搅拌反应2h,撤去热源,加入20g的无水氯化锂,继续搅拌使冷却至常温,加入30ml的三乙胺溶液,搅拌均匀后,在冰水浴条件下逐滴滴加20ml对氯化甲苯砜的二甲酰胺溶液,滴加完毕后继续搅拌反应24h,静置沉淀后滤出沉淀,依次以去离子水和无水乙醇洗涤,干燥后溶解在80ml的二甲亚砜中,加入15ml的乙二胺溶液,100℃搅拌反应4h,冷却至室温后加入丙酮析出沉淀,沉淀依次以丙酮和无水乙醇洗涤,干燥后得到氨基改性纤维素,以质量分数1%的醋酸溶液配制为3g/L的溶液,得到氨基改性纤维素溶液;其中,所述对氯化甲苯砜的二甲酰胺溶液中对氯化甲苯砜的质量分数为10%;
b3、配制pH值为8.5的三羟甲基氨基甲烷-盐酸缓冲溶液,以所述缓冲溶液分别配制3g/L的多巴胺溶液和5g/L的端巯基修饰的聚甲基丙烯酸溶液;
b4、将所述熔喷布置于等离子体清洗机中清洗3-5min,在清洗后的熔喷布表面喷涂所述多巴胺溶液,自然晾干后以蒸馏水冲洗,氮气吹干后喷涂氨基纤维素溶液,自然晾干后以蒸馏水冲洗,氮气吹干后喷涂所述端巯基修饰的聚甲基丙烯酸溶液,无氧环境下50℃保温24h,接枝完成后以蒸馏水冲洗,干燥。
优选的,所述多巴胺溶液的喷涂量为4-5ml/m2,所述氨基纤维素溶液的喷涂量为2-3ml/m2,所述端巯基修饰的聚甲基丙烯酸溶液的喷涂量为5-7ml/m2。
所制备的空气过滤无纺布可用作个人护理、医疗防护、工业气体过滤、发动机气体过滤、洁净室空气过滤、空气净化器、室内新风系统中的空气过滤材料。
本发明的有益效果为:
针对现有技术中过滤效率较低的问题,本发明利用具有面心立方结构的氧化镁微晶作为基底和模板,制备了自带电荷性质的石墨烯纳米片,将其添加到聚丙烯驻极母粒中,一方面,石墨烯纳米片本身自带的电荷性质提高了纤维本身的荷电性,另一方面,分散在熔体间的纳米片层结构间形成了无数的微型电容,在纤维内形成内电场,提高了纤维的驻极化效果,同时提高电荷的储存稳定性,进而提高过滤性能,对病菌的杀灭活性也得到了明显的提高,避免了废弃的过滤无纺布对环境造成的病菌二次污染;本发明所述无纺布柔软、均匀、致密,驻极效果佳,过滤效率和电荷保持率高,过滤长效达1年以上。
具体实施方式
结合以下实施例对本发明作进一步描述。
本发明的实施例涉及一种环保的空气过滤无纺布的生产工艺,包括以下步骤:
S1、将聚丙烯、驻极母粒和高分子驻极体混合均匀,制得混合料;其中,所述聚丙烯、所述驻极母粒和所述高分子驻极体的重量比为100:(4-8):(0.1-1);
S2、将所述混合料喂入螺杆挤出机,经所述螺杆挤出机熔融挤出形成熔体;
S3、所述熔体恒温保温在管道中,经计量泵计量后通过喷丝板喷出形成纤维,所述纤维经过恒温恒压的热风牵伸,在网帘上形成熔喷布;
S4、将S3制得的熔喷布依次进行恒温红外辐射热处理、5-6万伏的高压驻极处理和冷却处理后收卷得到所述空气过滤无纺布;
所述驻极母粒由聚丙烯、少层石墨烯纳米片、抗氧化剂、相容剂、成核剂组成;所述驻极母粒的制备方法包括以下步骤:
a1、称取5g的的氧化镁微晶粉末并置于氧化铝陶瓷舟中,将装有氧化镁微晶粉末的陶瓷舟移入管式炉中部,封闭管式炉,以氩气置换管内空气,调节氩气流量恒定在100-120ml/min,管式炉逐渐加热升温至920-1000℃,升温速率8-10℃/min,待升温至目标温度后保温10-30min,气氛切转为甲烷和氢气的混合气体,所述混合气体的流量恒定为60-72ml/min,开始在所述氧化镁微晶表面沉积少层石墨烯,沉积时间90-100min,沉积完成后将气氛切换为氩气,待管式炉自然冷却至室温,得到黑灰色的粉末状产物,将所述黑灰色粉末状产物转移至盐酸溶液中,缓慢搅拌12h以上,滤出不溶物,以去离子水洗涤至洗涤液中无金属离子检出,得到黑色粉末,将所述黑色粉末超声分散在质量分数15%的聚乙二醇水溶液中,再次过滤,得到所述少层石墨烯纳米片;
其中,所述氧化镁微晶粉末的纯度不小于99.9%;所述混合气体中甲烷和氢气的体积比为1:5,所述超声分散功率为200W,超声时间10-30min;
a2、按设定比例称取所述驻极母粒的各组成组分,加入到高速混合机中混合1-3min,混合转速1000-2000rpm,得到预混料;所述预混料经双螺杆挤出机熔融挤出,螺杆各区温度为190~230℃,真空造粒制得所述驻极母粒。
本发明以氧化镁微晶作为生长基底,以甲烷为碳源,使用化学气相沉积方法实现少层石墨烯的控制生长,石墨烯层的厚度在2-30nm,由于氧化镁具有O2-离子的NaCl型面心立方结构,沉积的石墨烯层复制了氧化镁微晶的形貌和离子取向,再利用盐酸溶液侵蚀除去氧化镁基底后,可以得到具有三维结构的空心立方结构的少层石墨烯,经超声处理后,立体结构的石墨烯破裂形成自带电荷性质的纳米片,将其添加到聚丙烯驻极母粒中,一方面,石墨烯纳米片本身自带的电荷性质提高了纤维本身的荷电性,另一方面,分散在熔体间的纳米片层结构间形成了无数的微型电容,在纤维内形成内电场,提高了纤维的驻极化效果,同时提高电荷的储存稳定性,进而提高过滤性能,对病菌的杀灭活性也得到了明显的提高,避免了废弃的过滤无纺布对环境造成的病菌二次污染;
本发明所述驻极母粒同时包含了改性剂和助剂,采用一步法合成,使驻极母粒可均匀分散于聚丙烯中,避免了分散不均匀、过滤效果不稳定等情况,助剂的加入进一步提高了纤维致密性及均匀性;加入驻极母粒之后,在保证常规的物理碰撞阻隔作用基础上,增强了静电吸附作用;驻极处理使得纤维载有电荷,结合熔喷超细纤维材料致密的特点,带电纤维间形成了大量的电极,不仅能够像磁铁一样吸引环境中大部分的带电微粒,同时也可将未带电的部分颗粒极化,使熔喷布的驻极效果大大改善,其表面电荷密度、过滤性能及电荷保持率均明显提高;
优选的,所述高分子驻极体为聚碳酸酯、聚甲基丙烯酸甲酯、聚偏氟乙烯中的一种或多种。
高分子驻极体是具驻极体功能的高分子材料,高分子驻极体具有优良的电荷贮存能力,即保持注入电荷的能力和偶极指向性,将其添加到所述驻极母粒中可以进一步提高纤维电荷的储存稳定性。
优选的,所述聚丙烯、所述少层石墨烯纳米片、所述抗氧化剂、所述相容剂和所述成核剂的重量比例为100:(8-18):(2-5):(1-2):(1-2)。
优选的,所述抗氧化剂为四[β-(3,5-二叔丁基-4-羟基苯基)丙酸]季戊四醇酯、β-(3,5-二叔丁基-4-羟基苯基)丙酸正十八碳醇酯或二缩三乙二醇双[β-(3-叔丁基-4-羟基-5-甲基苯基)丙酸酯]。
优选的,所述相容剂为马来酸酐接枝聚丙烯、马来酸酐接枝丙烯基弹性体、甲基丙烯酸甲酯接枝聚丙烯、甲基丙烯酸甲酯接枝丙烯基弹性体、甲基丙烯酸缩水甘油酯接枝聚丙烯、甲基丙烯酸缩水甘油酯接枝丙烯基弹性体中的一种或多种。
优选的,所述成核剂为硬脂酸盐,所述硬脂酸盐为硬脂酸锂、硬脂酸钠、硬脂酸镁、硬脂酸钙、硬脂酸钡、硬脂酸锌、二硬脂酸铝中的一种或多种。
优选的,步骤S3中所述熔喷布的制备还包括表面改性处理,所述表面改性处理包括以下步骤:
b1、保护气氛下,在10ml的甲基丙烯酸中加入0.65g的十二烷基三硫代碳酸酯和20ml的二甲酰胺溶液,充分搅拌均匀后加入0.07g的偶氮引发剂,再次搅拌后除氧,在保护气氛下,将混合溶液升温至70-75℃,保温反应8-10h,反应结束后自然冷却至室温,加入质量分数50%的乙醇溶液稀释,再加入乙醚析出聚合物沉淀,将沉淀分离并真空干燥,加入至50ml的去离子水中溶解,经吹氮除氧后加入12-14ml的乙醇胺,在保护气氛下搅拌反应20h,得到白色悬液,调节所述白色悬液的pH为3-4,过滤,滤液经透析后冻干,得到端巯基修饰的聚甲基丙烯酸;
b2、称取10g的干燥短绒棉纤维,加入至200ml的二甲酰胺溶液中,搅拌并升温至100℃,保温搅拌反应2h,撤去热源,加入20g的无水氯化锂,继续搅拌使冷却至常温,加入30ml的三乙胺溶液,搅拌均匀后,在冰水浴条件下逐滴滴加20ml对氯化甲苯砜的二甲酰胺溶液,滴加完毕后继续搅拌反应24h,静置沉淀后滤出沉淀,依次以去离子水和无水乙醇洗涤,干燥后溶解在80ml的二甲亚砜中,加入15ml的乙二胺溶液,100℃搅拌反应4h,冷却至室温后加入丙酮析出沉淀,沉淀依次以丙酮和无水乙醇洗涤,干燥后得到氨基改性纤维素,以质量分数1%的醋酸溶液配制为3g/L的溶液,得到氨基改性纤维素溶液;其中,所述对氯化甲苯砜的二甲酰胺溶液中对氯化甲苯砜的质量分数为10%;
b3、配制pH值为8.5的三羟甲基氨基甲烷-盐酸缓冲溶液,以所述缓冲溶液分别配制3g/L的多巴胺溶液和5g/L的端巯基修饰的聚甲基丙烯酸溶液;
b4、将所述熔喷布置于等离子体清洗机中清洗3-5min,在清洗后的熔喷布表面喷涂所述多巴胺溶液,自然晾干后以蒸馏水冲洗,氮气吹干后喷涂氨基纤维素溶液,自然晾干后以蒸馏水冲洗,氮气吹干后喷涂所述端巯基修饰的聚甲基丙烯酸溶液,无氧环境下50℃保温24h,接枝完成后以蒸馏水冲洗,干燥。
优选的,所述多巴胺溶液的喷涂量为4-5ml/m2,所述氨基纤维素溶液的喷涂量为2-3ml/m2,所述端巯基修饰的聚甲基丙烯酸溶液的喷涂量为5-7ml/m2。
驻极母粒提高了空气过滤无纺布的表面电荷密度、过滤性能及电荷保持率,但极化后的纤维由于静电的排斥作用使纤维扩散成间隙尺寸更大的孔洞,阻碍了过滤吸附性能的进一步提升,本发明在所述驻极母粒改性的基础上,通过表面接枝聚甲基丙烯酸,在表面形成一层带有羧基负电荷的聚甲基丙烯酸分子刷结构,在保持过滤通量的同时进一步提高了电荷负载量和过滤效率;表面的接枝分子层作为辅助过滤层,可以吸附粒径较小的污染物,甚至病毒这种纳米级的物质也可进行静电吸附或电荷相斥阻隔,其中,多巴胺在有氧化剂且弱碱性环境下会发生自聚合形成聚多巴胺,聚多巴胺能够在多种基底表面实现黏附形成聚多巴胺涂层,基于聚多巴胺涂层中含有大量可以参与反应官能团的特点,可以提高无纺布表面的接枝活性,同时通过端巯基修饰,将聚甲基丙烯酸分子链接枝在过滤材料表面,为进一步提高聚甲基丙烯酸的接枝密度,以氨基改性纤维素进一步提高活性接枝位点。
实施例1
一种环保的空气过滤无纺布的生产工艺,包括以下步骤:
S1、将聚丙烯、驻极母粒和高分子驻极体混合均匀,制得混合料;其中,所述聚丙烯、所述驻极母粒和所述高分子驻极体的重量比为100:6:0.5;
S2、将所述混合料喂入螺杆挤出机,经所述螺杆挤出机熔融挤出形成熔体,所述螺杆挤出机的五个加热区域温度分别设定为160℃、180℃、200℃、220℃、225℃;
S3、所述熔体恒温保温在管道中,经计量泵计量后通过喷丝板喷出形成纤维,所述纤维经过恒温恒压的热风牵伸,在网帘上形成熔喷布;
S4、将S3制得的熔喷布依次进行恒温红外辐射热处理、5-6万伏的高压驻极处理和冷却处理后收卷得到所述空气过滤无纺布;
所述驻极母粒由聚丙烯、少层石墨烯纳米片、抗氧化剂、相容剂、成核剂组成,;所述驻极母粒的制备方法包括以下步骤:
a1、称取5g的的氧化镁微晶粉末并置于氧化铝陶瓷舟中,将装有氧化镁微晶粉末的陶瓷舟移入管式炉中部,封闭管式炉,以氩气置换管内空气,调节氩气流量恒定在100-120ml/min,管式炉逐渐加热升温至920-1000℃,升温速率8-10℃/min,待升温至目标温度后保温10-30min,气氛切转为甲烷和氢气的混合气体,所述混合气体的流量恒定为60-72ml/min,开始在所述氧化镁微晶表面沉积少层石墨烯,沉积时间90-100min,沉积完成后将气氛切换为氩气,待管式炉自然冷却至室温,得到黑灰色的粉末状产物,将所述黑灰色粉末状产物转移至盐酸溶液中,缓慢搅拌12h以上,滤出不溶物,以去离子水洗涤至洗涤液中无金属离子检出,得到黑色粉末,将所述黑色粉末超声分散在质量分数15%的聚乙二醇水溶液中,再次过滤,得到所述少层石墨烯纳米片,所述少层石墨烯纳米片边长在500-600nm,厚度在50-100nm;
其中,所述氧化镁微晶粉末的纯度不小于99.9%;所述混合气体中甲烷和氢气的体积比为1:5,所述超声分散功率为200W,超声时间10-30min;
a2、按所述聚丙烯、所述少层石墨烯纳米片、所述抗氧化剂、所述相容剂和所述成核剂的重量比例为100:12:3:1.3:1.1称取所述驻极母粒的各组成组分,加入到高速混合机中混合1-3min,混合转速1000-2000rpm,得到预混料;所述预混料经双螺杆挤出机熔融挤出,螺杆各区温度为190~230℃,真空造粒制得所述驻极母粒;
其中,所述高分子驻极体为聚偏氟乙烯;
所述抗氧化剂为β-(3,5-二叔丁基-4-羟基苯基)丙酸正十八碳醇酯或二缩三乙二醇双[β-(3-叔丁基-4-羟基-5-甲基苯基)丙酸酯];
所述相容剂为马来酸酐接枝聚丙烯、马来酸酐接枝丙烯基弹性体、甲基丙烯酸甲酯接枝聚丙烯、甲基丙烯酸甲酯接枝丙烯基弹性体;
所述成核剂为硬脂酸钠、硬脂酸镁、硬脂酸钙或硬脂酸锌。
实施例2
一种环保的空气过滤无纺布的生产工艺,包括以下步骤:
S1、将聚丙烯、驻极母粒和高分子驻极体混合均匀,制得混合料;其中,所述聚丙烯、所述驻极母粒和所述高分子驻极体的重量比为100:6:0.5;
S2、将所述混合料喂入螺杆挤出机,经所述螺杆挤出机熔融挤出形成熔体,所述螺杆挤出机的五个加热区域温度分别设定为160℃、180℃、200℃、220℃、225℃;
S3、所述熔体恒温保温在管道中,经计量泵计量后通过喷丝板喷出形成纤维,所述纤维经过恒温恒压的热风牵伸,在网帘上形成熔喷布,对所述熔喷布进行表面改性处理,具体为:
S4、保护气氛下,在10ml的甲基丙烯酸中加入0.65g的十二烷基三硫代碳酸酯和20ml的二甲酰胺溶液,充分搅拌均匀后加入0.07g的偶氮引发剂,再次搅拌后除氧,在保护气氛下,将混合溶液升温至70-75℃,保温反应8-10h,反应结束后自然冷却至室温,加入质量分数50%的乙醇溶液稀释,再加入乙醚析出聚合物沉淀,将沉淀分离并真空干燥,加入至50ml的去离子水中溶解,经吹氮除氧后加入12-14ml的乙醇胺,在保护气氛下搅拌反应20h,得到白色悬液,调节所述白色悬液的pH为3-4,过滤,滤液经透析后冻干,得到端巯基修饰的聚甲基丙烯酸;
S5、称取10g的干燥短绒棉纤维,加入至200ml的二甲酰胺溶液中,搅拌并升温至100℃,保温搅拌反应2h,撤去热源,加入20g的无水氯化锂,继续搅拌使冷却至常温,加入30ml的三乙胺溶液,搅拌均匀后,在冰水浴条件下逐滴滴加20ml对氯化甲苯砜的二甲酰胺溶液,滴加完毕后继续搅拌反应24h,静置沉淀后滤出沉淀,依次以去离子水和无水乙醇洗涤,干燥后溶解在80ml的二甲亚砜中,加入15ml的乙二胺溶液,100℃搅拌反应4h,冷却至室温后加入丙酮析出沉淀,沉淀依次以丙酮和无水乙醇洗涤,干燥后得到氨基改性纤维素,以质量分数1%的醋酸溶液配制为3g/L的溶液,得到氨基改性纤维素溶液;其中,所述对氯化甲苯砜的二甲酰胺溶液中对氯化甲苯砜的质量分数为10%;
S6、配制pH值为8.5的三羟甲基氨基甲烷-盐酸缓冲溶液,以所述缓冲溶液分别配制3g/L的多巴胺溶液和5g/L的端巯基修饰的聚甲基丙烯酸溶液;
S7、将所述熔喷布置于等离子体清洗机中清洗3-5min,在清洗后的熔喷布表面喷涂所述多巴胺溶液,喷涂量为4-5ml/m2,自然晾干后以蒸馏水冲洗,氮气吹干后喷涂氨基纤维素溶液,喷涂量为2-3ml/m2,自然晾干后以蒸馏水冲洗,氮气吹干后喷涂所述端巯基修饰的聚甲基丙烯酸溶液,喷涂量为5-7ml/m2,无氧环境下50℃保温24h,接枝完成后以蒸馏水冲洗,干燥,制得表面改性熔喷布;
S8、将S3制得的熔喷布依次进行恒温红外辐射热处理、5-6万伏的高压驻极处理和冷却处理后收卷得到所述空气过滤无纺布;
所述驻极母粒由聚丙烯、少层石墨烯纳米片、抗氧化剂、相容剂、成核剂组成,;所述驻极母粒的制备方法包括以下步骤:
a1、称取5g的的氧化镁微晶粉末并置于氧化铝陶瓷舟中,将装有氧化镁微晶粉末的陶瓷舟移入管式炉中部,封闭管式炉,以氩气置换管内空气,调节氩气流量恒定在100-120ml/min,管式炉逐渐加热升温至920-1000℃,升温速率8-10℃/min,待升温至目标温度后保温10-30min,气氛切转为甲烷和氢气的混合气体,所述混合气体的流量恒定为60-72ml/min,开始在所述氧化镁微晶表面沉积少层石墨烯,沉积时间90-100min,沉积完成后将气氛切换为氩气,待管式炉自然冷却至室温,得到黑灰色的粉末状产物,将所述黑灰色粉末状产物转移至盐酸溶液中,缓慢搅拌12h以上,滤出不溶物,以去离子水洗涤至洗涤液中无金属离子检出,得到黑色粉末,将所述黑色粉末超声分散在质量分数15%的聚乙二醇水溶液中,再次过滤,得到所述少层石墨烯纳米片;
其中,所述氧化镁微晶粉末的纯度不小于99.9%;所述混合气体中甲烷和氢气的体积比为1:5,所述超声分散功率为200W,超声时间10-30min;
a2、按所述聚丙烯、所述少层石墨烯纳米片、所述抗氧化剂、所述相容剂和所述成核剂的重量比例为100:12:3:1.3:1.1称取所述驻极母粒的各组成组分,加入到高速混合机中混合1-3min,混合转速1000-2000rpm,得到预混料;所述预混料经双螺杆挤出机熔融挤出,螺杆各区温度为190~230℃,真空造粒制得所述驻极母粒;
其中,所述高分子驻极体为聚偏氟乙烯;
所述抗氧化剂为β-(3,5-二叔丁基-4-羟基苯基)丙酸正十八碳醇酯或二缩三乙二醇双[β-(3-叔丁基-4-羟基-5-甲基苯基)丙酸酯];
所述相容剂为马来酸酐接枝聚丙烯、马来酸酐接枝丙烯基弹性体、甲基丙烯酸甲酯接枝聚丙烯、甲基丙烯酸甲酯接枝丙烯基弹性体;
所述成核剂为硬脂酸钠、硬脂酸镁、硬脂酸钙或硬脂酸锌。
对比例
同实施例1,但所述少层石墨烯纳米片以二氧化硅为基底制备。
性能测试
过滤效率的测定在符合GB/14295-2008《空气过滤器》的试验台进行测试,采用CLJ-03A型激光尘埃粒子计数器,TSI-8108大粒径气溶胶发生器,采样流量为2.83L/min,膜厚0.1mm;常温(温度15℃,湿度70%)静置15d后再次测定过滤,测试结果见下表:
最后应当说明的是,以上实施例仅用以说明本发明的技术方案,而非对本发明保护范围的限制,尽管参照较佳实施例对本发明作了详细地说明,本领域的普通技术人员应当理解,可以对本发明的技术方案进行修改或者等同替换,而不脱离本发明技术方案的实质和范围。
Claims (9)
1.一种环保的空气过滤无纺布的生产工艺,其特征在于,包括以下步骤:
S1、将聚丙烯、驻极母粒和高分子驻极体混合均匀,制得混合料;其中,所述聚丙烯、所述驻极母粒和所述高分子驻极体的重量比为100:(4-8):(0.1-1);
S2、将所述混合料喂入螺杆挤出机,经所述螺杆挤出机熔融挤出形成熔体;
S3、所述熔体恒温保温在管道中,经计量泵计量后通过喷丝板喷出形成纤维,所述纤维经过恒温恒压的热风牵伸,在网帘上形成熔喷布;
S4、将S3制得的熔喷布依次进行恒温红外辐射热处理、5-6万伏的高压驻极处理和冷却处理后收卷得到所述空气过滤无纺布;
所述驻极母粒由聚丙烯、少层石墨烯纳米片、抗氧化剂、相容剂、成核剂组成;所述驻极母粒的制备方法包括以下步骤:
a1、称取5g的氧化镁微晶粉末并置于氧化铝陶瓷舟中,将装有氧化镁微晶粉末的陶瓷舟移入管式炉中部,封闭管式炉,以氩气置换管内空气,调节氩气流量恒定在100-120ml/min,管式炉逐渐加热升温至920-1000℃,升温速率8-10℃/min,待升温至目标温度后保温10-30min,气氛切转为甲烷和氢气的混合气体,所述混合气体的流量恒定为60-72ml/min,开始在所述氧化镁微晶表面沉积少层石墨烯,沉积时间90-100min,沉积完成后将气氛切换为氩气,待管式炉自然冷却至室温,得到黑灰色的粉末状产物,将所述黑灰色粉末状产物转移至盐酸溶液中,缓慢搅拌12h以上,滤出不溶物,以去离子水洗涤至洗涤液中无金属离子检出,得到黑色粉末,将所述黑色粉末超声分散在质量分数15%的聚乙二醇水溶液中,再次过滤,得到所述少层石墨烯纳米片;
其中,所述氧化镁微晶粉末的纯度不小于99.9%;所述混合气体中甲烷和氢气的体积比为1:5,所述超声分散功率为200W,超声时间10-30min;
a2、按设定比例称取所述驻极母粒的各组成组分,加入到高速混合机中混合1-3min,混合转速1000-2000rpm,得到预混料;所述预混料经双螺杆挤出机熔融挤出,螺杆各区温度为190~230℃,真空造粒制得所述驻极母粒;
步骤S3中所述熔喷布还包括表面改性处理,所述表面改性处理包括以下步骤:
b1、保护气氛下,在10ml的甲基丙烯酸中加入0.65g的十二烷基三硫代碳酸酯和20ml的二甲酰胺溶液,充分搅拌均匀后加入0.07g的偶氮引发剂,再次搅拌后除氧,在保护气氛下,将混合溶液升温至70-75℃,保温反应8-10h,反应结束后自然冷却至室温,加入质量分数50%的乙醇溶液稀释,再加入乙醚析出聚合物沉淀,将沉淀分离并真空干燥,加入至50ml的去离子水中溶解,经吹氮除氧后加入12-14ml的乙醇胺,在保护气氛下搅拌反应20h,得到白色悬液,调节所述白色悬液的pH为3-4,过滤,滤液经透析后冻干,得到端巯基修饰的聚甲基丙烯酸;
b2、称取10g的干燥短绒棉纤维,加入至200ml的二甲酰胺溶液中,搅拌并升温至100℃,保温搅拌反应2h,撤去热源,加入20g的无水氯化锂,继续搅拌使冷却至常温,加入30ml的三乙胺溶液,搅拌均匀后,在冰水浴条件下逐滴滴加20ml对氯化甲苯砜的二甲酰胺溶液,滴加完毕后继续搅拌反应24h,静置沉淀后滤出沉淀,依次以去离子水和无水乙醇洗涤,干燥后溶解在80ml的二甲亚砜中,加入15ml的乙二胺溶液,100℃搅拌反应4h,冷却至室温后加入丙酮析出沉淀,沉淀依次以丙酮和无水乙醇洗涤,干燥后得到氨基改性纤维素,以质量分数1%的醋酸溶液配制为3g/L的溶液,得到氨基改性纤维素溶液;其中,所述对氯化甲苯砜的二甲酰胺溶液中对氯化甲苯砜的质量分数为10%;
b3、配制pH值为8.5的三羟甲基氨基甲烷-盐酸缓冲溶液,以所述缓冲溶液分别配制3g/L的多巴胺溶液和5g/L的端巯基修饰的聚甲基丙烯酸溶液;
b4、将所述熔喷布置于等离子体清洗机中清洗3-5min,在清洗后的熔喷布表面喷涂所述多巴胺溶液,自然晾干后以蒸馏水冲洗,氮气吹干后喷涂氨基纤维素溶液,自然晾干后以蒸馏水冲洗,氮气吹干后喷涂所述端巯基修饰的聚甲基丙烯酸溶液,无氧环境下50℃保温24h,接枝完成后以蒸馏水冲洗,干燥。
2.根据权利要求1所述的一种环保的空气过滤无纺布的生产工艺,其特征在于,所述高分子驻极体为聚碳酸酯、聚甲基丙烯酸甲酯、聚偏氟乙烯中的一种或多种。
3.根据权利要求1所述的一种环保的空气过滤无纺布的生产工艺,其特征在于,所述驻极母粒中,所述聚丙烯、所述少层石墨烯纳米片、所述抗氧化剂、所述相容剂和所述成核剂的重量比例为100:(8-18):(2-5):(1-2):(1-2)。
4.根据权利要求1所述的一种环保的空气过滤无纺布的生产工艺,其特征在于,所述抗氧化剂为四[β-(3,5-二叔丁基-4-羟基苯基)丙酸]季戊四醇酯、β-(3,5-二叔丁基-4-羟基苯基)丙酸正十八碳醇酯或二缩三乙二醇双[β-(3-叔丁基-4-羟基-5-甲基苯基)丙酸酯]。
5.根据权利要求1所述的一种环保的空气过滤无纺布的生产工艺,其特征在于,所述相容剂为马来酸酐接枝聚丙烯、马来酸酐接枝丙烯基弹性体、甲基丙烯酸甲酯接枝聚丙烯、甲基丙烯酸甲酯接枝丙烯基弹性体、甲基丙烯酸缩水甘油酯接枝聚丙烯、甲基丙烯酸缩水甘油酯接枝丙烯基弹性体中的一种或多种。
6.根据权利要求1所述的一种环保的空气过滤无纺布的生产工艺,其特征在于,所述成核剂为硬脂酸盐,所述硬脂酸盐为硬脂酸锂、硬脂酸钠、硬脂酸镁、硬脂酸钙、硬脂酸钡、硬脂酸锌、二硬脂酸铝中的一种或多种。
7.根据权利要求1所述的一种环保的空气过滤无纺布的生产工艺,其特征在于,所述多巴胺溶液的喷涂量为4-5ml/m2,所述氨基纤维素溶液的喷涂量为2-3ml/m2,所述端巯基修饰的聚甲基丙烯酸溶液的喷涂量为5-7ml/m2。
8.一种环保的空气过滤无纺布,其特征在于,由权利要求1-7之一所述环保的空气过滤无纺布的生产工艺制备得到。
9.根据权利要求8所述的一种环保的空气过滤无纺布的应用,其特征在于,用作个人护理、医疗防护、工业气体过滤、发动机气体过滤、洁净室空气过滤、空气净化器、室内新风系统中的空气过滤材料。
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