CN115431613B - 一种多功能纤维复合天然乳胶制品及其制备方法 - Google Patents
一种多功能纤维复合天然乳胶制品及其制备方法 Download PDFInfo
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- CN115431613B CN115431613B CN202211277288.8A CN202211277288A CN115431613B CN 115431613 B CN115431613 B CN 115431613B CN 202211277288 A CN202211277288 A CN 202211277288A CN 115431613 B CN115431613 B CN 115431613B
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- Prior art keywords
- natural latex
- foaming
- multifunctional fiber
- spinning
- fiber composite
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Classifications
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Abstract
本发明属于功能纤维及复合材料技术领域,公开了一种多功能纤维复合天然乳胶制品及其制备方法。所述制备方法为:将功能纳米粒子与纤维载体经混合纺丝,织造成型,得到多功能纤维材料;将天然乳胶液与硫化剂、表面活性剂和硅橡胶增强粒子搅拌混合均匀,然后通过机械搅拌起泡,得到发泡胶料;将发泡胶料注入到模具中加热硫化,得到天然乳胶发泡材料;以所得多功能纤维材料为面料,天然乳胶发泡材料为填充料,复合制备得到多功能纤维复合天然乳胶制品。本发明方法所得产品能够结合多功能纤维材料的健康保健功能和天然乳胶材料的舒适功能,具有广阔的市场前景。
Description
技术领域
本发明属于功能纤维及复合材料技术领域,具体涉及一种多功能纤维复合天然乳胶制品及其制备方法。
背景技术
近年来,随着人民生活水平迅速提高和健康意识的日益增强,具有高舒适度及健康功能的枕头、床垫之类的床上用品行业正迎来蓬勃的发展。乳胶发泡海绵制品采用纯天然乳胶汁提炼制备而成,自然环保无污染,且本身具有一定的防螨抗菌能力;其蜂窝状设计可达到良好的透气效果,快速散发人体产生的热量;其独特的柔软触觉和乳胶高弹性能够顺应身体轮廓,达到健康安稳舒适的睡眠效果,成为近年来最火爆的寝具内充材质,深受广大消费者的喜爱。但乳胶发泡制品普遍存在发泡不均一,制品内部缺陷等问题,导致强度及耐用性不足的缺陷,同时由于乳胶发泡制品的制造工艺比较单一,对乳胶发泡制品附加健康保健功效的研究较少。
专利CN 106832455 A公开了一种能促进睡眠的乳胶发泡海绵。该乳胶发泡海绵,其原料按照质量份包含以下组分:100份天然胶乳、0.5~3.0份硫化剂、0.5~3.0份起泡剂和0.1~5.0份芳香植物精油微胶囊。该发明的乳胶发泡海绵制成的枕头或床垫,由于包含芳香植物精油微胶囊,能够缓释出芳香植物精油成分,从而能够促进舒缓神经、减轻压力、抚慰情绪以促进睡眠。该专利技术对乳胶发泡进行植物精油功能改性,但未对其发泡、强度及耐用性方面进行研究。专利CN110982131A公开了一种利用低蛋白胶乳生产乳胶发泡制品的方法。所述天然乳胶发泡制品的制备原料,以重量份计,包括胶乳100、硫化剂2~5、起泡剂0.5~6、穏泡剂1~5、胶凝剂0.5~1.5、活性剂3~5、助剂3~12、填料1~15。通过在乳胶发泡制品的生产制备过程中加入了适量的穏泡剂、活性剂,同时改变了生产工艺参数,使得制备的乳胶发泡制品具有很好的泡沫稳定性,泡孔尺寸均一,孔眼结构规整稳定,制品内部缺陷少等,制备所的发泡制品回弹性好,拉伸强度、断裂伸长率、回弹率等均得到显著的提升。但其使用的功能助剂较复杂。
具有健康保健功效的功能纤维材料技术已比较成熟,如具有抗菌、抗病毒、防霉、防螨、远红外、负离子、消臭、除醛、阻燃等健康保健功效的多功能纤维已有较多报道。在我们的前期申请中,也取得了较多的研究成果(CN 2020104460599、CN 2021109694785、CN202111480990X)。目前,采用功能纤维复合乳胶材料制备枕头、床垫、坐垫、等制品的商业化产品较少,具备广阔的市场前景。
发明内容
针对以上现有技术存在的缺点和不足之处,本发明的首要目的在于提供一种多功能纤维复合天然乳胶制品的制备方法。
本发明的另一目的在于提供一种通过上述方法制备得到的多功能纤维复合天然乳胶制品。
本发明目的通过以下技术方案实现:
一种多功能纤维复合天然乳胶制品的制备方法,包括如下制备步骤:
(1)多功能纤维材料制备:
将功能纳米粒子与纤维载体经混合纺丝,织造成型,得到多功能纤维材料;
(2)天然乳胶发泡材料制备:
将天然乳胶液与硫化剂、表面活性剂和硅橡胶增强粒子搅拌混合均匀,然后通过机械搅拌起泡,得到发泡胶料;将发泡胶料注入到模具中加热硫化,得到天然乳胶发泡材料;
(3)复合制品的制备:
以步骤(1)所得多功能纤维材料为面料,步骤(2)所得天然乳胶发泡材料为填充料,复合制备得到多功能纤维复合天然乳胶制品。
进一步地,步骤(1)中所述功能纳米粒子包括石墨烯,负离子粉(如电气石负离子粉、天然蛋白石矿粉等),远红外粉(如蛭石原矿石粉、麦饭石原矿石粉、远红外陶瓷粉等),抗菌防螨粉(银、铜、锌离子或氧化物粉等),除甲醛粉(纳米矿晶、二氧化钛等)、无机纳米除异味粉(氧化锌、二氧化钛、硅藻土等)中的至少一种,或负载中药抗病毒成分的载体粒子,所述负载中药抗病毒成分的载体粒子可以为吸附中药抗病毒成分的二氧化硅气凝胶微球,所述中药抗病毒成分包括艾草、板蓝根、蒲公英、金银花、野菊花、大青叶、穿心莲、黄芩、黄连、黄柏、柴胡、贯众、连翘、虎杖、射干、大黄、鱼腥草、香薷、佩兰、侧柏叶、黄精、五味子、牛蒡子、防风、紫苏、马鞭草、冬凌草、苦参、玄参、白英、地肤子、蛇莓、牛黄、紫草、广陈皮、霍香、薄荷中至少一种中药成分的提取液。上述负载中药抗病毒成分的载体粒子可通过本研究团队前期申请专利所记载的制备方法得到(如CN 2020104982156)。
进一步地,步骤(1)中所述纤维载体包括但不限于聚乳酸、锦纶、涤纶、氨纶、腈纶、粘胶、PP、PE、PET。
进一步地,步骤(1)中所述混合纺丝的方法可通过先制备功能母粒后共混纺丝或直接共混纺丝;所述纺丝的方法不限于熔融纺丝、溶液纺丝、静电纺丝、干法纺丝、湿法纺丝等。
进一步地,步骤(1)中所述多功能纤维材料是指具有抗菌、防螨、抗病毒、消臭、除醛、负离子、远红外中至少一种功能的纤维材料。
进一步地,步骤(2)中所述硫化剂由硫黄、活性剂氧化锌和促进剂PX(乙基苯基二硫代氨基甲酸锌)组成。
进一步优选地,所述硫化剂的用量为天然乳胶液质量的0.8%~4%。
进一步地,步骤(2)中所述表面活性剂为阴离子表面活性剂;优选为脂肪酸盐(如月桂酸钠)、脂肪醇硫酸盐(如十二烷基硫酸钠)或烷基苯磺酸盐(如十二烷基苯磺酸钠)阴离子表面活性剂。
进一步优选地,所述表面活性剂的用量为天然乳胶液质量的0.5%~2%。
进一步地,步骤(2)中所述硅橡胶增强粒子为阳离子改性的硅橡胶增强粒子,其通过如下方法制备得到:
将羟基硅油溶解于有机溶剂中,然后加入气相二氧化硅搅拌分散均匀,在50~80℃温度下加入氨基三甲氧基硅烷进行交联反应,然后加入2,3-环氧丙基三甲基氯化铵进行阳离子化反应,产物经真空干燥脱除有机溶剂,得到阳离子改性的硅橡胶增强粒子。
进一步地,所述羟基硅油为粘度(25℃)为50~500cst的低分子量羟基硅油;所述有机溶剂为异丙醇、苯或甲苯。
进一步地,所述气相二氧化硅的加入量为羟基硅油质量的5%~20%。本发明加入气相二氧化硅起到增强及成核的作用,并控制硅橡胶增强粒子的粒径,使其方便添加至乳胶体系中并达到增强效果。
进一步地,所述氨基三甲氧基硅烷选自氨丙基三甲氧基硅烷、氨乙基氨丙基三甲氧基硅烷、二乙烯三胺基丙基三甲氧基硅烷中的至少一种;氨基三甲氧基硅烷的加入量为羟基硅油质量的3%~12%。氨基三甲氧基硅烷的加入量过低会导致交联程度不够,硅橡胶增强粒子之间产生黏连,无法得到分散性能良好的增强粒子;氨基三甲氧基硅烷的加入量过高会导致成本增加。
进一步地,所述2,3-环氧丙基三甲基氯化铵的加入量为氨基三甲氧基硅烷摩尔量的0.5~1倍。本发明利用氨基三甲氧基硅烷的氨基与2,3-环氧丙基三甲基氯化铵的开环反应进行阳离子化,2,3-环氧丙基三甲基氯化铵的加入量过高会导致过量单体难以除去,加入量过低会导致阳离子化程度不够,所得硅橡胶增强粒子的分散性及与阴离子表面活性剂协同作用的起泡性及稳泡性能降低。
进一步优选地,所述硅橡胶增强粒子的加入量为天然乳胶液质量的2%~6%。
进一步地,所述机械搅拌起泡是指在150~350r/min转速及氮气保护条件下搅拌起泡5~30min。
进一步地,所述加热硫化是指先在60~70℃预硫化1~2h,然后送入100~120℃蒸汽室中深度硫化1~4h。
一种多功能纤维复合天然乳胶制品,通过上述方法制备得到。所述多功能纤维复合天然乳胶制品为枕头、床垫、坐垫等产品。
与现有技术相比,本发明的有益效果是:
(1)本发明将具有健康保健功能的多功能纤维材料与天然乳胶发泡材料进行结合,制备成枕头、床垫、坐垫等产品,能够结合多功能纤维材料的健康保健功能和天然乳胶材料的舒适功能。
(2)本发明天然乳胶材料的制备过程中,通过加入特定的硅橡胶增强粒子,具有良好的分散性及增强性,可以显著增强乳胶材料的力学性能,改善耐用性;同时协同阴离子表面活性剂达到良好的起泡性及稳泡性,提高发泡均匀性及稳定性,降低内部缺陷,提高产品质量。
具体实施方式
下面结合实施例对本发明作进一步详细的描述,但本发明的实施方式不限于此。
实施例1
本实施例的一种多功能纤维复合天然乳胶床垫的制备方法,包括如下制备步骤:
(1)多功能纤维材料制备:
将10重量份石墨烯及抗菌氧化锌纳米粒子与89.5重量份聚酯纤维切片在高速混合机中混合均匀,然后加入0.5重量份热稳定剂季戊四醇硬酯酸酯,再将混合物用双螺杆挤出机挤出得到石墨烯抗菌聚酯母粒。将所得石墨烯抗菌聚酯母粒与聚酯纤维切片混合后进行熔融共混纺丝,得到石墨烯抗菌多功能聚酯纤维。
(2)天然乳胶发泡材料制备:
将100重量份天然乳胶液与2重量份硫化剂(由1重量份硫黄、0.4重量份活性剂氧化锌和0.6重量份促进剂PX组成)、1.2重量份阴离子表面活性剂月桂酸钠和不同重量份硅橡胶增强粒子搅拌混合均匀,然后在200r/min转速及氮气保护条件下搅拌起泡20min,得到发泡胶料;将发泡胶料注入到模具中,先在60~70℃预硫化1h,然后送入105~110℃蒸汽室中深度硫化2h,冷却定型后切片,得到天然乳胶发泡材料。
(3)复合制品的制备:
以步骤(1)所得多功能纤维材料为面料,步骤(2)所得天然乳胶发泡材料为填充料,复合制备得到多功能纤维复合天然乳胶床垫。
本实施例中所用硅橡胶增强粒子为阳离子改性的硅橡胶增强粒子,其通过如下方法制备得到:
按重量份计,将100份粘度(25℃)为120cst的羟基硅油溶解于异丙醇中,然后加入10份气相二氧化硅搅拌分散均匀,将体系加热至65~75℃,加入6份氨乙基氨丙基三甲氧基硅烷进行交联反应1.5h,然后加入氨乙基氨丙基三甲氧基硅烷摩尔量0.8倍的2,3-环氧丙基三甲基氯化铵进行阳离子化反应3h,反应完成后将产物经真空干燥脱除溶剂,得到阳离子改性的硅橡胶增强粒子。
1)为研究不同硅橡胶增强粒子加入量情况下对天然乳胶发泡材料的影响,分别调整硅橡胶增强粒子的加入量为0重量份、1重量份、2重量份、3重量份、4重量份、5重量份、6重量份。测试所得天然乳胶发泡材料的泡孔均匀性(显微镜观察测试切片在一定范围内的泡孔完整性(以完整泡孔占所有泡孔的百分比)及均匀性(目测泡孔的大小均匀度,以优、良、差三个等级标准))、拉伸强度和断裂伸长率(GB/T 528-1998),测试结果如下表1所示。
表1
增强粒子加入量 | 泡孔完整性 | 泡孔均匀性 | 拉伸强度 | 断裂伸长率 |
0 | 62% | 差 | 0.14MPa | 156% |
1% | 78% | 良 | 0.19MPa | 185% |
2% | 92% | 优 | 0.25MPa | 232% |
3% | 94% | 优 | 0.28MPa | 249% |
4% | 97% | 优 | 0.31MPa | 278% |
5% | 98% | 优 | 0.32MPa | 267% |
6% | 98% | 优 | 0.31MPa | 262% |
由表1结果可知,通过在天然乳胶发泡材料中引入硅橡胶增强粒子,可显著增强天然乳胶发泡材料的力学强度。且可以看出,本发明加入阳离子改性的硅橡胶增强粒子对乳胶的发泡性能影响显著,相比不加入阳离子改性的硅橡胶增强粒子的情况下,本发明天然乳胶发泡材料的泡孔完整性及泡孔均匀性均明显改善,在硅橡胶增强粒子的加入量为天然乳胶液质量的2%~6%情况下,所得天然乳胶发泡材料的各项性能均达到较优水平。说明本发明的阳离子改性的硅橡胶增强粒子与阴离子表面活性剂协同作用,通过相反离子的缔合作用和疏水部分的相互作用,能够提高表面活性,达到良好的起泡性及稳泡性,从而显著提高产品质量。
2)为研究不同交联剂加入量对所得硅橡胶增强粒子的影响,分别调整氨乙基氨丙基三甲氧基硅烷的加入量为1重量份、3重量份、5重量份、8重量份、10重量份、12重量份。测试所得硅橡胶增强粒子的形态及粒径,并测试在4%加入量条件下对天然乳胶发泡材料增强效果的影响,结果如下表2所示。
表2
交联剂加入量 | 1% | 3% | 5% | 8% | 10% | 12% |
形态及粒径 | 黏连结团 | 100~900nm | 100~500nm | 40~200nm | 10~100nm | 10~100nm |
拉伸强度 | ---- | 0.26MPa | 0.28MPa | 0.32MPa | 0.32MPa | 0.32MPa |
断裂伸长率 | ---- | 219% | 236% | 281% | 295% | 308% |
由表2结果可见,交联剂加入量过低会导致交联程度不够,硅橡胶增强粒子之间产生黏连结团,分散性能降低,随着交联剂加入量的增加,所得硅橡胶增强粒子的粒径呈现降低的趋势,其在天然乳胶液中的分散性能更优,从而达到更好的增强力学性能的效果。
3)为研究不同阳离子化程度对所得硅橡胶增强粒子及天然乳胶发泡材料性能的影响,分别调整2,3-环氧丙基三甲基氯化铵的加入量为氨乙基氨丙基三甲氧基硅烷摩尔量的0倍、0.3倍、0.5倍、0.6倍、0.7倍、0.9倍、1.0倍,测试所得硅橡胶增强粒子的粒径,并测试在4%加入量条件下对天然乳胶发泡材料增强效果的影响,结果如下表3所示。
表3
由表3结果可知,阳离子化程度对所得硅橡胶增强粒子的粒径影响显著,其原因可能在于阳离子化程度越高,硅橡胶增强粒子在制备成核过程中的静电斥力越大,粒子间的黏连结团程度降低,从而使得粒径降低;同时其阳离子化程度越高,与阴离子表面活性剂的缔合作用越强,显著促进胶束在硅橡胶增强粒子表面形成,产生更高的表面活性,并最终改善其在天然乳胶液中的分散性能和达到更好的增强力学性能的效果。另外由发泡性能结果可知,发泡均匀性及稳定性的提高主要在于阳离子化,相比未阳离子化的硅橡胶增强粒子,本发明所得天然乳胶发泡材料的发泡均匀性及稳定性显著改善,且随着阳离子化程度的提高,这种改善效果越显著,说明本发明阳离子改性的硅橡胶增强粒子在阴离子表面活性剂作为发泡剂的情况下,通过相反离子的缔合作用和疏水部分的相互作用,能够提高表面活性,具有显著提高发泡均匀性及稳定性的技术效果。
实施例2
本实施例的一种多功能纤维复合天然乳胶枕的制备方法,包括如下制备步骤:
(1)多功能纤维材料制备:
将4重量份远红外陶瓷粉、4重量份纳米氧化银抗菌粒子及4重量份中药抗病毒纳米粒子(吸附有艾草、板蓝根、蒲公英、金银花、野菊花、大青叶、霍香、薄荷提取物的二氧化硅气凝胶微球)与88重量份聚酯纤维切片在高速混合机中混合均匀,然后加入0.5重量份热稳定剂季戊四醇硬酯酸酯,再将混合物用双螺杆挤出机挤出得到远红外抗病毒抗菌聚酯母粒。将所得远红外抗病毒抗菌聚酯母粒与聚酯纤维切片混合后进行熔融共混纺丝,得到远红外抗病毒抗菌多功能聚酯纤维。
(2)天然乳胶发泡材料制备:
将100重量份天然乳胶液与3重量份硫化剂(由1.6重量份硫黄、0.6重量份活性剂氧化锌和0.8重量份促进剂PX组成)、1.5重量份阴离子表面活性剂十二烷基苯磺酸钠和4重量份硅橡胶增强粒子搅拌混合均匀,然后在300r/min转速及氮气保护条件下搅拌起泡15min,得到发泡胶料;将发泡胶料注入到模具中,先在60~70℃预硫化1h,然后送入95~100℃蒸汽室中深度硫化2h,冷却定型后切片,得到天然乳胶发泡材料。
(3)复合制品的制备:
以步骤(1)所得多功能纤维材料为面料,步骤(2)所得天然乳胶发泡材料为填充料,复合制备得到多功能纤维复合天然乳胶枕。
本实施例中所用硅橡胶增强粒子为阳离子改性的硅橡胶增强粒子,其通过如下方法制备得到:
按重量份计,将100份粘度(25℃)为350cst的羟基硅油溶解于甲苯中,然后加入15份气相二氧化硅搅拌分散均匀,将体系加热至65~75℃,加入10份氨丙基三甲氧基硅烷进行交联反应2h,然后加入氨乙基氨丙基三甲氧基硅烷摩尔量0.6倍的2,3-环氧丙基三甲基氯化铵进行阳离子化反应3h,反应完成后将产物经真空干燥脱除溶剂,得到阳离子改性的硅橡胶增强粒子。
本实施例所得天然乳胶发泡材料经测定泡孔完整性为97%,泡孔均匀性优,拉伸强度为0.30MPa,断裂伸长率为254%。
上述实施例为本发明较佳的实施方式,但本发明的实施方式并不受上述实施例的限制,其它的任何未背离本发明的精神实质与原理下所作的改变、修饰、替代、组合、简化,均应为等效的置换方式,都包含在本发明的保护范围之内。
Claims (7)
1.一种多功能纤维复合天然乳胶制品的制备方法,其特征在于,包括如下制备步骤:
(1)多功能纤维材料制备:
将功能纳米粒子与纤维载体经混合纺丝,织造成型,得到多功能纤维材料;
(2)天然乳胶发泡材料制备:
将天然乳胶液与硫化剂、表面活性剂和硅橡胶增强粒子搅拌混合均匀,然后通过机械搅拌起泡,得到发泡胶料;将发泡胶料注入到模具中加热硫化,得到天然乳胶发泡材料;
(3)复合制品的制备:
以步骤(1)所得多功能纤维材料为面料,步骤(2)所得天然乳胶发泡材料为填充料,复合制备得到多功能纤维复合天然乳胶制品;
步骤(2)中所述表面活性剂为脂肪酸盐、脂肪醇硫酸盐或烷基苯磺酸盐阴离子表面活性剂;所述硅橡胶增强粒子为阳离子改性的硅橡胶增强粒子,其通过如下方法制备得到:
将羟基硅油溶解于有机溶剂中,然后加入气相二氧化硅搅拌分散均匀,在50~80℃温度下加入氨基三甲氧基硅烷进行交联反应,然后加入2,3-环氧丙基三甲基氯化铵进行阳离子化反应,产物经真空干燥脱除有机溶剂,得到阳离子改性的硅橡胶增强粒子;
所述氨基三甲氧基硅烷的加入量为羟基硅油质量的3%~12%;所述2,3-环氧丙基三甲基氯化铵的加入量为氨基三甲氧基硅烷摩尔量的0.5~1倍;
所述硅橡胶增强粒子的加入量为天然乳胶液质量的2%~6%。
2.根据权利要求1所述的一种多功能纤维复合天然乳胶制品的制备方法,其特征在于,步骤(1)中所述功能纳米粒子包括石墨烯,负离子粉,远红外粉,抗菌防螨粉,除甲醛粉、除异味粉中的至少一种,或负载中药抗病毒成分的载体粒子;所述纤维载体为聚乳酸、锦纶、涤纶、氨纶、腈纶、粘胶、PP、PE或PET;所述混合纺丝的方法为先制备功能母粒后共混纺丝或直接共混纺丝;所述纺丝的方法为熔融纺丝、溶液纺丝、静电纺丝、干法纺丝或湿法纺丝;所述多功能纤维材料是指具有抗菌、防螨、抗病毒、消臭、除醛、负离子、远红外中至少一种功能的纤维材料。
3.根据权利要求1所述的一种多功能纤维复合天然乳胶制品的制备方法,其特征在于,步骤(2)中所述硫化剂由硫黄、活性剂氧化锌和促进剂PX组成;硫化剂的用量为天然乳胶液质量的0.8%~4%;所述表面活性剂的用量为天然乳胶液质量的0.5%~2%。
4.根据权利要求1所述的一种多功能纤维复合天然乳胶制品的制备方法,其特征在于,所述羟基硅油为粘度为50~500 cst的低分子量羟基硅油;所述有机溶剂为异丙醇、苯或甲苯;所述气相二氧化硅的加入量为羟基硅油质量的5%~20%。
5.根据权利要求1所述的一种多功能纤维复合天然乳胶制品的制备方法,其特征在于,所述氨基三甲氧基硅烷选自氨丙基三甲氧基硅烷、氨乙基氨丙基三甲氧基硅烷、二乙烯三胺基丙基三甲氧基硅烷中的至少一种。
6.根据权利要求1所述的一种多功能纤维复合天然乳胶制品的制备方法,其特征在于,所述机械搅拌起泡是指在150~350r/min转速及氮气保护条件下搅拌起泡5~30min;所述加热硫化是指先在60~70℃预硫化1~2h,然后送入100~120℃蒸汽室中深度硫化1~4h。
7.一种多功能纤维复合天然乳胶制品,其特征在于,通过权利要求1~6任一项所述的方法制备得到,所述多功能纤维复合天然乳胶制品为枕头、床垫、坐垫产品。
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