CN117126446A - 一种原位合成含氧化锌乳液发泡材料的生产方法 - Google Patents
一种原位合成含氧化锌乳液发泡材料的生产方法 Download PDFInfo
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Abstract
本发明属于氧化锌材料技术领域,尤其是一种原位合成含氧化锌乳液发泡材料的生产方法,采用碱式碳酸锌作为原料用原位合成法制备,极大程度上避免额外添加氧化锌填料团聚的弊病,并且不影响发泡性和稳泡性,泡孔结构完整,过程中发挥填料、发泡剂、助硫化剂等多重作用,依靠原位反应,从而在乳液发泡材料内部生成氧化锌填料,具有较低的生产成本,配方简单,工艺简便;氧化锌是在乳液发泡材料生产过程中形成的,采用原位合成法制备出的氧化锌的尺寸也较小,生成氧化锌的同时,又起到发泡剂的作用,均匀分散,避免了粒子团聚,同时分布均匀的同时,气体逸出亦是均匀的,均匀膨胀,形成大小均匀的气孔,适用温度范围广,适用聚合物乳液种类多。
Description
技术领域
本发明属于氧化锌材料技术领域,尤其是一种原位合成含氧化锌乳液发泡材料的生产方法。
背景技术
乳液发泡材料,在立体发泡印花、乳液发泡弹性垫、乳液发泡涂层烟气过滤材料、乳液发泡伪装材料等领域有诸多用途。填料在基体中分散性越好,团聚程度越小,泡孔越小。另外,大量填料的加入势必会使填料发生部分团聚,而团聚部位疏松的结构将会成为发泡剂气体逸出的主要通道,以致最终发泡剂的利用率低下,难以制备出低密度的发泡材料。而填料的额外加入,对乳液发泡材料的泡孔结构影响较大。目前,大多数厂家选择扬汤止沸,舍弃额外添加填料,但发泡材料的强度低,填料赋予的功能无法实现。原位合成法是金属复合材料的制备过程中通过元素之间或化合物之间的化学反应在金属基体中反应生成增强物颗粒。这种方法产生于20世纪80年代,以往原位合成方法几乎只用于金属基复合材料。本发明者自1998年开始氧化锌以及氧化锌填充发泡材料的研究,研究成果已经申请了多项发明专利,并获得授权。其中CN113621164B的专利题为《一种原位合成含氧化锌乳液发泡材料的生产方法》,该原位合成氧化锌乳液发泡材料,采用前驱体碱式碳酸锌乳液,避免了以往添加填充氧化锌造成的粒子团聚,同时分布均匀的氧化锌生成的同时,用于耐高温织物如芳纶、聚苯并咪唑织物、岩碳纤维织物等耐高温纤维表面的发泡处理,或耐高温滤材的表面涂层发泡,其聚合物乳液为聚酰亚胺乳液、聚四氟乙烯乳液,是耐高温聚合物,并不适用于不耐高温的聚合物乳液和滤材,适用范围窄,应用范围受到很大的局限。本领域技术人员为解决上述问题,亟待开发一种原位合成含氧化锌乳液发泡材料的生产方法及其应用以满足现有的市场需求和性能要求。
发明内容
针对上述问题,本发明旨在提供一种原位合成含氧化锌乳液发泡材料的生产方法及其应用。
一种原位合成含氧化锌乳液发泡材料的生产方法,包括以下步骤:
第一步、准备碱式碳酸锌加入到水中,形成碱式碳酸锌糊;第二步、将碱式碳酸锌糊与聚合物乳液混合,并加入过氧化氢溶液,得碱式碳酸锌糊发泡乳液;
碱式碳酸锌与聚合物乳液混合后,加入过氧化氢溶液,反应释放二氧化碳,并形成过氧化锌,初步发泡;
以往过氧化锌作510软膏,起到杀菌收敛,用于皮肤、创面消毒清洗。形成过氧化锌后,经进一步的均匀刮涂形成发泡层或均匀地充填在型腔内或形成发泡涂层,进一步的升温交联,过氧化氢升温分解,原位生成氧化锌的同时,释放氧气,形成发泡作用,并且可以起到交联促进剂的作用;
第三步、将碱式碳酸锌发泡乳液在不锈钢带上均匀刮涂形成发泡层;或将碱式碳酸锌糊发泡乳液加入模具内,使碱式碳酸锌糊发泡乳液均匀地充填在型腔内,得可发料;或将碱式碳酸锌糊发泡乳液采用发泡涂层工艺涂布在连续织物上,形成发泡涂层;第四步、热处理发泡:将上一步得到的发泡层升温交联发泡;将上一步得到的发泡涂层升温交联发泡;将上一步得到的可发料升温交联发泡;发泡后冷却至室温,即得原位合成氧化锌乳液发泡材料。
进一步的,所述碱式碳酸锌糊的质量分数为50%~60%。
进一步的,所述聚合物乳液为天然橡胶乳液、酚醛树脂乳液、聚四氟乙烯乳液的其中一种。
进一步的,碱式碳酸锌糊、聚合物乳液、过氧化氢溶液的质量比为3~5∶1~2∶6~7。
进一步的,所述过氧化氢溶液的质量浓度为33~35%。
进一步的,所不锈钢带上均匀刮涂量400g/m2。
进一步的,所述连续织物为涤纶无纺布或聚酰亚胺无纺布。
进一步的,所述第二步碱式碳酸锌糊发泡乳液的泡沫密度350~550g/L。
进一步的,所述发泡涂层工艺为刮涂量为150~190g/m2,然后在80~90℃下预烘60~120s。
在日常生产实践过程中发现,额外添加到乳液发泡材料中的填料不仅容易团聚,且需要加入额外的分散剂、发泡剂,成分复杂。并且通常情况下,额外加入的粉状的固体填料都有一定的破泡作用,例如重钙等填料,在浆料放置时会出现沉降,使泡沫稳定性降低,大量泡破灭,而木质粉的密度较小并且基本不带电荷,而木质粉纤维等填料,大量分布于液膜表面,改变了液膜的局部张力,因而在干燥过程中,气泡多不完整,影响成型,诸如加入额外加入氧化锌等填料,仍然改变不了上述弊病。
本发明公开的含氧化锌乳液发泡材料的生产方法,采用碱式碳酸锌作为原料,采用原位合成法制备,极大程度上避免额外添加氧化锌填料团聚的弊病,并且不影响乳液发泡材料的发泡性和稳泡性,泡孔结构完整,过程中发挥填料、发泡剂、助硫化剂等多重作用,
依靠原位反应,从而在乳液发泡材料内部生成氧化锌填料,同时具备发泡功能,与额外添加锌白填料相比,原位合成法具有较低的生产成本,材料配方简单,生产工艺简便,氧化锌是在乳液发泡材料生产过程中形成的,采用原位合成法制备出的氧化锌的尺寸也较小,分布的更加均匀。生成氧化锌的同时,又起到发泡剂的作用,均匀分散,避免了以往添加填充氧化锌造成的粒子团聚,同时分布均匀的氧化锌生成的同时,气体的逸出亦是均匀的,乳液均匀膨胀,形成大小均匀的气孔,更好地均一发泡,适用温度范围广,适用聚合物乳液种类多,可用于涤纶无纺布等不耐高温连续织物表面的发泡处理,经烘干、焙烘,图案花纹即发泡变厚,呈现立体状态,或表面涂层发泡,来获得抗菌、光敏降解等性能,以及天然橡胶乳液等不耐高温的聚合物乳液发泡成型。
具体实施方式
下面用具体实施例说明本发明,但并不是对本发明的限制。
实施例1
原料及设备:江苏嘉禾JH830发泡炉、涂布刮刀JLTD20×120×2000、坤泰工业级优等碱式碳酸锌;东至华尔泰工业过氧化氢;固含量62%的海胶天然橡胶乳液,
原位合成含氧化锌乳液发泡材料的生产方法,包括以下步骤:
第一步、准备碱式碳酸锌加入到水中,形成碱式碳酸锌糊,碱式碳酸锌糊的质量分数为50%;第二步、过氧化氢溶液的质量浓度为33%,将碱式碳酸锌糊与天然橡胶乳液混合,并加入过氧化氢溶液,碱式碳酸锌糊、天然橡胶乳液、过氧化氢溶液的质量比为3∶1∶6,得碱式碳酸锌糊发泡乳液,碱式碳酸锌糊发泡乳液的泡沫密度350g/L;第三步、将碱式碳酸锌发泡乳液在不锈钢带上均匀刮涂形成发泡层,不锈钢带上均匀刮涂量400g/m2;第四步、热处理发泡:将上一步得到的发泡层升温交联发泡;发泡后冷却至室温,即得原位合成氧化锌乳液发泡材料。
产品:表观密度413.2kg/m3,压缩永久变形40.2%;拉伸强度20.4kPa;拉断伸长率95.6%;压陷硬度320N;含水率3.0%;压陷比3.0;
注:压缩永久变形测定压缩永久变形测定按GB/T6669-2008中的方法A进行,压缩试样厚度的50%。试验前,试样应在温度为27℃、相对湿度为65%进行16h状态调节。拉伸强度、拉断伸长率的测定拉伸强度和拉断伸长率的测定按GB/T6344-2008中的规定进行。试验前,试样应在温度为27℃、相对湿度为65%进行16h状态调节。老化性能按GB/T9640-2008的规定执行,老化时间为22h,老化温度为100℃。表面硬度的测定按GB/T10807-2006中的方法A进行。试验前,试样应在温度为27℃、相对湿度为65%至少进行16h状态调节。撕裂强度的测定撕裂强度按GB/T10808-2006的规定进行测定。试验前,试样应在温度为27℃、相对湿度为65%至少进行16h状态调节。含水率的测定使用水分测试仪进行水分测试。
实施例2
将实施例1第二步得到的碱式碳酸锌糊发泡乳液采用发泡涂层工艺涂布在江苏江海80g/m2的热轧法点子无纺布TDB-80涤纶无纺布连续织物上,形成发泡涂层,发泡涂层工艺为发泡比为1∶3,刮涂量为150g/m2,然后在80℃下预烘120s;第四步、热处理发泡:将上一步得到的发泡涂层升温150℃交联发泡烘焙5min;发泡后冷却至室温,即得原位合成氧化锌乳液发泡材料涂布的涤纶无纺布。
实施例3
原料及设备:江苏嘉禾JH830发泡炉、涂布刮刀JLTD20×120×2000、坤泰工业级优等碱式碳酸锌;东至华尔泰工业过氧化氢;JF-4DCAF4聚四氟乙烯分散乳液。
原位合成含氧化锌乳液发泡材料的生产方法,包括以下步骤:
第一步、准备碱式碳酸锌加入到水中,形成碱式碳酸锌糊,碱式碳酸锌糊的质量分数为55%;第二步、过氧化氢溶液的质量浓度为34%,将碱式碳酸锌糊与聚四氟乙烯分散乳液混合,并加入过氧化氢溶液,碱式碳酸锌糊、聚四氟乙烯分散乳液、过氧化氢溶液的质量比为4∶2∶7,得碱式碳酸锌糊发泡乳液,碱式碳酸锌糊发泡乳液的泡沫密度350~550g/L;第三步、将碱式碳酸锌糊发泡乳液采用发泡涂层工艺涂布在平均孔径90μm过滤效率42%、过滤阻力43Pa的利通达P84聚酰亚胺无纺布连续织物上,形成发泡涂层,发泡涂层工艺为刮涂量为190g/m2,然后在90℃下预烘60s;第四步、热处理发泡:将上一步得到的发泡涂层升温390℃30min交联发泡;发泡后冷却至室温,即得原位合成氧化锌乳液发泡材料。
得到的PTFE发泡涂层聚酰亚胺无纺布平均孔径76μm、过滤效率63%、过滤阻力44Pa。
实施例4
原料及设备:江苏嘉禾JH830发泡炉、涂布刮刀JLTD20×120×2000、坤泰工业级优等碱式碳酸锌;东至华尔泰工业过氧化氢;吉田803L酚醛树脂乳液。
原位合成含氧化锌乳液发泡材料的生产方法,包括以下步骤:
第一步、准备碱式碳酸锌加入到水中,形成碱式碳酸锌糊,碱式碳酸锌糊的质量分数为60%;第二步、过氧化氢溶液的质量浓度为35%,将碱式碳酸锌糊与酚醛树脂乳液混合,并加入过氧化氢溶液,碱式碳酸锌糊、酚醛树脂乳液、过氧化氢溶液的质量比为5∶2∶7,得碱式碳酸锌糊发泡乳液,碱式碳酸锌糊发泡乳液的泡沫密度550g/L;第三步、使碱式碳酸锌糊发泡乳液均匀地充填在型腔内,得可发料;第四步、热处理发泡:将上一步得到的发泡涂层升温150℃15min交联发泡;发泡后冷却至室温,即得原位合成氧化锌乳液发泡材料。
产品性能:密度72.3kg/m3;压缩强度0.15MPa;导热系数0.035W/m·k;尺寸稳定性1.38%;水蒸气透过系数3.5(Ng/(Pa·m·s));吸水率(体积分数)5.5%;燃烧性能氧指数40%;燃烧分级B1级。
注:密度的测定按GB/T6343规定的方法进行。压缩强度的测定按GB/T8813规定的方法进行。导热系数的测定按GB/T10294的规定进行。尺寸稳定性测定按GB/T8811规定的方法进行。温度70℃,时间48h;尺寸稳定性结果为各个方向尺寸变化率的绝对值的平均值。水蒸气透过系数的测定按QB/T2411-1998规定进行,试样厚度25mm,温度23℃,相对湿度梯度50%,Δp=1404.4Pa,试样数量5个。吸水率的测定按GB/T 8810规定的方法进行。燃烧性能的测定氧指数的测定按 GB/T 2406规定的方法进行。燃烧分级的测定按 GB 8624-2012规定的方法进行。
Claims (9)
1.一种原位合成含氧化锌乳液发泡材料的生产方法,其特征在于,包括以下步骤:
第一步、准备碱式碳酸锌加入到水中,形成碱式碳酸锌糊;第二步、将碱式碳酸锌糊与聚合物乳液混合,并加入过氧化氢溶液,得碱式碳酸锌糊发泡乳液;第三步、将碱式碳酸锌发泡乳液在不锈钢带上均匀刮涂形成发泡层;或将碱式碳酸锌糊发泡乳液加入模具内,使碱式碳酸锌糊发泡乳液均匀地充填在型腔内,得可发料;或将碱式碳酸锌糊发泡乳液采用发泡涂层工艺涂布在连续织物上,形成发泡涂层;第四步、热处理发泡:将上一步得到的发泡层升温交联发泡;将上一步得到的发泡涂层升温交联发泡;将上一步得到的可发料升温交联发泡;发泡后冷却至室温,即得原位合成氧化锌乳液发泡材料。
2.根据权利要求1所述的一种原位合成含氧化锌乳液发泡材料的生产方法,其特征在于,所述碱式碳酸锌糊的质量分数为50%~60%。
3.根据权利要求1所述的一种原位合成含氧化锌乳液发泡材料的生产方法,其特征在于,所述聚合物乳液为天然橡胶乳液、酚醛树脂乳液、聚四氟乙烯乳液中的其中一种。
4.根据权利要求1所述的一种原位合成含氧化锌乳液发泡材料的生产方法,其特征在于,碱式碳酸锌糊、聚合物乳液、过氧化氢溶液的质量比为3~5∶1~2∶6~7。
5.根据权利要求1所述的一种原位合成含氧化锌乳液发泡材料的生产方法,其特征在于,所述过氧化氢溶液的质量浓度为33%~35%。
6.根据权利要求1所述的一种原位合成含氧化锌乳液发泡材料的生产方法,其特征在于,所不锈钢带上均匀刮涂量400g/m2。
7.根据权利要求1所述的一种原位合成含氧化锌乳液发泡材料的生产方法,其特征在于,所述连续织物为涤纶无纺布或聚酰亚胺无纺布。
8.根据权利要求1所述的一种原位合成含氧化锌乳液发泡材料的生产方法,其特征在于,所述第二步碱式碳酸锌糊发泡乳液的泡沫密度350~550g/L。
9.根据权利要求1所述的一种原位合成含氧化锌乳液发泡材料的生产方法,其特征在于,所述发泡涂层工艺为刮涂量为150~190g/m2,然后在80~90℃下预烘60~120s。
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