CN113621164A - 一种原位合成氧化锌乳液发泡材料的制备方法 - Google Patents
一种原位合成氧化锌乳液发泡材料的制备方法 Download PDFInfo
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- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims description 8
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- UOURRHZRLGCVDA-UHFFFAOYSA-D pentazinc;dicarbonate;hexahydroxide Chemical compound [OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[Zn+2].[Zn+2].[Zn+2].[Zn+2].[Zn+2].[O-]C([O-])=O.[O-]C([O-])=O UOURRHZRLGCVDA-UHFFFAOYSA-D 0.000 description 4
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- 239000011667 zinc carbonate Substances 0.000 description 2
- 235000004416 zinc carbonate Nutrition 0.000 description 2
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- AHCZDNYRHNABAH-UHFFFAOYSA-N potassium silver oxido-(oxido(dioxo)chromio)oxy-dioxochromium Chemical compound [K+].[Ag+].[O-][Cr](=O)(=O)O[Cr]([O-])(=O)=O AHCZDNYRHNABAH-UHFFFAOYSA-N 0.000 description 1
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Abstract
本发明属于属于氧化锌材料技术领域，尤其是一种原位合成氧化锌乳液发泡材料的制备方法，碳酸锌能形成良好泡沫结构，与聚合物乳液有良好的相容性，具有易渗入乳液和泡沫破裂产生气体的作用，能在高温下分解，产生气体无毒，同时分解后生成氧化锌，利用原位合成氧化锌乳液发泡材料，生成氧化锌的同时，又起到发泡剂的作用，乳液中分散均匀，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，更好地均一发泡。而且合适较高的分解温度，使聚合物乳液具有良好的成型性能。同时可用于耐高温织物如芳纶、PBI织物、碳纤维织物等耐高温纤维表面的乳液发泡处理，来获得抗菌、光敏降解、耐辐射等性能。
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氧化锌乳液发泡材料的制备方法。
背景技术
以往人们仅是以氧化锌乳液擦在鼻子及脸颊上，将可防止太阳光造成的伤害。软垫主要采用泡沫塑料为基材，常用的有乳液发泡橡胶、聚氨酯发泡塑料以及再生发泡塑料等。乳液发泡橡胶是用天然的橡胶乳液通过发泡工艺制作而成。它可以加工成中间具有铅笔形孔洞的中空形式，使之更加柔软，并具有更好的透气性。它也可以加工成针孔形的片状、块状或所需要的任何形状。聚氨酯发泡塑料是石油化工的附产品，是本世纪四十年代最早的产品。它是将组成物混合在一起产生一种气体，立即使液体膨胀胶化而获得。它可以加工成不同的厚度和不同的形状，可以根据产品不同部位的压力大小和坚柔程度，加工出不同密度的产品类型。再生泡沫塑料或碎料发泡塑料是将现成的发泡塑料切成碎片，在发泡阶段掺入到混合乳液中一起胶化成型。再生泡沫塑料比一般泡沫塑料更密实，更坚硬，并且具有不同的挠度特性。它可以与一般发泡橡胶或泡沫塑料混合使用，或制作软垫的周边，使产品柔中有刚，软硬适中。而以上材料耐腐蚀性能、耐高温性能差，强度较差，本领域技术人员为解决上述问题，亟待开发一种原位合成氧化锌乳液发泡材料的制备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氧化锌乳液发泡材料的制备方法及其应用。
一种原位合成氧化锌乳液发泡材料的制备方法，包括以下步骤：
一、按重量份数计，氧化锌前驱体乳液85~90份分散在85~91份由氨水和氯化铵溶液体积比1∶1组成的混合液中，匀速磁力搅拌10~15min，使之混合均匀，然后慢慢滴加48~56份的聚合物乳液，保持连续的匀速磁力搅拌，得原位合成氧化锌乳液；
二、冷压成型：用20目的筛子过筛原位合成氧化锌乳液后加入敞开的型腔内，升温至100~105℃，静电降沉、抽水至含水量10~15%，然后用刮刀刮平，使树脂均匀地分布在型腔内，加料完毕后应立即进行预压成型，预压成型中需要排气，排气次数1~2次，时间0.5~1min，冷压预压成型的型坯脱模；
冷压预压成型采用原位合成氧化锌乳液静电降沉得到、分布均匀。以往的聚四氟乙烯分散树脂、聚酰亚胺树脂是一种粉末树脂，在贮存或运输过程中，由于受压和震动，容易结块成团，致使冷压时加料发生困难，或者所压制成的型坯密度不均匀，甚至出现开裂现象，而采用乳液混合，使氧化锌前驱体均匀的分散到混合乳液中，并用静电降沉20目的筛子过筛，保证了良好的乳液发泡质量，生产水平得到良好的控制，并实现乳液发泡。
敞开的型腔内，然后用刮刀刮平，使树脂均匀地分布在型腔内。乳液形式，型坯不会发生各次加料的界面上分层或开裂。
预压成型，其中压力过高，树脂颗粒在模内容易相互滑动，以致型坯内部出现裂纹，发泡性能受到影响，压力过低，型坯内部不紧密，密度不高，致使塑料制件的物理和力学性能显著下降。
排气在压制成型过程中，由于型腔中树脂粉末裹入的空气、乳液水份的挥发，不易排出，先一步产生气泡，而在烧结温度规定为380~400℃下，碱式碳酸锌已然分解成纳米氧化锌，具有纳米氧化锌的一般性质，并且原位生成分布均匀不团聚，同时在烧结过程中起到造孔发泡的作用，一举多得。
三、冷压预压成型的型坯脱模从模具中脱出后，放至烧结炉中，进行加热和保温烧结，烧结排气次数1~2次，时间0.5~1h，烧结温度规定为380~400℃，加热速度以30~40℃/h，保温时间为5~10min，后以15~24℃/h的速度缓慢冷却至室温，即得。
冷压成型后的型坯从模具中脱出后，放至烧结炉中在一定温度下进行加热和保温，松散粉粒冷压而成的型坯在烧结过程中熔结成密实的整体。聚四氯乙烯的烧结过程是一个相变过程，当烧结温度超过熔点时，大分子结构中的晶体部分全部转变为无定形结构，这时，物你外观由白色不透明体转变为胶状的弹性透明体。待这一转变过程充分完成后，再经冷却便是塑料制件。合理地控制烧结的全过程-升温、保温和冷却是确保塑件质量的重要因素。烧结温度聚四氟乙烯树脂的熔点是327℃，当温度高于415℃时，就会产生强烈的热分解，因此，型坯的烧结温度必须大于327℃而小于415℃，聚四氟乙烯的烧结温度主要根据树脂的热稳定性以及发泡过程来确定的。升温太快，型坯各部分膨胀不均，易使泡孔产生内应力，甚至出现裂纹，同时升温太快还会产生
保温保温就是将到达烧结温度的型坯在该温度下保持一定的时间使其完全“烧透”的过程。保温时间取决于烧结温度、原材料的热稳定性和泡孔性能。冷却是将已经烧结的型坯从烧结温度降到室温的过程。聚四氟乙烯的冷却同样是一个相变过程，即由非晶相变为晶相的过程。
进一步的，所述聚合物乳液为聚酰亚胺乳液、聚四氟乙烯乳液的其中一种。
进一步的，其特征在于，所述预压成型的压力取10~50MPa，型坯加压速度3~10mm/min，保压时间取3~5min。
进一步的，所述氧化锌前驱体乳液为重量份数计，把50份质量分数11.0%碳酸钠溶液加到25份质量分数40%的ZnSO4·7H2O溶液中，加入25份100℃的沸水混合均匀，即得。
碱式碳酸锌无定形白色微细粉末，无臭、无味，可溶于氨水及铵盐，140℃开始分解，300℃时生成ZnO。
进一步的，所述步骤b的静电降沉为乳液中加1000~1200V的高压直流电时间长达8~10min，电极距离4.0~6mm。
本发明的有益效果：
本发明采用制备方法简便、原料来源广泛的碳酸锌乳液，其既能按要求形成所需要的泡沫结构，与其他活性剂及印花助剂有良好的相容性，具有易渗入织物和促进泡沫及时破裂的作用，能在高温下分解，且产生大量的无毒气体的良好作用，同时分解后生成氧化锌。以往人们仅是以氧化锌乳液擦在鼻子及脸颊上，作防晒霜，将可防止太阳光造成的伤害。本发明利用原位合成氧化锌乳液发泡材料，生成氧化锌的同时，又起到发泡剂的作用，乳液发泡氧化锌的前驱体碱式碳酸锌乳液中分散均匀，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。而且合适较高的分解温度，使乳液具有良好的成型性能。本发明可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，经烘干、焙烘，图案花纹即发泡变厚，呈现立体状态，或耐高温滤材的表面涂层发泡，来获得抗菌、光敏降解等性能。
相比现有技术本发明具有如下优点：
本发明公开的原位合成氧化锌乳液发泡材料的制备方法，具有可设计，绝缘性突出，特别是具有优异的耐高低温、耐辐射、难燃、低发烟，以及无有害气体释放等性能，这些独特的性能是传统泡沫塑料所无法比拟的。由于其尺寸可调的多孔结构和性能良好，具有质轻、阻燃、热稳定、抗辐射、隔热、吸声等优异综合性能，因而在航空、航天、武器装备等领域被广泛用于高性能隔热和吸声材料。
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
首先、重量份数计，把50份质量分数11.0%碳酸钠溶液加到25份质量分数40%的ZnSO4·7H2O溶液中，加入25份100℃的沸水混合均匀，即得氧化锌前驱体乳液，按重量份数计，氧化锌前驱体乳液90份分散在91份由氨水和氯化铵溶液体积比1∶1组成的混合液中，匀速磁力搅拌10min，使之混合均匀，然后慢慢滴加48份的聚四氟乙烯分散乳液，保持连续的匀速磁力搅拌，得原位合成氧化锌乳液；
其次、冷压成型：用20目的筛子过筛原位合成氧化锌乳液后加入敞开的型腔内，升温至105℃，向乳液中加1200 V的高压直流电时间长达10min，电极距离6 mm进行静电降沉、抽水至含水量15%，然后用刮刀刮平，使树脂均匀地分布在型腔内，加料完毕后应立即进行预压成型，预压成型中需要排气，排气次数2次，时间1min，冷压预压成型的型坯脱模，预压成型的压力取50MPa，型坯加压速度10mm/min，保压时间取5min；然后、冷压预压成型的型坯脱模从模具中脱出后，放至烧结炉中，进行加热和保温烧结，烧结排气次数2次，时间1h，烧结温度规定为400℃，加热速度以40℃/h，保温时间为10min，后以24℃/h的速度缓慢冷却至室温，即得。JF-4DCA F4聚四氟乙烯分散乳液。
其中，原位合成氧化锌乳液发泡材料的表观密度为5.0kg/cm3、导热系数0.04W/m·K、拉伸强度0.05MPa、压缩永久变形30%、-55℃12h，不龟裂；300℃12h，表面不发粘，接受辐射累计剂量达到10000Gy后，外观无明显变化。
实施例2
首先、重量份数计，把45份质量分数11.5%碳酸钠溶液加到25份质量分数42%的ZnSO4·7H2O溶液中，加入20份100℃的沸水混合均匀，即得氧化锌前驱体乳液，按重量份数计，氧化锌前驱体乳液85份分散在85份由氨水和氯化铵溶液体积比1∶1组成的混合液中，匀速磁力搅拌10min，使之混合均匀，然后慢慢滴加48份的聚酰亚胺乳液，保持连续的匀速磁力搅拌，得原位合成氧化锌乳液；
其次、冷压成型：用20目的筛子过筛原位合成氧化锌乳液后加入敞开的型腔内，升温至100℃，向乳液中加1000V的高压直流电时间长达8min，电极距离4.0mm进行静电降沉、抽水至含水量10%，然后用刮刀刮平，使树脂均匀地分布在型腔内，加料完毕后应立即进行预压成型，预压成型中需要排气，排气次数1次，时间0.5min，冷压预压成型的型坯脱模；然后、冷压预压成型的型坯脱模从模具中脱出后，放至烧结炉中，进行加热和保温烧结，烧结排气次数1次，时间0.5h，烧结温度规定为380℃，加热速度以30℃/h，保温时间为5min，后以15℃/h的速度缓慢冷却至室温，即得。
聚酰亚胺纳米乳液的制备按比例准确称取UR3800聚酰亚胺溶液100份、DMAc15份和三乙胺，其中三乙胺与DMAc的重量比例在0.35，甲醇与DMAc重量的比值在1.7，在30℃搅拌混合，然后向体系中缓慢加入甲醇继续搅拌混合，以上制得的混合物在25℃恒温水浴中恒温10min，就可制得聚酰亚胺乳液。
其中，原位合成氧化锌乳液发泡材料的表观密度为4.8kg/cm3、导热系数0.05W/m·K、拉伸强度0.09MPa、压缩永久变形28.36%、-55℃24h，不龟裂；300℃12h，表面不发粘，接受辐射累计剂量达到10000Gy后，外观无明显变化。
注：导热系数按GB/T10295-2008绝热材料稳态热阻及有关特性的测定.热流计法规定进行，拉伸强度按照GB/T6344-2008软质泡沫聚合材料.拉伸强度和断裂伸长率的测定规定进行，耐温性按照GB/T9640-2008软质和硬质泡沫聚合材料.加速老化试验方法规定进行；耐辐照按JJF1018-1990使用重铬酸钾(银)剂量计测量γ射线水吸收剂量标准方法规定进行测试，10000Gy剂量，测试20个试样，每个试样尺寸100mm×100mm×25mm。
Claims (5)
1.一种原位合成氧化锌乳液发泡材料的制备方法，其特征在于，包括以下步骤：
a、按重量份数计，氧化锌前驱体乳液85~90份分散在85~91份由氨水和氯化铵溶液体积比1∶1组成的混合液中，匀速磁力搅拌10~15min，使之混合均匀，然后慢慢滴加48~56份的聚合物乳液，保持连续的匀速磁力搅拌，得原位合成氧化锌乳液；
b、冷压成型用20目的筛子过筛原位合成氧化锌乳液后加入敞开的型腔内，升温至100~105℃，静电降沉、抽水至含水量10~15%，然后用刮刀刮平，使树脂均匀地分布在型腔内，加料完毕后应立即进行预压成型，预压成型中需要排气，排气次数1~2次，时间0.5~1min，脱模冷压成型的型坯脱模；c、烧结冷压成型后的型坯从模具中脱出后，放至烧结炉中在一定温度下进行加热和保温，烧结排气次数1~2次，时间0.5~1h，烧结温度规定为380~400℃，加热速度以30~40℃/h，保温时间为5~10min，小以15~24℃/h的速度缓慢冷却至室温，即得。
2.根据权利要求1所述的一种原位合成氧化锌乳液发泡材料的制备方法，其特征在于，所述聚合物乳液为聚酰亚胺乳液、聚四氟乙烯乳液的其中一种。
3.根据权利要求1所述的一种原位合成氧化锌乳液发泡材料的制备方法，其特征在于，所述预压成型的压力取10~50MPa，型坯加压速度3~10mm/min，保压时间取3~5min。
4.根据权利要求1所述的一种原位合成氧化锌乳液发泡材料的制备方法，其特征在于，所述步骤a氧化锌前驱体乳液为重量份数计，把45~50份质量分数11.0~11.5%Na2CO3溶液加到20~25份质量分数40~42%的ZnSO4·7H2O溶液中，加入2份煮沸过的蒸馏水混合均匀，即得。
5.根据权利要求1所述的一种原位合成氧化锌乳液发泡材料的制备方法，其特征在于，所述步骤b的静电降沉为乳液中加1000~1200V的高压直流电时间长达8~10min，电极距离4.0~6mm。
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