CN111454695A - 一种具有阻燃杀菌功能的双层相变微胶囊材料及制备方法 - Google Patents
一种具有阻燃杀菌功能的双层相变微胶囊材料及制备方法 Download PDFInfo
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Abstract
本发明涉及一种具有阻燃杀菌功能的双层相变微胶囊材料及制备方法，包括膨胀蛭石15‑20份、正十八烷烃8‑15份、四氯化钛30‑50份、盐酸1‑4份、去离子水100‑130份、环氧树脂7‑15份、水性固化剂7‑15份、乳化剂0.3‑1份，并且公开了相变微胶囊的制备方法。本发明的有益效果是：产率高达88％以上；相变潜热高，相变温度为28‑30℃，相变潜热达到233.5Jg‑1；过热温度范围小，仅为1℃。另外该相变微胶囊具有良好的杀菌作用，在太阳光照射条件下能有效杀灭大肠杆菌和淋球菌，并且防火等级达到A级。本发明制备的相变微胶囊可广泛应用于衣物及消防阻燃建筑材料等领域。
Description
技术领域
本发明涉及一种具有阻燃杀菌功能的双层相变微胶囊材料及制备方法，属于功能材料领域。
背景技术
目前已知的相变材料已超过4300多种，可依据不同的分类标准进行分类。常见的分类依据主要有：按物质属性分类、按相变温度分类、按相变形式和相变过程分类。根据物质属性分为无机盐类相变材料、有机小分子相变材料和高分子相变材料；根据相变温度分为低温相变材料、中温相变材料、高温相变材料：根据相变形式和相变过程分为固-固、固-液、气-液、固-气相变材料，常用的是固-固、固-液相变材料。固-液相变材料的研究较早，其理论系统和技术相对成熟，是目前应用最多的一类相变材料。石蜡是由石油工业裂解、精制的产物，由几种直链烷烃组成的混合物，其通式为CnH2n+2。随着碳原子个数的不同，其熔点和相变储热性能也有所不同，可供选择的相变温度和相变储热范围较广。而且其还具有价格低廉、化学性能稳定、几乎不存在过冷和相分离、相变体积小、无毒安全可靠等优点，因此是目前应用最广泛的相变材料之一。高纯度的直链烷烃是石油的精炼产物，比石蜡的相变储热要大得多，是理想的高焓值相变材料，较高的储热能更好地满足低温防护热量的需求。可根据实际使用需求选择相变温度、相变焓值适合的材料，也可两种或几种复配使用。
相变微胶囊由于其不仅可有效解决相变材料泄漏问题延长其使用年限，还可以增加相变材料的有效接触面积。随着微胶囊技术的不断发展，微胶囊化逐渐成为封装相变材料的一种重要技术方法。但是现有的相变微胶囊材料普遍功能单一，只能发挥储能蓄热的作用。
近年来，膨胀蛭石在相变材料领域的应用方兴未艾，已得到了越来越多科研人员的关注，但一般只做为载体进行研究，且文献很少，基于其与相变材料的相容及协同工作的可行性也缺少相关研究。
为了克服现有相变材料的不足，本发明公开了一种以正十八烷为相变材料(核)，二氧化钛为内壳，膨胀蛭石为外壳的相变微胶囊及配方。该方法制备相变微胶囊产率高达88％以上；相变潜热高，相变温度为28-30℃，相变潜热达到233.5Jg-1；过热温度范围小，仅为1℃。另外该相变微胶囊具有良好的杀菌作用，在太阳光照射条件下能有效杀灭大肠杆菌和淋球菌，并且防火等级达到A级。本发明制备的相变微胶囊可广泛应用于衣物及消防阻燃建筑材料等领域。而且本发明创新性地通过实验证明了蛭石也可作为相变微胶囊的包覆层进一步的发挥在此领域的作用，为相变微胶囊提供致密结构的同时，不会影响相变芯材的热力学性能，且由于其具有很好的阻燃性，在有防火保温要求的技术领域具有更加广阔的前景。
发明内容
本发明要解决的技术问题是：基于上述问题，本发明提供一种具有阻燃杀菌功能的双层相变微胶囊材料及制备方法。
本发明解决其技术问题所采用的一个技术方案是：按重量份计，包括膨胀蛭石15-20份、正十八烷烃8-15份、四氯化钛30-50份、盐酸1-4份、去离子水100-130份、环氧树脂7-15份、水性固化剂7-15份、乳化剂0.3-1份。
进一步地，盐酸浓度为15wt％。
进一步地，所述的乳化剂为萘磺酸甲醛缩合物钠盐、烷基酚聚氧乙烯醚甲醛缩合物硫酸盐、聚丙烯酸钠和柠檬酸脂肪酸甘油酯中的一种或几种。
进一步地，膨胀蛭石是由300目的蛭石在1000℃下高温煅烧1小时制得到。
进一步地，所述水性固化剂型号为CU-500，黏度为1000～5000mPa.s(25℃)。
双层相变微胶囊材料是采用界面共聚合方法制备得到的，具体包括以下步骤：
先将蛭石在1000℃下高温煅烧1小时制得膨胀蛭石，放置一旁待用；
再将正十八烷、四氯化钛和盐酸加入容器中混合，通过搅拌实现混合均匀(300转/分)，搅拌40分钟。然后加入去离子水并将溶液温度由室温逐渐提高至100℃(升温速率为10℃﹒min-1)，加入乳化剂，并进行回流，保持反应1小时，实现水解-聚合-包覆过程，此后置于空气中常温熟化12h得到粉末。
进一步地，将水性固化剂与环氧树脂进行质量比1：1配比，搅拌混合均匀，待搅拌30分钟(600转/分)后将上一步骤的粉末加入其中，通过搅拌将环氧树脂均匀涂覆在粉末颗粒表面，持续搅拌2h(900转/分)，再将预处理得到的膨胀蛭石加入其中，通过搅拌40分钟实现混合均匀(600转/分)。并在烘箱中固化1h(70℃)，然后将自然环境降温得到的粉末，经过清洗、干燥得到以膨胀蛭石为外壳，二氧化钛为内壳，正十八烷为核的双层相变微胶囊。
本发明的有益效果是：
(1)本发明中膨胀蛭石作为相变微胶囊外层包覆层，与二氧化钛形成双层致密微胶囊结构，由于内外壁选材的强度较高，整体稳定性更佳，使用寿命更长；(2)膨胀蛭石作为外层包覆层，还能使得相变微胶囊具有高阻燃性，在衣物织品等特定领域方向具有较强应用前景。(3)相变微胶囊产率高达88％以上；(4)相变潜热高，相变温度为28-30℃，相变潜热达到233.5Jg-1；(5)过热温度范围小，仅为1℃；(6)另外该相变微胶囊具有良好的杀菌作用，在太阳光照射条件下能有效杀灭大肠杆菌和淋球菌，并且防火等级达到A级。本发明制备的相变微胶囊可广泛应用于衣物及消防阻燃建筑材料等领域。
附图说明
下面结合附图对本发明进一步说明。
图1为本发明实施例3制备的相变微胶囊的扫描电子显微镜照片。
具体实施方式
现在结合具体实施例对本发明作进一步说明，以下实施例旨在说明本发明而不是对本发明的进一步限定。
实施例1
将蛭石在1000℃下高温煅烧1小时制得膨胀蛭石，放置一旁待用；将8g正十八烷，30g四氯化钛和4g盐酸加入容器中混合，通过搅拌实现混合均匀(300转/分)，搅拌40分钟。然后加入130g去离子水并将溶液温度由室温逐渐提高至100℃(升温速率为10℃min-1)，并进行回流，加入0.3g乳化剂，保持反应1小时，实现水解-聚合-包覆过程，置于空气中常温熟化12h得到粉末。将7g水性固化剂CU-500与7g环氧树脂进行质量比1：1配比，通过搅拌实现混合均匀，搅拌30分钟(600转/分)后将上一步骤得到的粉末加入容器中，再通过搅拌将环氧树脂均匀涂覆在粉末颗粒表面，持续搅拌2h(900转/分)。取第一步得到的15g膨胀蛭石加入容器中，通过搅拌实现混合均匀(600转/分)，搅拌40分钟。并在烘箱中固化1h(70℃)，然后将溶液自然降温得到的粉末，经过过滤、清洗和干燥过程得到以膨胀蛭石为外壳，二氧化钛为内壳，正十八烷为核的双层相变微胶囊。
实施例2
将蛭石在1000℃下高温煅烧1小时制得膨胀蛭石，放置一旁待用；将15g正十八烷，30g四氯化钛和1g盐酸加入容器中混合，通过搅拌实现混合均匀(300转/分)，搅拌40分钟。然后加入100g去离子水并将溶液温度由室温逐渐提高至100℃(升温速率为10℃min-1)，并进行回流，加入1g乳化剂，保持反应1小时，实现水解-聚合-包覆过程，此后置于空气中常温熟化12h得到粉末。将10g水性固化剂CU-500与10g环氧树脂进行质量比1：1配比，通过搅拌实现混合均匀，搅拌30分钟(600转/分)后将上一步骤得到的粉末加入容器中，再通过搅拌将环氧树脂均匀涂覆在粉末颗粒表面，持续搅拌2h(900转/分)。再将第一步得到的20g膨胀蛭石加入容器中，通过搅拌实现混合均匀(600转/分)，搅拌40分钟。并在烘箱中固化1h(70℃)，然后将溶液自然降温得到的粉末，经过过滤、清洗和干燥过程得到以膨胀蛭石为外壳，二氧化钛为内壳，正十八烷为核的双层相变微胶囊。
实施例3
将蛭石在1000℃下高温煅烧1小时制得膨胀蛭石，放置一旁待用；将15g正十八烷，40g四氯化钛和2g盐酸加入容器中混合，通过搅拌实现混合均匀(300转/分)，搅拌40分钟。然后加入110g去离子水并将溶液温度由室温逐渐提高至100℃(升温速率为10℃min-1)，并进行回流，加入0.5g乳化剂，保持反应1小时，实现水解-聚合-包覆等过程，此后置于空气中常温熟化12h得到粉末。将12g水性固化剂CU-500与12g环氧树脂进行质量比1：1配比，通过搅拌实现混合均匀，搅拌30分钟(600转/分)后将上一步骤得到的粉末加入容器中，再通过搅拌将环氧树脂均匀涂覆在粉末颗粒表面，持续搅拌2h(900转/分)。再将第一步得到的20g膨胀蛭石加入容器中，通过搅拌实现混合均匀(600转/分)，搅拌40分钟。并在烘箱中固化1h(70℃)，然后将溶液自然降温得到的粉末，经过过滤、清洗和干燥过程得到以膨胀蛭石为外壳，二氧化钛为内壳，正十八烷为核的双层相变微胶囊。
实施例4
将12g蛭石在1000℃下高温煅烧1小时制得膨胀蛭石，放置一旁待用；将8g正十八烷，50g四氯化钛和1g盐酸加入容器中混合，通过搅拌实现混合均匀(300转/分)，搅拌40分钟。然后加入110g去离子水并将溶液温度由室温逐渐提高至100℃(升温速率为10℃min-1)，并进行回流，加入1g乳化剂，保持反应1小时，实现水解-聚合-包覆等过程，此后置于空气中常温熟化12h得到粉末。将10g水性固化剂CU-500与10g环氧树脂进行质量比1：1配比，通过搅拌实现混合均匀，搅拌30分钟(600转/分)后将上一步骤得到的粉末加入容器中，再通过搅拌将环氧树脂均匀涂覆在粉末颗粒表面，持续搅拌2h(900转/分)。再将第一步得到的20g膨胀蛭石加入容器中，通过搅拌实现混合均匀(600转/分)，搅拌40分钟。然后将溶液自然降温得到的粉末，经过过滤、清洗和干燥过程得到以膨胀蛭石为外壳，二氧化钛为内壳，正十八烷为核的双层相变微胶囊。
对比例1
对比例1与实施例1相比，区别在于，未加入膨胀蛭石为外壳，得到以二氧化钛为外壳，正十八烷为核的相变微胶囊。
上述实施例制得的相变微胶囊的性能测试结果如下表：
且实施例1-4得到的双层相变微胶囊材料的防火等级达到A级，具体参照下列标准GB50222-2017。
产率即相变微胶囊包裹率，通过计算微胶囊中表面相变芯材和总相变芯材的含量来计算并最终得到包裹率。
过热现象特指是由于微胶囊工作环境快速加热过程中，受内部导热速度的影响，到达相变温度时，微胶囊受热不均匀，芯材未发生相变或者只有部分发生相变的情况。实际延迟的相变温度与理论相变温度的差值即为相变微胶囊的过热温度，通过一步求差即可得到。过热温度越小，越说明微胶囊的制作工艺好，受热均匀,若过热温度过高则说明此批微胶囊组分制备不均匀，进而无法得到准确的工作温度，不利于其发挥在微观上的把控作用，因此，过热温度是越低越好。
大肠杆菌存活率、淋球菌存活率的检测方法为：采用牛肉蛋白胨为培养基，分别加入大肠杆菌和淋球菌(将细菌涂布余固体培养基表面)，加入双层相变微胶囊材料，在37℃培养48小时。然后用生理盐水刮洗菌落，倒入无菌小试管中并震荡得到菌悬液。使用细菌计数板在显微镜下直接计数。与不加入双层相变微胶囊材料的菌液为基准，计算存活率。
上表可以看到本发明的相变微胶囊各项性能优异，完全符合国家相关标准，并且节能环保。
以上述依据本发明的理想实施例为启示，通过上述的说明内容，相关工作人员完全可以在不偏离本项发明技术思想的范围内，进行多样的变更以及修改。本项发明的技术性范围并不局限于说明书上的内容，必须要根据权利要求范围来确定其技术性范围。
Claims (6)
1.一种具有阻燃杀菌功能的双层相变微胶囊材料，其特征在于：按重量份计，包括膨胀蛭石15-20份、正十八烷烃8-15份、四氯化钛30-50份、盐酸1-4份、去离子水100-130份、环氧树脂7-15份、水性固化剂7-15份，乳化剂0.3-1份。
2.根据权利要求1所述的一种具有阻燃杀菌功能的双层相变微胶囊材料，其特征在于：盐酸浓度为15wt％。
3.根据权利要求1所述的一种具有阻燃杀菌功能的双层相变微胶囊材料，其特征在于：所述的乳化剂为萘磺酸甲醛缩合物钠盐、烷基酚聚氧乙烯醚甲醛缩合物硫酸盐、聚丙烯酸钠和柠檬酸脂肪酸甘油酯中的一种或几种。
4.根据权利要求1所述的一种具有阻燃杀菌功能的双层相变微胶囊材料，其特征在于：所述水性固化剂型号为CU-500，黏度为1000～5000mPa.s。
5.根据权利要求1所述的一种具有阻燃杀菌功能的双层相变微胶囊材料，其特征在于：膨胀蛭石是由300目蛭石在1000℃下高温煅烧制得。
6.根据权利要求1-5任一项所述的一种具有阻燃杀菌功能的双层相变微胶囊材料的制备方法，其特征在于：具体包括以下步骤：
(1)将正十八烷、四氯化钛和盐酸，通过搅拌实现混合均匀，然后加入去离子水并将溶液温度由室温逐渐提高至100℃，加入乳化剂，并进行回流，保持反应1小时，实现水解-聚合-包覆过程，此后置于空气中常温熟化12h得到粉末；
(2)将水性固化剂与环氧树脂进行质量比1：1配比，通过搅拌实现混合均匀，搅拌后将步骤(1)中得到的粉末加入容器中，通过搅拌将环氧树脂均匀涂覆在粉末颗粒表面，持续搅拌2h；
(3)将膨胀蛭石加入步骤(2)的容器中，通过搅拌将其均匀包覆在浆体颗粒外层，搅拌40分钟，并在烘箱中固化，得到以膨胀蛭石为外壳，二氧化钛为内壳，正十八烷为核的双层相变微胶囊。
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