CN107855107B - 溶胶-微波一步法制备炭担载铝硅酸钠复合材料的方法 - Google Patents
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Abstract
溶胶‑微波一步法制备炭担载铝硅酸钠复合材料的方法，属于复合材料制备技术领域。将干燥稻壳与氢氧化铝溶胶进行充分的混合得到表面粘附氢氧化铝溶胶的稻壳，再将氢氧化铝溶胶负载的稻壳和适量的活性炭一并放入微波炉中加热处理，通过原位化合反应，析出铝硅酸钠纳米颗粒；同时稻壳中的有机物炭化成炭，析出的铝硅酸钠纳米颗粒负载于炭基体之上，从而获得炭担载铝硅酸钠复合材料。制备的炭担载铝硅酸钠复合材料，其宏观形态为稻壳状，呈黑色；微观形态为无数球形的铝硅酸钠颗粒无规则分布在炭基体的表面。兼具有炭和铝硅酸钠分子筛优点，可望用于工业催化剂和吸附剂等领域。
Description
技术领域
本发明涉及一种溶胶-微波一步法制备炭担载铝硅酸钠复合材料的方法，属于复合材料制备技术领域。
背景技术
稻壳是稻米加工过程中数量最大的副产品。稻壳的组成中75％为有机物，25％为二氧化硅。我国是一个产粮大国，每年的稻壳产量约为数千万吨。长期以来国内外对稻壳的综合利用进行了广泛的研究，获得了许多可供利用的途径。目前，稻壳的综合利用方面很多，如焚烧取热，作为饲料、压制成稻壳板、制备水玻璃、白炭黑以及活性炭等。
但是，真正能够形成宏量生产的，能大量消耗稻壳的利用途径并不多，或是经济效益不显著、增值不大；或是在工艺上、技术上、质量上、环境污染等方面还存在一些问题。因此，许多地方把稻壳作为废弃物，这不仅是对资源的极大浪费，在经济上造成巨大损失，而且对环境也造成了很大污染。研究解决稻壳的合理利用，变废为宝，是摆在我们面前的一项意义重大的任务。如果采用一般的方法进行焚烧，即产生炭化，但作为吸附材料的价值不大，只能用于改良土壤。
有关通过稻壳制备炭担载铝硅酸钠复合材料至今尚未见文献报道。
发明内容
本发明针对现有技术中所存在的不足之处，提供一种工艺简单、安全可靠、成本低廉适合连续规模化生产的溶胶-微波一步法制备炭担载铝硅酸钠复合材料的方法。
为了实现上述目的，本发明所采用的技术方案为：一种溶胶-微波一步法制备炭担载铝硅酸钠复合材料的方法，将干燥稻壳与氢氧化铝溶胶进行充分的混合得到表面粘附氢氧化铝溶胶的稻壳，再将氢氧化铝溶胶负载的稻壳和适量的活性炭一并放入微波炉中加热处理，通过原位化合反应，析出铝硅酸钠纳米颗粒；同时稻壳中的有机物炭化成炭，析出的铝硅酸钠纳米颗粒负载于炭基体之上，从而获得炭担载铝硅酸钠复合材料。
作为本发明制备方法的优选技术方案，具体包括如下步骤：
1)、将硫酸铝和氢氧化钠固体分别加入盛有适量去离子水的两个烧杯中，超声使其完全溶解得到溶液A和B，将溶液A和B混合，搅拌得到氢氧化铝溶胶C；
2)、将氢氧化铝溶胶与适量的稻壳混合，并通过搅拌改善氢氧化铝溶胶与稻壳表面粘附状况，从而获得氢氧化铝溶胶/稻壳复合前驱体；
3)、将获得的氢氧化铝溶胶/稻壳复合前驱体和适量的活性炭一起放置于微波炉中进行微波加热反应，得到炭担载铝硅酸钠复合材料。
作为本发明制备方法的进一步优选技术方案，步骤2)中氢氧化铝溶胶与稻壳按照质量比为0.5～5：5～100混合。步骤3)中微波反应时间为10～60min，微波功率为中火～高火。步骤3)中用于引发微波强吸收作用的活性炭与氢氧化铝溶胶/稻壳复合前驱体的质量比为0.1～1：5～100。
本发明提供一种溶胶-微波一步法制备炭担载铝硅酸钠复合材料的方法，即将一定量洁净的干燥稻壳与新配置的氢氧化铝溶胶进行充分的混合，得到表面粘附氢氧化铝溶胶的稻壳；再将一定量的氢氧化铝溶胶负载的稻壳和适量的活性炭一并放入微波炉中加热处理若干时间后，获得炭担载铝硅酸钠复合材料。通过一系列的表征表明，制备的复合材料是由炭担载铝硅酸钠纳米颗粒构成，两者结合状况良好。
与现有技术相比，本发明具有以下优点：
1)、制备的炭担载铝硅酸钠复合材料，其宏观形态为稻壳状，呈黑色；微观形态为无数球形的铝硅酸钠颗粒无规则分布在炭基体的表面，铝硅酸钠纳米颗粒的平均粒径为0.5～24μm，炭颗粒的尺寸为400～2000μm。
2)、制备方法具有原理简单、操作方便、所需设备简单、制备效率高和安全可靠等优点，可用于宏量制备。同时，从新的角度解决了稻壳的综合利用问题。
3)、制备的炭担载铝硅酸钠复合材料具有多孔结构和形态，兼具有炭和铝硅酸钠分子筛优点，可望用于工业催化剂和吸附剂等领域。
附图说明
图1为本发明的制备方法流程图。
图2为实施例1制备的复合材料的XRD谱图。
图3为实施例1制备的复合材料的FE-SEM图(低倍率)。
图4为实施例1制备的复合材料的FE-SEM图(高倍率)。
具体实施方式
下面结合附图和具体实施例对本发明进行详细说明。
本发明方法所得复合材料的结构、形貌和组成分别选用X射线粉末衍射(XRD)和场发射扫描电子显微镜(FE-SEM)进行表征。
本发明一种溶胶-微波一步法制备炭担载铝硅酸钠复合材料的方法，其工艺流程如图1所示，整个过程无需经历洗涤和干燥等操作，制备原理简单，因此可以用于宏量制备。具体是：将一定量洁净的干燥稻壳与新配置的氢氧化铝溶解进行充分的混合，得到表面粘附氢氧化铝溶胶的稻壳；再将一定量的氢氧化铝溶胶负载的稻壳和适量的活性炭一并放入微波炉中加热处理；反应若干时间后，即可获得了炭担载铝硅酸钠复合材料。
本发明的反应原理如下：
首先，在微波反应条件下，粘附或浸入到稻壳表层的Al(OH)3将与稻壳中的SiO2进行化合反应形成NaAlSi3O8纳米颗粒(见反应式1)；稻壳在脱硅、炭化后形成了炭骨架(见示意式2)。
反应后NaAlSi3O8纳米颗粒嵌入在炭基体的表面，从而形成了炭担载铝硅酸钠纳米复合材料(见示意式3)。
实施例1
溶胶-微波一步法制备炭担载铝硅酸钠复合材料的方法，包括如下步骤：
1)、将硫酸铝和氢氧化钠固体分别加入盛有适量去离子水的两个烧杯中，超声使其完全溶解得到溶液A和B，将溶液A和B混合，搅拌得到氢氧化铝溶胶C；
2)、将氢氧化铝溶胶与稻壳按照质量比为0.5：100混合，并通过搅拌改善氢氧化铝溶胶与稻壳表面粘附状况，从而获得氢氧化铝溶胶/稻壳复合前驱体；
3)、将获得的氢氧化铝溶胶/稻壳复合前驱体和活性炭(引发微波强吸收作用)按照质量比为50：0.1混合，一起放置于微波炉中进行微波加热反应，微波反应时间为10min，微波功率为中火～高火，得到炭担载铝硅酸钠复合材料。
图1为实施例1制备的复合材料工艺流程图，由图1可看最终产物颜色为黑色，宏观上呈颗粒状。
图2为实施例1制备的复合材料的XRD谱图。与NaAlSi3O8标准XRD谱图(PDF#19-1184)比较后可知，除了炭外，复合材料中还存在NaAlSi3O8物相。
图3和4为实施例1制备的复合材料的FE-SEM图，由图可以看出，制备出的复合材料结构中，炭基体表面分布着若干球形颗粒，即为NaAlSi3O8纳米颗粒，铝硅酸钠纳米颗粒的平均粒径为0.5～24μm，炭颗粒的尺寸为400～2000μm。
实施例2
溶胶-微波一步法制备炭担载铝硅酸钠复合材料的方法，包括如下步骤：
1)、将硫酸铝和氢氧化钠固体分别加入盛有适量去离子水的两个烧杯中，超声使其完全溶解得到溶液A和B，将溶液A和B混合，搅拌得到氢氧化铝溶胶C；
2)、将氢氧化铝溶胶与稻壳按照质量比为5：5混合，并通过搅拌改善氢氧化铝溶胶与稻壳表面粘附状况，从而获得氢氧化铝溶胶/稻壳复合前驱体；
3)、将获得的氢氧化铝溶胶/稻壳复合前驱体和活性炭(引发微波强吸收作用)按照质量比为100：1混合，一起放置于微波炉中进行微波加热反应，微波反应时间为60min，微波功率为中火～高火，得到炭担载铝硅酸钠复合材料。
实施例3
溶胶-微波一步法制备炭担载铝硅酸钠复合材料的方法，包括如下步骤：
1)、将硫酸铝和氢氧化钠固体分别加入盛有适量去离子水的两个烧杯中，超声使其完全溶解得到溶液A和B，将溶液A和B混合，搅拌得到氢氧化铝溶胶C；
2)、将氢氧化铝溶胶与稻壳按照质量比为2.5：50混合，并通过搅拌改善氢氧化铝溶胶与稻壳表面粘附状况，从而获得氢氧化铝溶胶/稻壳复合前驱体；
3)、将获得的氢氧化铝溶胶/稻壳复合前驱体和活性炭(引发微波强吸收作用)按照质量比为5：0.5混合，一起放置于微波炉中进行微波加热反应，微波反应时间为40min，微波功率为中火～高火，得到炭担载铝硅酸钠复合材料。
以上内容仅仅是对本发明的构思所作的举例和说明，所属本技术领域的技术人员对所描述的具体实施例做各种各样的修改或补充或采用类似的方式替代，只要不偏离发明的构思或者超越本权利要求书所定义的范围，均应属于本发明的保护范围。
Claims (6)
1.溶胶-微波一步法制备炭担载铝硅酸钠复合材料的方法，其特征在于，将干燥稻壳与氢氧化铝溶胶进行充分的混合得到表面粘附氢氧化铝溶胶的稻壳，再将氢氧化铝溶胶负载的稻壳和适量的活性炭一并放入微波炉中加热处理，通过原位化合反应，析出铝硅酸钠颗粒；同时稻壳中的有机物炭化成炭，析出的铝硅酸钠颗粒负载于炭基体之上，从而获得炭担载铝硅酸钠复合材料，具体包括如下步骤：
1）、将硫酸铝和氢氧化钠固体分别加入盛有适量去离子水的两个烧杯中，超声使其完全溶解得到溶液A和B，将溶液A和B混合，搅拌得到氢氧化铝溶胶C；
2）、将氢氧化铝溶胶与适量的稻壳混合，并通过搅拌改善氢氧化铝溶胶与稻壳表面粘附状况，从而获得氢氧化铝溶胶/稻壳复合前驱体；
3）、将获得的氢氧化铝溶胶/稻壳复合前驱体和适量的活性炭一起放置于微波炉中进行微波加热反应，得到炭担载铝硅酸钠复合材料。
2.如权利要求1所述的制备方法，其特征在于，步骤2）中氢氧化铝溶胶与稻壳按照质量比为0.5~5：5~100混合。
3.如权利要求1所述的制备方法，其特征在于，步骤3）中微波反应时间为10~60 min。
4.如权利要求1所述的制备方法，其特征在于，步骤3）中微波功率为中火~高火。
5.如权利要求1所述的制备方法，其特征在于，步骤3）中用于引发微波强吸收作用的活性炭与氢氧化铝溶胶/稻壳复合前驱体的质量比为0.1~1：5~100。
6.一种如权利要求1~5任一项所述方法制备的炭担载铝硅酸钠复合材料，其特征在于，产物宏观形态为稻壳状，呈黑色；产物微观形态为若干球形的铝硅酸钠颗粒无规则分布在炭基体的表面，铝硅酸钠颗粒的平均粒径为0.5~24 μm，炭颗粒的尺寸为400~2000μm。
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