CN107974672A - 一种基于生物质碳材料的多孔板材孔径调变方法 - Google Patents

一种基于生物质碳材料的多孔板材孔径调变方法 Download PDF

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CN107974672A
CN107974672A CN201711159836.6A CN201711159836A CN107974672A CN 107974672 A CN107974672 A CN 107974672A CN 201711159836 A CN201711159836 A CN 201711159836A CN 107974672 A CN107974672 A CN 107974672A
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李晓锦
韩东锐
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Qingdao Institute of Bioenergy and Bioprocess Technology of CAS
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Abstract

本发明涉及多孔板材，具体的说是一种基于生物质碳材料的多孔板材孔径的调节方法。利用糖溶液填充多孔板材的孔隙，将孔隙中的糖通过升温碳化，从而实现对多孔板孔径的调节。发明原料为糖类和水，来源广泛，成本低廉，处理液对环境无污染，而且操作设备易得，工艺简便易行。

Description

一种基于生物质碳材料的多孔板材孔径调变方法
技术领域
本发明涉及多孔板材，具体的说是一种基于生物质碳材料的多孔板材孔径的调节方法。
背景技术
多孔材料是由基体骨架连续相和气孔分散相或连续相组成的两相复合材料，其性质取决于所用基体材料、气孔率和气孔结构。多孔碳和多孔金属广泛应用于石油化工、航空航天、环境保护等领域，用于制造净化、过滤、催化支架、电极等装置。多孔材料的应用除受其基体本身限制外，更受到其孔径、气孔率和气孔结构的影响，通过后续工艺对多孔材料的孔径、气孔率和孔结构进行调节，可以降低多孔材料制备过程中的参数控制要求，提高多孔材料的适用范围，从而降低制备成本，增加适应性。
CN106450375A通过真空加压的方式将环氧树脂溶液浸渍入多孔石墨板中，将石墨板放入压力为0.5～1MPa的环境下，使环氧树脂浸入石墨板内，待环氧树脂溶液完全固化后，即完成对石墨板的封孔处理。但是该方法需要真空和压力环境，能耗较高。且未对固化后的环氧树脂进行碳化处理，降低了石墨板的导电性能。
中科院大连化学物理研究所采用正硅酸乙酯或钛酸四丁酯水解反应生成SiO2或TiO2纳米颗粒对多孔钛板的孔径进行调节，但是该工艺的反应控制困难，且水解生成的纳米颗粒严重影响了多孔钛板的导电性能。
目前尚无对多孔金属进行孔径调节的专利，相类似的技术可见于CN101736386A、CN106191959A等铝合金阳极氧化后处理工艺专利。但是其封孔剂都是由有机化合物、酸或重金属盐配置而成，成分繁多，配方复杂，对操作人员的身体健康和环境都有危害，而且封孔处理会对多孔金属基体本身造成损伤。
发明内容
本发明的目的在于提供一种基于生物质碳材料的多孔板材孔径的调节方法。
为实现上述目的，本发明采用的技术方案为：
一种基于生物质碳材料的多孔板材孔径的调节方法，利用糖溶液填充多孔板材的孔隙，将孔隙中的糖通过升温碳化，从而实现对多孔板孔径的调节。
进一步的说：
1)将多孔板材在25℃-60℃下浸渍于浓度为30wt％-67wt％的糖溶液中，并不断搅拌；
2)将上述浸渍后多孔板材取出后进行漂洗，而后烘干；
3)将上述获得多孔板材在真空条件下使浸入多孔板材孔中的糖升温碳化实现对多孔板孔径的调节。
所述糖溶液为单糖、二糖或多糖经去离子水溶解所得。优选所述糖为葡萄糖、果糖或蔗糖。
所述多孔板材为多孔碳板、多孔钛板、多孔铝板、多孔不锈钢板，其中，多孔板材的孔径为微米量级。
所述烘干为自然晾干或于烘箱烘干，其中，烘箱烘干为带有加热、鼓风的烘箱中烘干，烘干温度控制在50℃-150℃。
所述真空气氛炉中通入氮气或氩气。
所述碳化中以1℃/min-5℃/min的升温速率升温至300℃-900℃。
在上述工艺方法中，多孔板竖直放置于溶液中，多孔板的放置位置和溶液的运动方向应保证溶液较易进入金属板的孔隙中。提高溶液的浓度和温度，可以增加浸入多孔板孔隙中的糖的量；其中烘干是将浸渍、表面清洗过的多孔板材放入带有加热、鼓风的烘箱中烘干，碳化过程中，在真空气氛炉中应通入气氛保护，碳化终了温度为300℃-900℃，保温时间为0.5h-1h，保温结束后，多孔板材在气氛保护下随炉冷却。
本发明具有如下优点：
(1)用于多孔板材孔径调节的原料为糖类和水，来源广泛，成本低廉，处理液对环境无污染。
(2)通过浸渍和碳化即可实现对多孔板材孔径的可控调节，设备易得，操作工艺简便易行。
(3)浸入多孔板材孔隙中糖类升温碳化后的产物炭是电导体，不会影响多孔板材的导电性能。
附图说明
图1为本发明实施例提供的封孔处理前后的孔容积随孔径变化曲线图。
图2a为本发明实施例提供的封孔处理前的扫描电镜照片。
图2b为本发明实施例提供的封孔处理后的扫描电镜照片。
具体实施方式
下面结合附图进一步通过实施例，对本发明的技术方案作具体的描述。
实施例1
选取厚度为0.8mm的多孔钛板，切取Φ7cm圆片，用去离子水将试片冲洗干净。浸渍前，圆片需在烘箱中烘干水分，设置温度50℃，保温1h。用去离子水配置60wt％的蔗糖(日照市东港区家乐园食品厂)溶液，将圆片竖直放置在溶液中，溶液温度为室温，使用电磁搅拌器缓慢搅拌溶液，浸泡时间为1h。将浸渍完成的试片放置在去离子水中，轻轻摆动，漂清试片表面附着溶液，待表面无黏手感时即从水中取出，自然晾干。将浸渍晾干后的圆片放入真空气氛炉中，氮气氛保护，以5℃/min升温速率升温至400℃的碳化温度，然后在400℃保温1h。保温结束后，试样随炉冷却。通过泡点表征多孔钛板处理前后的孔径变化，多孔钛板处理前后的泡点分别为0.06MPa和0.10MPa。
实施例2
选取厚度为0.8mm的多孔钛板，切取Φ7cm圆片，用去离子水将试片冲洗干净。浸渍前，圆片需在烘箱中烘干水分，设置温度50℃，保温1h。用去离子水配置30wt％的蔗糖(日照市东港区家乐园食品厂)溶液，将圆片竖直放置在溶液中，溶液温度为室温，使用电磁搅拌器缓慢搅拌溶液，浸泡时间为0.5h。将浸渍完成的试片放置在去离子水中，轻轻摆动，漂清试片表面附着溶液，待表面无黏手感时即从水中取出，然后放置到烘箱中，设置温度为70℃，保温1h。将浸渍晾干后的圆片放入真空气氛炉中，氮气氛保护，碳化温度为400℃，以2℃/min升温速率升温至400℃的碳化温度，然后在400℃保温1h。保温结束后，试样随炉冷却。通过泡点表征多孔板材处理前后的孔径变化，多孔钛板处理前后的泡点分别为0.06MPa和0.075MPa。
实施例3
选取厚度为5mm的多孔碳板，切取Φ7cm圆片，用去离子水将试片冲洗干净。浸渍前，圆片需在烘箱中烘干水分，设置温度50℃，保温1h。配置60wt％的蔗糖(日照市东港区家乐园食品厂)溶液，将圆片竖直放置在溶液中，溶液温度为室温，使用电磁搅拌器缓慢搅拌溶液，浸泡时间为0.5h。将浸渍完成的试片放置在去离子水中，轻轻摆动，漂清试片表面附着溶液，待表面无黏手感时即从水中取出，然后放置到烘箱中，设置温度为70℃，保温1h。将浸渍晾干后的圆片放入真空气氛炉中，氮气氛保护，以5℃/min升温速率升温至400℃的碳化温度，然后在400℃保温1h。保温结束后，试样随炉冷却。通过泡点表征多孔板材处理前后的孔径变化，多孔碳板处理前后的泡点分别为0.08MPa和0.11MPa。压汞实验显示，处理前后的中值孔径分别为0.58μm和0.47μm，孔隙率分别为10.4％和8.3％。封孔处理前后的孔容积随孔径变化曲线如图1所示，表明处理后大孔和中孔在整个孔隙中所占比例显著下降，而小孔所占比例显著上升。微观形貌照片如图2所示，由微观照片可以看出，处理后的碳板孔径变小，大孔和中孔的数量降低。

Claims (8)

1.一种基于生物质碳材料的多孔板材孔径的调节方法，其特征在于：利用糖溶液填充多孔板材的孔隙，将孔隙中的糖通过升温碳化，从而实现对多孔板孔径的调节。
2.按权利要求1所述的基于生物质碳材料的多孔板材孔径的调节方法，其特征在于：
1)将多孔板材在25℃-60℃下浸渍于浓度为30wt％-67wt％的糖溶液中，并不断搅拌；
2)将上述浸渍后多孔板材取出后进行漂洗，而后烘干；
3)将上述获得多孔板材在真空条件下使浸入多孔板材孔中的糖升温碳化实现对多孔板孔径的调节。
3.按权利要求1或2基于生物质碳材料的多孔板材孔径的调节方法，其特征在于：所述糖溶液为单糖、二糖或多糖经去离子水溶解所得。
4.按权利要求3所述的基于生物质碳材料的多孔板材孔径的调节方法，其特征在于：所述糖为葡萄糖、果糖或蔗糖。
5.按权利要求3所述的基于生物质碳材料的多孔板材孔径的调节方法，其特征在于：所述多孔板材为多孔碳板、多孔钛板、多孔铝板、多孔不锈钢板，其中，多孔板材的孔径为微米量级。
6.按权利要求2所述的基于生物质碳材料的多孔板材孔径的调节方法，其特征在于：所述烘干为自然晾干或于烘箱烘干，其中，烘箱烘干为带有加热、鼓风的烘箱中烘干，烘干温度控制在50℃-150℃。
7.按权利要求2所述的基于生物质碳材料的多孔板材孔径的调节方法，其特征在于：所述真空气氛炉中通入氮气或氩气。
8.按权利要求2所述的基于生物质碳材料的多孔板材孔径的调节方法，其特征在于：所述碳化中以1℃/min-5℃/min的升温速率升温至300℃-900℃进行碳化。
CN201711159836.6A 2017-11-20 2017-11-20 一种基于生物质碳材料的多孔板材孔径调变方法 Pending CN107974672A (zh)

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