CN109553416A - 一种泡沫碳的制备方法 - Google Patents

一种泡沫碳的制备方法 Download PDF

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CN109553416A
CN109553416A CN201811537885.3A CN201811537885A CN109553416A CN 109553416 A CN109553416 A CN 109553416A CN 201811537885 A CN201811537885 A CN 201811537885A CN 109553416 A CN109553416 A CN 109553416A
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dough
carbon
pore creating
creating material
preparation
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穆松林
穆欣颦
杜军
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South China University of Technology SCUT
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South China University of Technology SCUT
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Abstract

本发明公开了一种用于制备泡沫碳的制备方法，该方法包括以下步骤：包括以下步骤：制作面团、发泡定型、预处理、碳化烧结，制得所述泡沫碳。更高要求时，可在保护气氛下，进行石墨化处理，制得石墨化的泡沫碳。本发明所述方法的碳源为面粉、玉米粉等可再生资源，廉价易得，发明工艺简单安全、成本低廉、易于实现产业化。

Description

一种泡沫碳的制备方法
技术领域
本发明属于泡沫碳制备，具体涉及一种以面粉、玉米粉、糯米粉、米粉的一种或多种的混合物为碳源的泡沫碳的制备方法。
背景技术
泡沫碳是一种新型碳质材料，是一种以碳元素为主要组成的三维网状轻质多孔材料。泡沫碳是一种性能优异，用途广泛的新型材料。具有密度低、耐高温、耐腐蚀、耐酸碱、吸水率低、隔热好、具有导电性，此外，通过掺杂或表面处理后还可具有特殊功能，如催化，选择性吸附等特性。这些优异的性能使泡沫碳在热交换器、催化剂载体、电子器件、食品、制药、石油化工、交通运输以及航空航天等许多民用和军用领域具有广阔的应用前景。近几年受到国内外学者和研究人员的高度关注，当前相关研究主要集中在废水及废气的吸附材料、催化剂载体、超级电容器的电极材料、绝热材料、热能储存器、吸波材料等领域。
依据石墨化程度不同，泡沫碳可分为非石墨化泡沫碳和石墨化泡沫碳。从泡沫碳材料的制备方法上看，主要有常规发泡法、模板法、超临界法等，存在操作复杂或工艺条件苛刻的问题。目前，泡沫碳材料的制备原料以非生物质原料为主，如沥青、树脂和煤等化合物。CN200710163858.X申请保护“一种高导热泡沫碳材料的制备方法”，需要将聚氧化乙烯、聚乙烯醇或聚甲基纤维素与蒸馏水混合搅拌4-10小时制备分散剂；中间相沥青粉碎过筛，与添加物共混球磨1-2小时，然后烘干1-2小时，得到掺杂后的中间相沥青原料；制备时需氮气保护，需要外压作用，450-500℃恒温2-3小时，冷却至室温制得沥青泡沫体；再在氮气保护下，升温至800-1000℃，恒温1-2小时，自然冷却至室温，制得泡沫碳；该技术工序多，耗时长。CN201611014928.0公开了“光催化降解甲醛功能泡沫碳的制备方法”以聚氨酯和活性碳为原料经热处理制得聚氨酯泡沫碳，然后担载TiO2制得具有光催化活性的功能泡沫碳。工艺使用到聚醚、硬泡硅油、水、五甲基二乙烯三胺AM-1、二氯一氟乙烷、环乙胺、二苯基甲烷、二异氰酸酯MDI，涉及化工原料多，步骤繁琐。CN201010161966.5公开了“一种用呋喃树脂制备泡沫碳的方法”，采用了呋喃树脂，其发泡碳化过程耗时至少需要38小时，耗时太长。CN201310527246.X申请并获得授权的专利技术“一种混合基泡沫碳材料的制备方法”，采用煤粉和酚醛树脂混合制备泡沫碳。除沥青、树脂、煤三大类碳源外，也有一些其他碳源的工艺。专利CN201410523690.9保护“一种纳米级壁厚的薄壁泡沫炭材料及其制备方法”，利用酸液对玉米淀粉的点蚀水解和脱水作用，在微波条件下使淀粉快速发泡炭化，形成纳米级壁厚的薄壁泡沫炭材料，涉及步骤较多。CN201610943820.3申请保护“一种基于废弃生物质泡沫炭材料的制备方法”，工序涉及废弃物预处理、液化处理、树脂化处理、泡沫化处理、还有活化和碳化处理，步骤较多，而采用废弃物则意味着原料成分不稳定。
由上可知，目前国内报道的工艺，大多碳源为不可再生资源，或者碳源不稳定。而且从制备工艺来看，需在较高的温度和压力(600℃左右，7-10MPa)下发泡。至今，我国还未实现泡沫碳的产业化，其根本原因在于：1)现有的工艺涉及步骤较多，工序繁琐，不利于实现产业化；2)主要工艺以沥青、树脂、煤等为原料，一方面这些都是化石能源或其衍生产品，具有不可再生的特性；另一方面其价格受石油供给量影响很大，企业风险较大；3)所需的设备较多，导致前期投入大、生产成本高，阻碍了技术的产业化；4)除原料外，生产中还涉及不少化工原料，有些为挥发性大，易燃易爆化工产品，此外，大多工艺中涉及加压条件，安全隐患较大也是阻碍技术产业化的一大障碍。
综上，基于资源丰富且可再生的生物质资源为原料，利用简单的工艺路线制备综合性能优异且稳定的泡沫碳材料已经成为该领域的研究热点。
发明内容
本发明的目的在于针对现有技术的不足，提供一种制备泡沫碳的方法，采用价格低廉、来源广泛的面粉、玉米粉、糯米粉、米粉或任意组合的混合物做为碳源，成本低廉，简单易行的泡沫碳制备方法；所述制备方法涉及的工序简单易操作，对设备要求不高，简单易行，具有良好的产业化前景。
本发明的目的通过以下技术方案实现。
本发明所述的泡沫碳的制备方法，其工艺包含如下步骤：
(1)制作面团：造孔剂均匀分散在水中，将碳源粉体加入含造孔剂的水中，搅拌成面团；
(2)发泡定型：将面团压制成型，然后放入加热炉中，升温至90-120℃，保温20-40min，使面团发泡定型；
(3)预处理：将炉温升至180-350℃，对定型的面团进行预处理，处理时间10-120min，排出面团中水分；
(4)碳化烧结：将步骤(3)预处理后的面团移入高温炉，在真空条件、氮气或惰性气体保护下，升温至1000-2000℃，对面团进行碳化处理，处理时间为1-60min，然后在真空、氮气或惰性气体保护下冷却，制得所述泡沫碳。
上述步骤(1)中，所述碳源粉体为普通食用产品，如面粉、玉米粉、糯米粉或米粉中一种或两种以上，其粒度范围：50-150目。所述粉体或组合物为本发明的泡沫碳制备方法中的基础碳源，其它功能化添加物(如碳纤维、碳纳米管)可提供少量的碳；
上述步骤(1)中，加水量按碳源粉体重量的0.35-0.7的比例添加。
上述步骤(1)中，造孔剂用量为1-200g/千克碳源粉体，随种类不同用量有所不同。所述造孔剂为生物菌类造孔剂、有机物造孔剂或无机化合物造孔剂中任一种或两种以上，且当造孔剂中含有生物菌类造孔剂或有机物造孔剂时，搅拌成面团前，温度控制在0-38℃，成面团后于40-42℃条件下静置发酵0.5-3小时。
上述步骤(1)中，所述生物菌类造孔剂为酵母、酸奶中一种或两种的组合，所述有机物造孔剂为白糖、蜂蜜、牛奶、酒精或白酒中的一种或两种以上。
上述步骤(1)中，所述无机物造孔剂为碳酸钠、碳酸钙、碳酸氢钠、碳酸氢钙、碳酸铵、碳酸氢铵、碳酸钾、碳酸氢钾、碳酸镁等加热或高温条件下能分解产生气体的无机化合物；当采用上述造孔剂时，无需等待发酵。
所述步骤(1)中，在碳源粉体加入水中前，将强化或功能化添加物与造孔剂一起加入水中，用搅拌设备搅拌均匀，并在搅拌条件下缓慢加入碳源粉体，使添加物均匀分散于碳源粉体中，并揉制成团。所述添加物的用量为1-5000g/千克碳源。所述添加物用于泡沫碳的强化或功能化。
所述强化或功能化添加物是用于泡沫碳强化或功能化的物质，为普通陶瓷、玻璃、氧化物的粉体、微球、片状或不规则颗粒，具体为ZrO2、TiO2、Al2O3、Y2O3、La2O3、CeO2、Nd2O3等物质的一种或多种；
所述强化或功能化添加物是用于泡沫碳强化或功能化的物质，为玻璃纤维、陶瓷纤维、碳纤维、碳纳米管、石墨烯等物质的一种或多种；
所述强化或功能化添加物是用于泡沫碳强化或功能化的物质，为单质金属或合金混合物的粉体、微球、纤维、片状或不规则颗粒。具体为铁、钴、镍、铜、锌、锰、铝、镁、铬、钒、钛、钨、钼、钯、钌、铱、铂、金、银、镓、铟、锡、锗、硅等物质的一种或多种，或这些物质任意比组合形成的合金的一种或多种，或合金与单质的任意组合；
本发明所述的泡沫碳制备方法，也可不添加强化或功能化物质，直接制备普通的泡沫碳；
上述步骤(2)中，将面团压制成片、块或者用模具压制成特定形状，面团发泡定型较佳温度范围为：100-110℃，较佳保温时间为：25-35min；
上述步骤(3)中，经发泡定型的面团放入炉中进行预处理，较佳处理温度范围：210-300℃，炉温升温速度：5-10℃/min，较佳保温时间：15-90min；所述保护作用的氮气，纯度应达到99.999％或以上。所述惰性气体为氦气或氩气，纯度应达到99.999％或以上；
在步骤(3)中，当有更高要求时，可在真空或氮气或者惰性气体保护下进行预处理；
在步骤(4)中，升温过程中，500℃前，升温速度设定为5-10℃/min，防止升温太快，残余水分气化太快，或物质分解产生气体，可能导致气孔被大量破坏，500℃后，升温速度为10-20℃/min。
在步骤(4)中，如要求更高，则碳化后还可进行石墨化处理，即在完成上述碳化处理的保温时间后，以10-20℃/min的升温速度，继续升温至2500-3200℃，进行石墨化处理，到达预定温度后，保温时间1-20min，并在真空、氮气或惰性气体保护下冷却，制得石墨化的泡沫碳，不计强化或功能化添加物，泡沫碳的碳含量超过99％。
上述步骤(4)中所述保护作用的氮气，纯度应达到99.999％或以上。所述惰性气体为氦气或氩气，纯度应达到99.999％或以上；
与现有技术相比，本发明具有如下优点：
(1)本发明所述方法的碳源为面粉、玉米粉、糯米粉、米粉一种或多种的任意组合物，为可再生资源，廉价易得；
(2)本发明所述制备方法涉及化工试剂少，所用原料均为常见的廉价固态试剂，无挥发、易燃、有毒、刺激性强的化工试剂，原料安全、储运方便；
(3)本发明所述制备方法不涉及高精尖仪器设备，无需球磨、超声、高压等设备，有利于实现实用化；在制备面团时加入强化或功能化添加物，制备的泡沫碳的抗压强度得到一定程度的提高；
(4)由本发明所述泡沫碳制备方法，工艺简单、操作简便，成本低廉，相对于其他制备方法，本方法耗时短，效率高，极易实现产业化。
附图说明
图1为本发明实施例2制备得到的泡沫碳的图。
具体实施方式
为更好的理解本发明的技术特点，下面结合实施例对本发明作进一步说明，需要强调的是，实施例并非对本发明保护范围的限制。
以下通过具体实施例进行进一步的说明：
实施例1
以1000g碳源粉体为例进行说明。
(1)容器中放入水450g，加入酵母10g，搅拌均匀，加入白糖50g，搅拌溶解完全，搅拌条件下，将1000g面粉(100目)缓慢撒入，待面粉添加完成后，进行反复揉制，最后制成均匀的面团。将面团置于40±2℃的恒温箱中静置1小时，等待酵母发酵。
(2)发酵完成的面团，按需要压制成块状，厚度5mm，放入105±2℃的烘箱内，烘烤30min使面团发泡定型。
(3)上述发泡定型步骤完成后，使炉温继续升高至230℃进行预处理，保温30min，可除去水分，并将易氧化的元素氧化去除。
(4)上述预处理完成后，将预处理后的试样移入高温炉，启用氮气保护措施，500℃以下时，升温速度设定为8℃/min，防止升温太快，残余水分气化太快，或物质分解产生气体，可能导致气孔被大量破坏。500℃后，升温速度为18℃/min，升温至1300℃，保温15min，在保护气氛下冷却至200℃，即可取出试样，完成本发明所述泡沫碳的制备。通过本实施例所述工艺制备的泡沫炭孔隙率大，孔径均匀，平均孔径0.3mm，抗压强度1.8MPa。
实施例2
以1000g碳源粉体为例进行说明。
(1)容器中放入水500g，加入酵母5g，搅拌均匀，加入白糖60g，加入TiO2粉(型号R248)150g，搅拌分散均匀，并在搅拌条件下，将600g面粉(100目)与400g(100目)玉米粉的混合物缓慢撒入，待添加完成后，进行反复揉制，最后制成均匀的面团。将面团置于40±2℃的恒温箱中静置1小时，等待酵母发酵。取水30g，加入5gNaHCO3溶解完成，将NaHCO3溶液加入面团，重新揉制，使整个面团均匀，静置20min，完成面团的准备。
(2)发酵后的面团，按需要压制成20×20×10mm，放入105±2℃的烘箱内，烘烤35min使面团发泡定型。
(3)上述发泡定型步骤完成后，使炉温继续升高至230℃进行预处理，保温40min，可除去水分，并将易氧化的元素氧化去除。
(4)上述预处理完成后，将预处理后的试样移入高温炉，启用氮气保护措施，500℃以下时，升温速度设定为8℃/min，防止升温太快，残余水分气化太快，或物质分解产生气体，可能导致气孔被大量破坏。500℃后，升温速度为20℃/min，升温至1500℃，保温20min，在保护气氛下冷却至200℃，即可取出试样，完成本发明所述泡沫碳的制备。采用本例所述工艺制备的泡沫炭(参见图1)平均孔径0.2mm，抗压强度2.1MPa。所以在原料中增加强化添加物后，抗压强度得到一定程度的提高。
实施例3
以1000g碳源粉体为例进行说明。
(1)容器中放入水550g，加入酵母10g，搅拌均匀，加入白糖80g，加入长度为1-5mm的碳纤维50g，搅拌分散均匀，并在搅拌条件下，将500g面粉(80目)、300g玉米粉(80目)以及200g糯米粉的均匀混合粉体缓慢撒入，待添加完成后，进行反复揉制，最后制成均匀的面团。将面团置于40±2℃的恒温箱中静置1小时，等待酵母发酵。
(2)发酵后的面团，按需要压制成厚度50mm的片状，放入100±2℃的烘箱内，烘烤40min使面团发泡定型。
(3)上述发泡定型步骤完成后，使炉温继续升高至250℃进行预处理，保温25min，可除去水分，并将易氧化的元素氧化去除。
(4)上述预处理完成后，将预处理后的试样移入高温炉，启用氮气保护措施，500℃以下时，升温速度设定为8℃/min，防止升温太快，残余水分气化太快，或物质分解产生气体，可能导致气孔被大量破坏。500℃后，升温速度为18℃/min，升温至1200℃，保温30min，在保护气氛下冷却至200℃，即可取出试样，完成本发明所述泡沫碳的制备。通过本实施例所述工艺制备的泡沫炭孔隙率大，平均孔径0.4mm，抗压强度2.2MPa。
实施例4
以1000g碳源粉体为例进行说明。
(1)容器中放入水550g，加入酵母8g，搅拌均匀，加入白糖100g，加入ZrO2粉体(200目)50g，5-10mm的氧化铝陶瓷纤维(直径3-5μm)30g，镍粉20g(粒径150μm)，搅拌分散均匀，并在搅拌条件下，将1000g面粉(100目)缓慢撒入，待面粉添加完成后，进行反复揉制，最后制成均匀的面团。将面团置于45±2℃的恒温箱中静置0.5小时，等待酵母发酵。
(2)发酵后的面团，按需要压制成100×100×5mm，放入108±2℃的烘箱内，烘烤25min使面团发泡定型。
(3)上述发泡定型步骤完成后，使炉温继续升高至210℃进行预处理，保温45min，可除去水分，并将易氧化的元素氧化去除。
(4)上述预处理完成后，将预处理后的试样移入高温炉，启用氮气保护措施，500℃以下时，升温速度设定为8℃/min，防止升温太快，残余水分气化太快，或物质分解产生气体，可能导致气孔被大量破坏。500℃后，升温速度为18℃/min，升温至1300℃，保温25min，在保护气氛下冷却至200℃，即可取出试样，完成氧化铝陶瓷纤维增强的泡沫碳。采用本例所述工艺制备的泡沫炭平均孔径0.2mm，抗压强度可达2.5MPa。在制备面团时加入强化或功能化添加物后，抗压强度显著提升。
以上实施例仅为本发明较优的实施方式，仅用于解释本发明，而非限制本发明，本领域技术人员在未脱离本发明精神实质下所作的改变、替换、修饰等均应属于本发明的保护范围。

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1.一种泡沫碳制备方法，其特征在于，包括以下步骤：(1)制作面团：造孔剂均匀分散在水中，将碳源粉体加入含造孔剂的水中，搅拌成面团；(2)发泡定型：将面团压制成型，然后放入加热炉中，升温至90-120℃，保温20-40min，使面团发泡定型；(3)预处理：将炉温升至180-350℃，对定型的面团进行预处理，处理时间10-120min，排出面团中水分；(4)碳化烧结：将步骤(3)预处理后的面团移入高温炉，在真空条件、氮气或惰性气体保护下，升温至1000-2000℃，对面团进行碳化处理，处理时间为1-60min，然后在真空、氮气或惰性气体保护下冷却，制得所述泡沫碳。
2.根据权利要求1所述泡沫碳制备方法，其特征在于，所述碳源粉体是面粉、玉米粉、糯米粉或米粉中的一种或两种以上；造孔剂的量为1-200g/千克碳源粉体，所述造孔剂为生物菌类造孔剂、有机物造孔剂或无机化合物造孔剂中任意一种或两种以上，且当造孔剂中含有生物菌类造孔剂或有机物造孔剂时，搅拌成面团前，温度控制在0-38℃，成面团后于40-42℃条件下静置发酵0.5-3小时。
3.根据权利要求2所述泡沫碳制备方法，其特征在于，所述生物菌类造孔剂为酵母、酸奶的一种或两种以上；所述有机物造孔剂为白糖、蜂蜜、牛奶、酒精或白酒中的一种或两种以上；所述无机物造孔剂为碳酸钠、碳酸钙、碳酸氢钠、碳酸氢钙、碳酸铵、碳酸氢铵、碳酸钾、碳酸氢钾或碳酸镁中一种或两种以上。
4.根据权利要求1所述泡沫碳制备方法，其特征在于，所述步骤(1)中，在碳源粉体加入水中前，将强化或功能化添加物与造孔剂一起加入水中，并在搅拌条件下缓慢加入碳源粉体，所述添加物的用量为1-5000g/千克碳源。
5.根据权利要求4所述泡沫碳制备方法，其特征在于：所述强化或功能化添加物为普通陶瓷、玻璃、ZrO2、TiO2、Al2O3、Y2O3、La2O3、CeO2或Nd2O3中的一种或两种以上，所述添加物为粉体、微球、片状或不规则颗粒。
6.根据权利要求4所述泡沫碳制备方法，其特征在于，所述强化或功能化添加物为玻璃纤维、陶瓷纤维、碳纤维、碳纳米管或石墨烯中的一种或两种以上。
7.根据权利要求4所述泡沫碳制备方法，其特征在于：所述强化或功能化添加物为铁、钴、镍、铜、锌、锰、铝、镁、铬、钒、钛、钨、钼、钯、钌、铱、铂、金、银、镓、铟、锡、锗或硅中的一种或两种以上，所述添加物为粉体、微球、片状或不规则颗粒。
8.根据权利要求1所述泡沫碳制备方法，其特征在于，所述步骤(2)中发泡条件为升温至100-110℃，保温25-35min，所述步骤(3)中预处理条件为210-300℃，升温速度为5-10℃/min，保温时间为15-90min。
9.根据权利要求1所述泡沫碳制备方法，其特征在于，所述步骤(4)中，升温过程中，500℃前，升温速度设定为5-10℃/min，500℃后，升温速度为10-20℃/min。
10.根据权利要求1所述的制备方法，其特征在于，在所述步骤(4)的碳化处理后，以10-20℃/min的升温速度，继续升温至2500-3200℃，保温1-20min，进行石墨化处理，并在真空、氮气或惰性气体保护下冷却，制得石墨化的泡沫碳。
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