CN116639965A - 一种不规则结构的蜂窝型活性炭及其制备方法 - Google Patents
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Abstract
本发明涉及活性炭技术领域,且公开了一种不规则结构的蜂窝型活性炭及其制备方法,即以部分煅烧过的硅藻土与未煅烧的硅藻土为原料。利用纤维素遇水受热膨胀甚至糊化的特性,对硅藻土可以造孔和粘结。样品在高温下烧制得到多孔陶瓷,因纤维素膨胀而留下不规则的孔隙。利用回收的电解铝碳渣以及黄麻杆作为碳源制备活性炭。以煤焦油为高温粘合剂、羧甲基纤维素为低温粘合剂、豆油为增塑剂,混合电解铝碳渣和浸泡过磷酸的黄麻杆粉末,制备出活性炭反应物,在熔融状态下将多孔陶瓷浸渍吸附,然后送入反应管内碳化、活化,最终可以得到不规则结构的蜂窝型活性炭。
Description
技术领域
本发明涉及活性炭技术领域,具体为一种不规则结构的蜂窝型活性炭及其制备方法。
背景技术
活性炭是一种以碳为主要成分,内部具有大量孔隙并且比表面积巨大的微晶材料。其特殊的结构使它具有除了导电导热、机械强度高等碳材料拥有的特点外,同时还具有吸附能力强、易再生等优点。活性炭根据形状分类主要有颗粒活性炭、柱状活性炭、蜂窝活性炭、炭纤维等。其中蜂窝活性炭开孔率高、几何表面积大、扩散路程短,尤其是压力损失小,在吸附、催化等领域有广泛的应用前景。目前蜂窝活性炭的制备方式主要有涂载法和整体挤出法,申请号200410092429.4的专利《一种由煤直接制备蜂窝活性炭的方法》公开了以煤粉、乳化煤焦油、水溶性粘合剂、润滑剂和水经过粉碎、配料、捏合、挤出成型、干燥、碳化、活化,最终得到蜂窝状活性炭。
涂载法制备蜂窝型活性炭可以多孔陶瓷为基体。多孔陶瓷是一种有较多微孔、具有三维立体骨架结构的无机非金属材料。陶瓷材料本身耐高温、耐酸碱、机械强度高、不易变形,以硅藻土为原料制备的多孔陶瓷不仅成本低廉而且气孔率高,如文献《硅藻土基多孔陶瓷的制备及研究》报道了一种以硅藻土为主要原料,并以粘土为粘结剂、木屑为造孔剂制备出了一种较为理想的多孔陶瓷。
发明内容
(一)解决的技术问题
针对现有技术的不足,本发明提供了一种不规则结构的蜂窝型活性炭及其制备方法,赋予蜂窝型活性炭一种特异的不规则结构,提高了吸附率,有别于市面上的蜂窝炭。
(二)技术方案
一种不规则结构的蜂窝型活性炭的制备方法,所述制备方法如下:
步骤一、将生硅藻土组分1高温煅烧后冷却至20-30℃,得到煅烧硅藻土,将生硅藻土组分2和纤维素75-85℃干燥24-36h,然后将生硅藻土组分2与煅烧硅藻土一起球磨过筛,向过筛后的硅藻土混合物中加入去离子水球磨6-10h,再加入纤维素,搅拌1-4h,将浆料注入模具中干压成型,成型样品在85-95℃下干燥,然后送入反应炉中在空气气氛下升温焙烧,待自然冷却至20-35℃后,得到不规则结构的多孔陶瓷;
步骤二、将黄麻杆干燥粉碎后与磷酸溶液搅拌混合,煮沸3-8h后过滤,滤渣烘干,得到黄麻杆粉末,再将电解铝碳渣过筛水洗,然后干燥粉碎,再依次向粉末中加入黄麻杆粉末、煤焦油、羧甲基纤维素、豆油和去离子水混合均匀,将混合物手工反复捏合成泥状,送入练泥机中反复练泥,得到活性炭反应物,将其放在电炉上140-160℃加热熔融,然后放入不规则结构的多孔陶瓷浸渍吸附30-50min,取出陶瓷冷却至20-30℃,除去表面的活性炭反应物,得到负载活性炭反应物的多孔陶瓷;
步骤三、将负载活性炭反应物的多孔陶瓷置于反应管中,在氮气气氛下,以3-5℃/min的速率升温至750℃,碳化2-4h,碳化结束后再向反应管中通入水蒸气进行活化,2-4h后将产物取出冷却,用去离子水多次洗涤,烘干后得到不规则结构的蜂窝型活性炭。
优选的,所述步骤一中煅烧硅藻土、生硅藻土组分2、纤维素和去离子水的质量比为18-24:15-20:15-25:35-45。
优选的,所述步骤一中高温煅烧的温度为1100-1300℃,时间为1-3h。
优选的,所述步骤一中焙烧的升温速率为1-3℃/min,并分别在200℃、300℃、400℃、500℃保温1-3h,500℃以后升温速率为4-6℃/min,并在1000℃下保温20-40min。
优选的,所述步骤二中黄麻杆与磷酸的质量比为1:3.5-4.2。
优选的,所述步骤二中电解铝碳渣、黄麻杆粉末、煤焦油、羧甲基纤维素、豆油和去离子水的质量比为30-35:20-28:30-37:8-13:2-5:36-47。
(三)有益的技术效果
以廉价易得的硅藻土为原料。未煅烧过的生硅藻土吸水率和气孔率较大,而煅烧过的硅藻土的体积密度和抗折强度较大。因此将部分煅烧后与未煅烧的硅藻土混合可以将性能优化。利用纤维素遇水受热膨胀甚至糊化的特性,可以对硅藻土起到造孔和粘结的作用。干压成型后将样品在高温下烧制得到多孔陶瓷,因纤维素膨胀而留下不规则的孔隙。为了响应环保政策,利用回收的电解铝碳渣以及黄麻杆作为碳源制备活性炭。电解铝碳渣的主要成分为碳,而黄麻杆也是制备活性炭的优质材料,不仅木质素含量高,还具有中空多孔结构,利用磷酸可以将其分解、烧蚀。以煤焦油为高温粘合剂、羧甲基纤维素为低温粘合剂、豆油为增塑剂,混合电解铝碳渣和浸泡过磷酸的黄麻杆粉末,制备出活性炭反应物,在熔融状态下将多孔陶瓷浸渍其中,待吸附完成后冷却至室温,送入反应管内碳化,利用水蒸气活化,最终可以得到不规则结构的蜂窝型活性炭。
具体实施方式
实施例1
步骤一、将10g生硅藻土组分1在1200℃下煅烧2h后冷却至25℃,得到煅烧硅藻土,生硅藻土组分2和纤维素80℃干燥30h,然后将3g生硅藻土组分2与3.5g煅烧硅藻土一起球磨过筛,向过筛后的硅藻土混合物中加入6.5g去离子水球磨8h,再加入3g纤维素,搅拌2h,将浆料注入模具中干压成型,成型样品在90℃下干燥,然后送入反应炉中在空气气氛下升温焙烧,升温速率为2℃/min,并分别在200℃、300℃、400℃、500℃保温2h,500℃以后升温速率为5℃/min,并在1000℃下保温30min,待自然冷却至25℃后,得到不规则结构的多孔陶瓷;
步骤二、将6g黄麻杆干燥粉碎后与含24.6g磷酸的水溶液搅拌混合,煮沸5h后过滤,滤渣烘干,得到黄麻杆粉末,再将16.3g电解铝碳渣过筛水洗,然后干燥粉碎,再依次向粉末中加入13g黄麻杆粉末、17.4g煤焦油、5.6g羧甲基纤维素、2.1g豆油和19.7g去离子水混合均匀,将混合物手工反复捏合成泥状,送入练泥机中反复练泥,得到活性炭反应物,将其放在电炉上150℃加热熔融,然后放入不规则结构的多孔陶瓷浸渍吸附40min,取出陶瓷冷却至25℃,除去表面的活性炭反应物,得到负载活性炭反应物的多孔陶瓷;
步骤三、将负载活性炭反应物的多孔陶瓷置于反应管中,在氮气气氛下,以5℃/min的速率升温至750℃,碳化4h,碳化结束后再向反应管中通入水蒸气进行活化,4h后将产物取出冷却,用去离子水多次洗涤,烘干后得到不规则结构的蜂窝型活性炭。
实施例2
步骤一、将11g生硅藻土组分1在1200℃下煅烧2.5h后冷却至25℃,得到煅烧硅藻土,生硅藻土组分2和纤维素80℃干燥32h,然后将2.8g生硅藻土组分2与3.8g煅烧硅藻土一起球磨过筛,向过筛后的硅藻土混合物中加入6.2g去离子水球磨8h,再加入3.7g纤维素,搅拌3h,将浆料注入模具中干压成型,成型样品在90℃下干燥,然后送入反应炉中在空气气氛下升温焙烧,升温速率为2℃/min,并分别在200℃、300℃、400℃、500℃保温2h,500℃以后升温速率为5℃/min,并在1000℃下保温30min,待自然冷却至30℃后,得到不规则结构的多孔陶瓷;
步骤二、将6g黄麻杆干燥粉碎后与含23g磷酸的水溶液搅拌混合,煮沸5h后过滤,滤渣烘干,得到黄麻杆粉末,再将16.5g电解铝碳渣过筛水洗,然后干燥粉碎,再依次向粉末中加入12g黄麻杆粉末、17.5g煤焦油、6g羧甲基纤维素、2g豆油和20.5g去离子水混合均匀,将混合物手工反复捏合成泥状,送入练泥机中反复练泥,得到活性炭反应物,将其放在电炉上150℃加热熔融,然后放入不规则结构的多孔陶瓷浸渍吸附40min,取出陶瓷冷却至25℃,除去表面的活性炭反应物,得到负载活性炭反应物的多孔陶瓷;
步骤三、将负载活性炭反应物的多孔陶瓷置于反应管中,在氮气气氛下,以3℃/min的速率升温至750℃,碳化2h,碳化结束后再向反应管中通入水蒸气进行活化,2h后将产物取出冷却,用去离子水多次洗涤,烘干后得到不规则结构的蜂窝型活性炭。
实施例3
步骤一、将8g生硅藻土组分1在1100℃下煅烧1h后冷却至20℃,得到煅烧硅藻土,生硅藻土组分2和纤维素75℃干燥24h,然后将2.5g生硅藻土组分2与3g煅烧硅藻土一起球磨过筛,向过筛后的硅藻土混合物中加入5.8g去离子水球磨6h,再加入2.5g纤维素,搅拌1h,将浆料注入模具中干压成型,成型样品在85℃下干燥,然后送入反应炉中在空气气氛下升温焙烧,升温速率为1℃/min,并分别在200℃、300℃、400℃、500℃保温1h,500℃以后升温速率为4℃/min,并在1000℃下保温20min,待自然冷却至20℃后,得到不规则结构的多孔陶瓷;
步骤二、将6g黄麻杆干燥粉碎后与含25.2g磷酸的水溶液搅拌混合,煮沸8h后过滤,滤渣烘干,得到黄麻杆粉末,再将17.5g电解铝碳渣过筛水洗,然后干燥粉碎,再依次向粉末中加入14g黄麻杆粉末、18.5g煤焦油、6.5g羧甲基纤维素、2.5g豆油和23.5g去离子水混合均匀,将混合物手工反复捏合成泥状,送入练泥机中反复练泥,得到活性炭反应物,将其放在电炉上160℃加热熔融,然后放入不规则结构的多孔陶瓷浸渍吸附50min,取出陶瓷冷却至30℃,除去表面的活性炭反应物,得到负载活性炭反应物的多孔陶瓷;
步骤三、将负载活性炭反应物的多孔陶瓷置于反应管中,在氮气气氛下,以4℃/min的速率升温至750℃,碳化2.5h,碳化结束后再向反应管中通入水蒸气进行活化,3h后将产物取出冷却,用去离子水多次洗涤,烘干后得到不规则结构的蜂窝型活性炭。
实施例4
步骤一、将13g生硅藻土组分1在1300℃下煅烧3h后冷却至25℃,得到煅烧硅藻土,生硅藻土组分2和纤维素85℃干燥36h,然后将3.3g生硅藻土组分2与4g煅烧硅藻土一起球磨过筛,向过筛后的硅藻土混合物中加入7.5g去离子水球磨10h,再加入4.2g纤维素,搅拌4h,将浆料注入模具中干压成型,成型样品在95℃下干燥,然后送入反应炉中在空气气氛下升温焙烧,升温速率为3℃/min,并分别在200℃、300℃、400℃、500℃保温3h,500℃以后升温速率为6℃/min,并在1000℃下保温40min,待自然冷却35℃后,得到不规则结构的多孔陶瓷;
步骤二、将6g黄麻杆干燥粉碎后与含21g磷酸的水溶液搅拌混合,煮沸3h后过滤,滤渣烘干,得到黄麻杆粉末,再将15g电解铝碳渣过筛水洗,然后干燥粉碎,再依次向粉末中加入10g黄麻杆粉末、15g煤焦油、4g羧甲基纤维素、1g豆油和18g去离子水混合均匀,将混合物手工反复捏合成泥状,送入练泥机中反复练泥,得到活性炭反应物,将其放在电炉上140℃加热熔融,然后放入不规则结构的多孔陶瓷浸渍吸附30min,取出陶瓷冷却至20℃,除去表面的活性炭反应物,得到负载活性炭反应物的多孔陶瓷;
步骤三、将负载活性炭反应物的多孔陶瓷置于反应管中,在氮气气氛下,以5℃/min的速率升温至750℃,碳化2h,碳化结束后再向反应管中通入水蒸气进行活化,4h后将产物取出冷却,用去离子水多次洗涤,烘干后得到不规则结构的蜂窝型活性炭。
实施例5
步骤一、3g生硅藻土组分1在1100℃下煅烧3h后冷却至20℃,得到煅烧硅藻土,生硅藻土组分2和纤维素85℃干燥24h,然后将3.3g生硅藻土组分2与3g煅烧硅藻土一起球磨过筛,向过筛后的硅藻土混合物中加入7.5g去离子水球磨6h,再加入4.2g纤维素,搅拌1h,将浆料注入模具中干压成型,成型样品在95℃下干燥,然后送入反应炉中在空气气氛下升温焙烧,升温速率为1℃/min,并分别在200℃、300℃、400℃、500℃保温3h,500℃以后升温速率为4℃/min,并在1000℃下保温40min,待自然冷却至20℃后,得到不规则结构的多孔陶瓷;
步骤二、将6g黄麻杆干燥粉碎后与含25.2g磷酸的水溶液搅拌混合,煮沸3h后过滤,滤渣烘干,得到黄麻杆粉末,再将17.5g电解铝碳渣过筛水洗,然后干燥粉碎,再依次向粉末中加入10g黄麻杆粉末、18.5g煤焦油、4g羧甲基纤维素、2.5g豆油和18g去离子水混合均匀,将混合物手工反复捏合成泥状,送入练泥机中反复练泥,得到活性炭反应物,将其放在电炉上160℃加热熔融,然后放入不规则结构的多孔陶瓷浸渍吸附30min,取出陶瓷冷却至30℃,除去表面的活性炭反应物,得到负载活性炭反应物的多孔陶瓷;
步骤三、将负载活性炭反应物的多孔陶瓷置于反应管中,在氮气气氛下,以4℃/min的速率升温至750℃,碳化3h,碳化结束后再向反应管中通入水蒸气进行活化,3h后将产物取出冷却,用去离子水多次洗涤,烘干后得到不规则结构的蜂窝型活性炭。
利用比表面积测定仪测定产品的N2吸附脱附等温线,根据数据结果通过BET方程和BJH计算模型得出平均孔径和孔容积。
根据国标GB/T2006-2008测试机械强度。
根据表格可知本发明制得的蜂窝型活性炭的比表面积在390-410m2/g左右,孔容积在0.4-0.5cm3/g左右,机械强度在7.0-8.5MPa左右。
Claims (6)
1.一种不规则结构的蜂窝型活性炭的制备方法,其特征在于:所述制备方法如下:
步骤一、将生硅藻土组分1高温煅烧后冷却至20-30℃,得到煅烧硅藻土,将生硅藻土组分2和纤维素75-85℃干燥24-36h,然后将生硅藻土组分2与煅烧硅藻土一起球磨过筛,向过筛后的硅藻土混合物中加入去离子水球磨6-10h,再加入纤维素,搅拌1-4h,将浆料注入模具中干压成型,成型样品在85-95℃下干燥,然后送入反应炉中在空气气氛下升温焙烧,待自然冷却至20-35℃后,得到不规则结构的多孔陶瓷;
步骤二、将黄麻杆干燥粉碎后与磷酸溶液搅拌混合,煮沸3-8h后过滤,滤渣烘干,得到黄麻杆粉末,再将电解铝碳渣过筛水洗,然后干燥粉碎,再依次向粉末中加入黄麻杆粉末、煤焦油、羧甲基纤维素、豆油和去离子水混合均匀,将混合物手工反复捏合成泥状,送入练泥机中反复练泥,得到活性炭反应物,将其放在电炉上140-160℃加热熔融,然后放入不规则结构的多孔陶瓷浸渍吸附30-50min,取出陶瓷冷却至20-30℃,除去表面的活性炭反应物,得到负载活性炭反应物的多孔陶瓷;
步骤三、将负载活性炭反应物的多孔陶瓷置于反应管中,在氮气气氛下,以3-5℃/min的速率升温至750℃,碳化2-4h,碳化结束后再向反应管中通入水蒸气进行活化,2-4h后将产物取出冷却,用去离子水多次洗涤,烘干后得到不规则结构的蜂窝型活性炭。
2.根据权利要求1所述的不规则结构的蜂窝型活性炭的制备方法,其特征在于:所述步骤一中煅烧藻土、生硅藻土组分2、纤维素和去离子水的质量比为18-24:15-20:15-25:35-45。
3.根据权利要求1所述的不规则结构的蜂窝型活性炭的制备方法,其特征在于:所述步骤一中高温煅烧的温度为1100-1300℃,时间为1-3h。
4.根据权利要求1所述的不规则结构的蜂窝型活性炭的制备方法,其特征在于:所述步骤一中焙烧的升温速率为1-3℃/min,并分别在200℃、300℃、400℃、500℃保温1-3h,500℃以后升温速率为4-6℃/min,并在1000℃下保温20-40min。
5.根据权利要求1所述的不规则结构的蜂窝型活性炭的制备方法,其特征在于:所述步骤二中黄麻杆与磷酸的质量比为1:3.5-4.2。
6.根据权利要求1所述的不规则结构的蜂窝型活性炭的制备方法,其特征在于:所述步骤二中电解铝碳渣、黄麻杆粉末、煤焦油、羧甲基纤维素、豆油和去离子水的质量比为30-35:20-28:30-37:8-13:2-5:36-47。
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CN117258755A (zh) * | 2023-09-15 | 2023-12-22 | 福建省鑫森炭业股份有限公司 | 一种抗开裂蜂窝活性炭及其制备方法 |
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