CN108048957A - 一种中空结构的活性碳纤维的制备工艺 - Google Patents
一种中空结构的活性碳纤维的制备工艺 Download PDFInfo
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- D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
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Abstract
本发明公开了一种中空结构的活性碳纤维的制备工艺，该方法步骤如下：将高碳材料输入到高速纺丝机中纺丝获得中空纤维；将中空纤维置于加入交联剂的化学交联器中反应；然后放入碳化活化装置中预氧化；之后通入惰性气体并在惰性气体保护下，升温到550‑750℃，进行碳化2h，碳化处理完成后升温到1000‑1200℃并通入活化剂进行活化处理2h；e、活化处理后将碳化完成的纤维转入温度为2500‑2800℃的石墨化炉中碳化1‑3小时，继续通入氮气进行保护并冷却至常温即可得到具有中空结构的活性碳纤维。本发明的产品外径可控制在5‑100μm、且可以相应控制内径的尺寸，制备工艺简单、成本低、无污染且产品性能好、产量大。
Description
技术领域
本发明涉及碳纤维的制备领域，具体的说是一种制备工艺简单、产品性能好且成品率高、无污染、综合成本低的中空结构的活性碳纤维的制备工艺。
背景技术
活性碳纤维（activated carbon fiber, ACF）因其优异的吸附性能而广泛用于空气净化和除湿、冰箱的除异味、气体净制、有机溶剂及化合物回收、工业有机废水治理、防毒气、水净化、净制高纯水、催化剂或催化剂载体以及生理用品等，并且用活性碳纤维毡回收有机溶剂早已工业化，空气净化机、除湿机及净水器业已问世，在环境保护方面充分显示了它的高效吸附效能。此外基于其丰富的孔隙结构和碳质的特性，作为储能材料和电极材料，活性碳纤维在新能源领域正在发挥着重要作用。中空的碳纤维具有强度高、导电性强等优点，借助于微米操作技术可以对中空碳纤维进行单根操作，可以用于微电子器件、电容器、电池电极材料等，但具有中空结构的活性碳纤维产品未见报道，也没有批量生产。
发明内容
本发明的目的是针对现有技术存在的缺陷，提供一种制备工艺简单、产品性能好且成品率高、无污染、综合成本低的中空结构的活性碳纤维的制备工艺。
本发明的目的是通过以下技术方案解决的：
一种中空结构的活性碳纤维的制备工艺，其特征在于：该方法步骤如下：
a、将高碳材料输入到高速纺丝机中，高速纺丝机在350-420℃下将高碳材料纺丝，即得中空纤维；
b、将纺出的中空纤维置于化学交联器中，加入交联剂盐酸、甲醛或氧气使其在60-75℃下反应2h；
c、将步骤（b）处理过的中空纤维放入碳化活化装置中，经空压机吹入大量热风，使碳化活化装置内按照3-8℃/min的升温速率升温到280-350℃，预氧化1h；
d、然后通入惰性气体并在惰性气体保护下，升温到550-750℃，进行碳化2h，碳化处理完成后升温到1000-1200℃并通入活化剂进行活化处理2h；
e、活化处理后将碳化完成的纤维转入温度为2500-2800℃的石墨化炉中碳化1-3小时，继续通入氮气进行保护并冷却至常温即可得到具有中空结构的活性碳纤维。
所述步骤（a）中的高碳材料是指酚醛树脂、沥青、聚丙烯腈、ABS树脂或丁苯橡胶。
所述步骤（a）中的高碳材料的含碳量超过85%。
所述步骤（c）中的预氧化升温速率为5-7℃/min。
所述步骤（d）中的活化剂为碳酸氢钠、硫酸、磷酸中的两种或三种混合而成的混合物。
本发明相比现有技术有如下优点：
本发明制备的活性碳纤维具有较大的比表面积、较强的吸附活性和机械强度；并且活性碳纤维的伸长率高，不易断裂，电化学性能好，产品外径可控制在5-100μm、且可以相应控制内径的尺寸，制备工艺简单、操作容易、产品性能好，并且成品率高、综合成本低，耗能比值低，废气废水废物全部循环利用，无污染。
具体实施方式
下面结合实施例对本发明作进一步的说明。
一种中空结构的活性碳纤维的制备工艺，该方法步骤如下：a、将粉碎后的高碳材料输入到高速纺丝机中，高速纺丝机在350-420℃下将高碳材料纺丝，即得中空纤维；b、将纺出的中空纤维置于化学交联器中，加入交联剂盐酸、甲醛或氧气使其在60-75℃下反应2h；c、将步骤（b）处理过的中空纤维放入碳化活化装置中，经空压机吹入大量热风，使碳化活化装置内按照5-7℃/min的升温速率升温到280-350℃，预氧化1h；d、然后通入惰性气体并在惰性气体保护下，升温到550-750℃，进行碳化2h，碳化处理完成后升温到1000-1200℃并通入碳酸氢钠、硫酸、磷酸中的两种或三种混合而成的活化剂进行活化处理2h；e、活化处理后将碳化完成的纤维转入温度为2500-2800℃的石墨化炉中碳化1-3小时，继续通入氮气进行保护并冷却至常温即可得到具有中空结构的活性碳纤维。在上述工艺中，高碳材料的含碳量超过85%且高碳材料是指酚醛树脂、沥青、聚丙烯腈、ABS树脂或丁苯橡胶。
实施例1
将粉碎后的沥青输入到高速纺丝机中，高速纺丝机在380℃下将高碳材料纺丝，即得中空纤维；将纺出的中空纤维置于化学交联器中，加入交联剂盐酸、甲醛或氧气使其在65℃下反应2h；之后中空纤维放入碳化活化装置中，经空压机吹入大量热风，使碳化活化装置内按照5℃/min的升温速率升温到320℃，预氧化1h；然后通入惰性气体并在惰性气体保护下，升温到720℃，进行碳化2h，碳化处理完成后升温到1100℃并通入碳酸氢钠、磷酸混合而成的活化剂进行活化处理2h；活化处理后将碳化完成的纤维转入温度为2800℃的石墨化炉中碳化2小时，继续通入氮气进行保护并冷却至常温即可得到具有中空结构的活性碳纤维。
实施例2
将粉碎后的酚醛树脂输入到高速纺丝机中，高速纺丝机在400℃下将高碳材料纺丝，即得中空纤维；将纺出的中空纤维置于化学交联器中，加入交联剂盐酸、甲醛或氧气使其在70℃下反应2h；之后中空纤维放入碳化活化装置中，经空压机吹入大量热风，使碳化活化装置内按照6℃/min的升温速率升温到325℃，预氧化1h；然后通入惰性气体并在惰性气体保护下，升温到700℃，进行碳化2h，碳化处理完成后升温到1120℃并通入硫酸、磷酸混合而成的活化剂进行活化处理2h；活化处理后将碳化完成的纤维转入温度为2750℃的石墨化炉中碳化3小时，继续通入氮气进行保护并冷却至常温即可得到具有中空结构的活性碳纤维。
实施例3
将粉碎后的聚丙烯腈输入到高速纺丝机中，高速纺丝机在360℃下将高碳材料纺丝，即得中空纤维；将纺出的中空纤维置于化学交联器中，加入交联剂盐酸、甲醛或氧气使其在60℃下反应2h；之后中空纤维放入碳化活化装置中，经空压机吹入大量热风，使碳化活化装置内按照7℃/min的升温速率升温到340℃，预氧化1h；然后通入惰性气体并在惰性气体保护下，升温到650℃，进行碳化2h，碳化处理完成后升温到1080℃并通入碳酸氢钠、硫酸、磷酸混合而成的活化剂进行活化处理2h；活化处理后将碳化完成的纤维转入温度为2780℃的石墨化炉中碳化2.5小时，继续通入氮气进行保护并冷却至常温即可得到具有中空结构的活性碳纤维。
实施例4
将粉碎后的丁苯橡胶输入到高速纺丝机中，高速纺丝机在420℃下将高碳材料纺丝，即得中空纤维；将纺出的中空纤维置于化学交联器中，加入交联剂盐酸、甲醛或氧气使其在75℃下反应2h；之后中空纤维放入碳化活化装置中，经空压机吹入大量热风，使碳化活化装置内按照5℃/min的升温速率升温到310℃，预氧化1h；然后通入惰性气体并在惰性气体保护下，升温到580℃，进行碳化2h，碳化处理完成后升温到1150℃并通入碳酸氢钠、硫酸混合而成的活化剂进行活化处理2h；活化处理后将碳化完成的纤维转入温度为2800℃的石墨化炉中碳化1.5小时，继续通入氮气进行保护并冷却至常温即可得到具有中空结构的活性碳纤维。
本发明制备的活性碳纤维具有较大的比表面积、较强的吸附活性和机械强度；并且活性碳纤维的伸长率高，不易断裂，电化学性能好，产品外径可控制在5-100μm、且可以相应控制内径的尺寸，制备工艺简单、操作容易、产品性能好，并且成品率高、综合成本低，耗能比值低，废气废水废物全部循环利用，无污染。
以上实施例仅为说明本发明的技术思想，不能以此限定本发明的保护范围，凡是按照本发明提出的技术思想，在技术方案基础上所做的任何改动，均落入本发明保护范围之内；本发明未涉及的技术均可通过现有技术加以实现。
Claims (5)
1.一种中空结构的活性碳纤维的制备工艺，其特征在于：该方法步骤如下：
a、将高碳材料输入到高速纺丝机中，高速纺丝机在350-420℃下将高碳材料纺丝，即得中空纤维；
b、将纺出的中空纤维置于化学交联器中，加入交联剂盐酸、甲醛或氧气使其在60-75℃下反应2h；
c、将步骤（b）处理过的中空纤维放入碳化活化装置中，经空压机吹入大量热风，使碳化活化装置内按照3-8℃/min的升温速率升温到280-350℃，预氧化1h；
d、然后通入惰性气体并在惰性气体保护下，升温到550-750℃，进行碳化2h，碳化处理完成后升温到1000-1200℃并通入活化剂进行活化处理2h；
e、活化处理后将碳化完成的纤维转入温度为2500-2800℃的石墨化炉中碳化1-3小时，继续通入氮气进行保护并冷却至常温即可得到具有中空结构的活性碳纤维。
2.根据权利要求1所述的中空结构的活性碳纤维的制备工艺，其特征在于：所述步骤（a）中的高碳材料是指酚醛树脂、沥青、聚丙烯腈、ABS树脂或丁苯橡胶。
3.根据权利要求1或2所述的中空结构的活性碳纤维的制备工艺，其特征在于：所述步骤（a）中的高碳材料的含碳量超过85%。
4.根据权利要求1所述的中空结构的活性碳纤维的制备工艺，其特征在于：所述步骤（c）中的预氧化升温速率为5-7℃/min。
5.根据权利要求1所述的中空结构的活性碳纤维的制备工艺，其特征在于：所述步骤（d）中的活化剂为碳酸氢钠、硫酸、磷酸中的两种或三种混合而成的混合物。
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| CN108906017A (zh) * | 2018-06-27 | 2018-11-30 | 江苏弗瑞仕环保科技有限公司 | 用于空气净化的光催化材料的制备方法 |
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| CN112201800A (zh) * | 2020-09-10 | 2021-01-08 | 广东德九新能源有限公司 | 一种高导电性石墨化碳纤维电极及其制备方法和应用 |
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