CN109137488A - 一种钴-铁-磷非晶合金/聚合物复合纤维及生产方法 - Google Patents

一种钴-铁-磷非晶合金/聚合物复合纤维及生产方法 Download PDF

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CN109137488A
CN109137488A CN201710497670.2A CN201710497670A CN109137488A CN 109137488 A CN109137488 A CN 109137488A CN 201710497670 A CN201710497670 A CN 201710497670A CN 109137488 A CN109137488 A CN 109137488A
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刘志红
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Abstract

一种钴‑铁‑磷非晶合金/聚合物复合纤维长度可连续，复合纤维为圆形、扁平等断面；复合纤维包覆层为钴‑铁‑磷非晶合金，具体成分为Co60‑85%，Fe10‑25%，P5‑25%，复合纤维芯丝材质为聚合物；复合纤维外径为0.01‑0.5mm，复合纤维芯丝直径为0.005‑0.4mm。复合纤维生产方法步骤为：(1)采用碱性溶液，对聚合物纤维进行除油脱脂；(2)采用铬酐和硫酸溶液进行纤维表面的粗化；(3)采用酸性的锡盐溶液进行纤维的敏化；(4)采用硝酸银和氨水溶液进行纤维表面的活化；(5)纤维的化学镀钴‑铁‑磷合金；(6)纤维电刷镀钴‑铁‑磷非晶合金。

Description

一种钴-铁-磷非晶合金/聚合物复合纤维及生产方法
技术领域
本发明涉及到金属复合纤维领域，尤其是涉及一种钴-铁-磷非晶合金/聚合物复合纤维及生产方法。
背景技术
非晶合金由于具有以下特点；①非晶态合金在很宽的范围内可以制成各种组成的样品，从而可以在较宽大范围内调变它们的电子性质；②催化活性中心可以以单一的形式均匀分布在化学均匀的环境中；③非晶态合金表面具有浓度较高的不饱和中心，且不饱和中心的配位数具有一定的范围，因而使其催化活性和选择性一般优于相应的晶态催化剂；④其表面的非多孔性是其摆脱了多项催化剂存在的反应物种的扩散影响表面反应的问题。
非晶态合金催化剂可以用于加氢、氧化、裂解、异构化等反应。目前，非晶态合金催化剂的制备方法有多种，一般来说可以将其分为两大类：液体骤冷法和原子（离子）沉积法。非晶合金催化电极以沉积薄膜或镀层的二维催化电极为主，但其反应器面积较小，导致产率较小。
针对以上不足，本发明提出一种钴-铁-磷非晶合金/聚合物复合纤维及其制备方法，钴-铁-磷非晶合金/聚合物复合纤维可用来织成布作于催化剂，可极大的增加钴铁磷催化剂反应器的表面积，同时，也可省却粉末催化剂的载体，此纤维还可广泛应用于磁介质粉体、电磁波吸收剂等。
发明内容
本发明要解决的技术问题是提供一种钴-铁-磷非晶合金/聚合物复合纤维，复合纤维为圆形、扁平等断面，复合纤维包覆层为钴-铁-磷非晶合金，具体成分为Co60-85%，Fe10-25%，P5-25%，复合纤维芯丝材质为聚合物，复合纤维外径为0.01-0.5mm，复合纤维芯丝直径为0.005-0.4mm。
钴-铁-磷非晶合金/聚合物复合纤维的生产方法：对聚合物纤维先进行表面处理（粗化、敏化、活化），然后纤维的化学镀钴-铁-磷合金，最后，电刷镀制成钴-铁-磷非晶合金/聚合物复合纤维。
本发明解决其技术问题所采用的方案，包括以下步骤：
(1) 采用碱性溶液，对聚合物纤维进行除油脱脂；
(2) 采用铬酐和硫酸溶液进行纤维表面的粗化；粗化液组成为铬酐30-100g/L 、200-400 ml/L 硫酸，粗化处理温度为50-70℃：
(3) 采用酸性的锡盐溶液进行纤维的敏化；敏化液组成为氯化锡5-10g/L，盐酸10-50ml/L ：
(4) 采用硝酸银和氨水溶液进行纤维表面的活化；
(5) 纤维的化学镀钴-铁-磷合金，溶液组成为：硫酸钴0.05-0.5mol/L，可溶性亚铁盐0.03-0.3mol/L，次磷酸钠0.1-0.5mol/L，羧酸盐0.05-0.5 mol/L，还原剂2-10g/L，滴定强酸溶液Ph值为3-5，化学镀时溶液温度为50-85℃，化学镀时间为0.5-2min；
所述还原剂为碘化钾、硼氢化盐等；
(6) 纤维电刷镀钴-铁-磷非晶合金
电刷镀溶液组成：可溶性钴盐1.2-3.5mol/L、酸0.2-0.8mol/L、可溶性亚铁盐0.2-1.5mol/L、亚磷酸或次磷酸盐0.3-1.0mol/L、 络合剂0.5-15g/L、还原剂2-8g/L、余量水；
上述酸包括硼酸、磷酸、羧酸等多元中强酸；
上述络合剂包括糖精、羧酸盐等；
所述还原剂为碘化钾、抗坏血酸等；
制备工艺参数为：阳极采用石墨板，电刷镀纤维，电极相对运动速度为5-20m/min（优选10-15m/min），滴定强酸溶液使镀液Ph值2-6，施镀温度为30-80℃。
本发明具有以下优点：
1. 由于采用铁基非晶合金颗粒作为催化剂，可提高电极的催化性能；
2. 由于采用电镀+剥离+破碎制备铁基非晶合金微粒，微粒基本形状为层片状，这提高了非晶合金催化剂反应的表面积；
3.由于采用槽型电极架，并在两侧板开设有长方形孔，端部也未封闭，最大限度提高了溶液在电极内部的可流动性，增大催化电极与溶液的相对流动，可提高催化电极的催化效率；
4. 由于采用抽插式结构，因此电极的反应器面积以及催化电极板的间距很容易调整，也便于更换与维修。
具体实施方式：
以下结合实施例对本发明作进一步说明：
实施例1：钴-铁-磷非晶合金/聚丙烯复合纤维的成形工艺
（1）选择φ0.05 mm聚丙烯纤维，先采用氢氧化钠溶液进行化学除油；
（2）除油后纤维的粗化，粗化的水溶液配比为80g/L 铬酐、250ml/L 硫酸，粗化处理温度为70℃，粗化处理时间8 min；
（3）聚丙烯纤维的敏化，其溶液组成为氯化锡8g/L，盐酸40ml/L ，敏化处理时间1 min；
（4）采用硝酸银和氨水溶液进行纤维表面的活化，活化后的纤维经甲醛溶液还原；
（5）纤维的化学镀钴-铁-磷合金，溶液成分为：氯化钴0.1mol/L，氯化亚铁0.03mol/L、酒石酸0.08 mol/L，次磷酸钠0.1mol/L，碘化钾2.5g/L，硼氢化钠4g/L，滴定盐酸溶液Ph值为4，化学镀时间为0.5 min；
（6）电刷镀钴-铁-磷非晶合金
电镀液组成：氯化钴2.5mol/L、氯化亚铁0.6mol、L，硼酸0.4mol/L、次磷酸钠0.4mol/L，柠檬酸钠1.2g/L、碘化钾3g/L，余量水；制备工艺参数为：阳极采用石墨板，在纤维两侧电刷镀，电极相对运动速度为8 m/min，滴定强酸溶液使镀液Ph值3。
实施例2：钴-铁-磷非晶合金/尼龙复合纤维的成形工艺
（1）选择φ0.05 mm聚丙烯纤维，先采用氢氧化钠溶液进行化学除油；
（2）除油后纤维的粗化，粗化的水溶液配比为80g/L 铬酐、250ml/L 硫酸，粗化处理温度为70℃，粗化处理时间8 min；
（3）聚丙烯纤维的敏化，其溶液组成为氯化锡8g/L，盐酸40ml/L ，敏化处理时间1 min；
（4）采用硝酸银和氨水溶液进行纤维表面的活化，活化后的纤维经甲醛溶液还原；
（5）纤维的化学镀钴-铁-磷合金，溶液成分为：氯化钴0.1mol/L，硫酸亚铁0.04mol/L、酒石酸0.1 mol/L，次磷酸钠0.1mol/L，碘化钾3 g/L，硼氢化钠2g/L，滴定盐酸溶液Ph值为4，化学镀时间为0.5 min；
（6）电刷镀钴-铁-磷非晶合金
电镀液组成：硫酸钴3mol/L、硫酸亚铁0.5mol/L，硼酸0.4mol/L、次磷酸钠0.35mol/L，糖精3g/L，柠檬酸钠2 g/L、余量水；制备工艺参数为：阳极采用石墨板，在纤维两侧电刷镀，电极相对运动速度为8 m/min，滴定强酸溶液使镀液Ph值3。

Claims (4)

1.一种钴-铁-磷非晶合金/聚合物复合纤维，其特征在于，长度可连续，复合纤维为圆形、扁平等断面；复合纤维包覆层为钴-铁-磷非晶合金，具体成分为Co60-85%，Fe10-25%，P5-25%，复合纤维芯丝材质为聚合物；复合纤维外径为0.01-0.5mm，复合纤维芯丝直径为0.005-0.4mm。
2.一种钴-铁-磷非晶合金/聚合物复合纤维生产方法，其特征在于，步骤为：(1) 采用碱性溶液，对聚合物纤维进行除油脱脂；(2) 采用铬酐和硫酸溶液进行纤维表面的粗化；(3) 采用酸性的锡盐溶液进行纤维的敏化； (4) 采用硝酸银和氨水溶液进行纤维表面的活化； (5) 纤维的化学镀钴-铁-磷合金； (6) 纤维电刷镀钴-铁-磷非晶合金。
3.权利要求2所述，化学镀的溶液组成为：硫酸钴0.05-0.5mol/L，可溶性亚铁盐0.03-0.3mol/L，次磷酸钠0.1-0.5mol/L，羧酸盐0.05-0.5 mol/L，还原剂2-10g/L；其工艺参数特征在于，溶液Ph值为3-5，化学镀时溶液温度为50-85℃，化学镀时间为0.5-2min；
上述还原剂为碘化钾、硼氢化盐等。
4.权利要求2所述，电刷镀溶液组成为：可溶性钴盐1.2-3.5mol/L、酸0.2-0.8mol/L、可溶性亚铁盐0.2-1.5mol/L、亚磷酸或次磷酸盐0.3-1.0mol/L、 络合剂0.5-15g/L、还原剂2-8g/L、余量水；
上述酸包括硼酸、磷酸、羧酸等多元中强酸；
上述络合剂包括糖精、羧酸盐等；
上述还原剂为碘化钾、抗坏血酸等；
上述工艺参数为：阳极采用石墨板，电极相对运动速度为5-20m/min（优选10-15m/min），滴定强酸溶液使镀液Ph值2-6，施镀温度为30-80℃。
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