CN109136889A - 一种钴-镍-磷催化反应器及生产方法 - Google Patents

一种钴-镍-磷催化反应器及生产方法 Download PDF

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CN109136889A
CN109136889A CN201710497639.9A CN201710497639A CN109136889A CN 109136889 A CN109136889 A CN 109136889A CN 201710497639 A CN201710497639 A CN 201710497639A CN 109136889 A CN109136889 A CN 109136889A
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罗奕兵
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Abstract

一种钴‑镍‑磷催化反应器及生产方法，反应器由钴‑镍‑磷复合纤维和反应器架子组成，钴‑镍‑磷复合纤维长度可连续，复合纤维的断面为圆形、扁平、薄带等形状，复合纤维的截面面积不大于2 mm2；复合纤维的包覆层为钴‑镍‑磷合金或非晶合金，具体成分为Co为40‑85%，Ni为10‑20%，P为6‑20%，包覆层厚度不大于0.5mm，包覆层与芯丝之间采用化学镀镍为过渡层，复合纤维的芯丝材质为聚合物，芯丝断面形状可为圆形、扁平、薄带等形状。反应器及生产步骤为：（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)纤维的化学镀镍；(6)纤维电刷镀钴‑镍‑磷非晶合金（或合金）；（7）钴‑镍‑磷催化反应器的制备。

Description

一种钴-镍-磷催化反应器及生产方法
技术领域
本发明涉及到催化反应器的生产领域，尤其是涉及一种钴-镍-磷催化反应器及生产方法。
背景技术
软磁材料的功能主要是导磁、电磁能量的转换与传输。目前，应用于软磁材料大体上可分为四类：合金薄带或薄片；非晶态合金薄带；磁介质粉料，经电绝缘介质包覆和粘合后按要求压制成形；铁氧体。以过渡金属（铁、钴、镍）为基质的非晶合金具有优异的软磁性，饱和磁感应强度高和交流损耗低，可广泛应用于高、低频变压器（部分代替硅钢片和坡莫合金）、磁传感器、记录磁头、磁屏蔽材料等。随着电子工程技术的迅速发展，先进软磁材料的研制和开发逐渐成为该领域的一个热点。采用过渡金属（铁、钴、镍）为基质的纤维制备磁介质粉体材料，可显著提高器件的软磁性能。同时，对钴镍磷合金的研究表明，具有较高的析氢催化活性，有利于降低槽压，提高效率。目前，对钴镍磷合金的相关研究更多集中于块体材料以及平板类镀层的相关领域。
针对以上不足，提出一种一种钴-镍-磷催化反应器及生产方法，是以钴-镍-磷非晶合金或合金作为催化剂，以聚合物芯丝（或带）作为催化剂载体，此反应器可广泛应用于各种气态、液态的催化反应。
发明内容
本发明要解决的技术问题是提供一种钴-镍-磷催化反应器及生产方法，反应器由钴-镍-磷复合纤维和反应器架子组成，复合纤维长度可连续，复合纤维的断面可为圆形、扁平、薄带等形状，复合纤维的截面面积不大于2 mm2；复合纤维的包覆层为钴-镍-磷合金或非晶合金，具体成分为Co为40-85%，Ni为10-20%，P为6-20%，包覆层厚度不大于0.5mm，包覆层与芯丝之间采用化学镀镍为过渡层，复合纤维的芯丝材质为聚合物，芯丝断面形状可为圆形、扁平、薄带等形状。
本发明解决其技术问题所采用的方案，具体步骤为：
(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；粗化液组成为铬酐50g/L 、200-400ml/L 硫酸：
(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5-15g/L，盐酸20-50ml/L ：
(4) 采用硝酸银和氨水溶液进行纤维表面的活化；
(5) 纤维的化学镀镍，溶液组成为：硫酸镍0.03-0.15mol/L，还原剂0.1-0.5 mol/L，络合剂0.05-0.5mol/L，滴定强碱溶液Ph值为4-7，化学镀时溶液温度为20-40℃，化学镀时间为0.5-2min；
所述还原剂为肼，胺基硼烷；
所述络合剂为醇胺、无机铵盐等。
(6) 纤维电刷镀钴-镍-磷非晶合金（或合金）
电刷镀钴-镍-磷非晶合金的溶液组成：可溶性钴盐2.5-4.5mol/L、酸0.2-1mol/L、可溶性镍盐0.5-1.5mol/L、亚磷酸或次磷酸盐0.3-1.2mol/L、 络合剂10-30 g/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；
所述的钴-镍-磷非晶合金制备工艺参数为：阳极采用石墨板，电刷镀纤维，电极相对运动速度为2-10m/min，滴定强酸溶液使镀液Ph值2-6，施镀温度为50-80℃。
电刷镀钴-镍-磷合金的溶液组成：可溶性钴盐1-3.5 mol/L、酸0.2-0.8 mol/L、可溶性镍盐0.3-1.2mol/L、亚磷酸或次磷酸盐0.2-1mol/L、 络合剂5-15g/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；
所述的钴-镍-磷合金制备工艺参数为：阳极采用石墨板，电刷镀纤维，电极相对运动速度为10-20 m/min，滴定强酸溶液使镀液Ph值3-6，施镀温度为30-60℃。
（7）钴-镍-磷催化反应器的制备
采用结构材料制造催化反应器架子，在催化器反应器架子上往复缠绕钴-镍-磷复合纤维，制成催化反应器。
本发明的优点是：
（1）选择不同规格的聚合物芯丝，可制备不同规铬和断面形状的连续钴-镍-磷催化反应器；
（2）可通过调整电刷镀工艺参数，可分别制得钴-镍-磷合金或钴-镍-磷非晶合金催化反应器；
（3）由于在电刷镀溶液中未添加光亮剂等，制备钴-镍-磷表面粗糙，可增大催化反应器的有效面积；
（4）由于采用聚合物芯丝，使复合纤维具有很好的柔软性，可很容易用于制备不同尺寸规格的催化反应器；
（5）这种催化反应器可很容易组合成更大更复杂的催化反应器。
附图说明
图1为本发明设备示意图。其中，催化反应器架子（1）、钴镍磷复合纤维（2）。
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-镍-磷合金催化反应器的生产工艺
(1) 聚合物芯丝采用聚丙烯纤维，纤维直径为0.02mm，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40g/L 、220ml/L硫酸：
(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5g/L，盐酸30ml/L ：
(4) 采用硝酸银和氨水溶液进行纤维表面的活化；
(5) 纤维的化学镀镍，溶液组成为：硫酸镍0..06 mol/L，肼0.3 mol/L，三乙醇胺0.25mol/L，滴定强碱溶液Ph值为9 ，化学镀时溶液温度为30 ℃，化学镀时间为1 min；
(6) 纤维电刷镀钴-镍-磷合金
电刷镀钴-镍-磷合金的溶液组成：可溶性钴盐1.5 mol/L、硼酸0.35 mol/L、硫酸镍0.4mol/L、亚磷酸0.35 mol/L、 醋酸钠10g/L、糖精2g/L、余量水；
所述的钴-镍-磷合金制备工艺参数为：阳极采用石墨板，电刷镀纤维，电极相对运动速度为12 m/min，滴定强酸溶液使镀液Ph值5，施镀温度为50℃。
（7）钴-镍-磷催化反应器的制备
采用钢铁制造催化反应器架子，在催化器反应器架子上往复缠绕钴-镍-磷复合纤维，制成催化反应器。
在催化反应器架子上来回缠绕钴-镍-磷复合纤维，制成催化反应器。
实施例2：钴-镍-磷非晶合金催化反应器的生产工艺
(1) 聚合物芯丝采用聚丙烯薄带，薄带断面尺寸为0.05×1 mm，采用碱性溶液，对聚合物薄带进行除油脱脂；
(2) 采用铬酐和硫酸溶液进行薄带表面的粗化；粗化液组成为铬酐60 g/L 、200ml/L硫酸：
(3) 采用酸性的锡盐溶液进行薄带的敏化；敏化液组成为氯化锡8g/L，盐酸40 ml/L ：
(4) 采用硝酸银和氨水溶液进行纤维表面的活化；
(5) 纤维的化学镀镍，溶液组成为：硫酸镍0.1mol/L，一甲基胺硼烷0.2mol/L，氯化铵0.15 mol/L，滴定氨水溶液Ph值为10，化学镀时溶液温度为25 ℃，化学镀时间为2min；
(6) 电刷镀钴-镍-磷非晶合金
电刷镀钴-镍-磷非晶合金的溶液组成：可溶性钴盐3.5 mol/L、酸0.8 mol/L、氯化镍1.2 mol/L、次磷酸盐0.8 mol/L、 醋酸钠25g/L、糖精3g/L、余量水；
所述的钴-镍-磷合金制备工艺参数为：阳极采用石墨板，电刷镀纤维，电极相对运动速度为8 m/min，滴定强酸溶液使镀液Ph值2，施镀温度为60℃。
（7）钴-镍-磷催化反应器的制备
采用铝合金制造催化反应器架子，在催化器反应器架子上往复缠绕钴-镍-磷复合纤维，制成催化反应器。
实施例3：钴-镍-磷合金催化反应器的生产工艺
(1) 聚合物芯丝采用尼龙纤维，纤维直径为0.1 mm，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55g/L 、250ml/L硫酸：
(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10g/L，盐酸35ml/L ：
(4) 采用硝酸银和氨水溶液进行纤维表面的活化；
(5) 纤维的化学镀镍，溶液组成为：硫酸镍0..08 mol/L，肼0.35 mol/L，三乙醇胺0.25mol/L，滴定强碱溶液Ph值为9 ，化学镀时溶液温度为20 ℃，化学镀时间为1 min；
(6) 纤维电刷镀钴-镍-磷合金
电刷镀钴-镍-磷合金的溶液组成：可溶性钴盐1.8 mol/L、磷酸0.4 mol/L、硫酸镍0.3mol/L、亚磷酸0.45 mol/L、 醋酸钠8 g/L、糖精2g/L、余量水；
所述的钴-镍-磷合金制备工艺参数为：阳极采用石墨板，电刷镀纤维，电极相对运动速度为12 m/min，滴定强酸溶液使镀液Ph值5，施镀温度为50℃。
（7）钴-镍-磷催化反应器的制备
采用玻璃钢制造催化反应器架子，在催化器反应器架子上往复缠绕钴-镍-磷复合纤维，制成催化反应器。

Claims (5)

1.一种钴-镍-磷催化反应器及生产方法，其特征在于，反应器由钴-镍-磷复合纤维和反应器架子组成，复合纤维长度可连续，复合纤维的断面可为圆形、扁平、薄带等形状，复合纤维的截面面积不大于2 mm2；复合纤维的包覆层为钴-镍-磷合金或非晶合金，具体成分为Co为40-85%，Ni为10-20%，P为6-20%，包覆层厚度不大于0.5mm，包覆层与芯丝之间采用化学镀镍为过渡层，复合纤维的芯丝材质为聚合物，芯丝断面形状可为圆形、扁平、薄带等形状。
2.一种钴-镍-磷催化反应器及生产方法，其生产方法特征在于，生产步骤为：（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) 纤维的化学镀镍；(6) 纤维电刷镀钴-镍-磷非晶合金（或合金）；（7）钴-镍-磷催化反应器的制备。
3. 权利要求2所述的化学镀镍的溶液组成为：硫酸镍0.03-0.15mol/L，还原剂0.1-0.5mol/L，络合剂0.05-0.5mol/L，滴定强碱溶液Ph值为4-7，化学镀时溶液温度为20-40℃，化学镀时间为0.5-2min；
所述还原剂为肼，胺基硼烷；
所述络合剂为醇胺、无机铵盐等。
4.权利要求2所述的电刷镀钴-镍-磷非晶合金的溶液组成：可溶性钴盐2.5-4.5mol/L、酸0.2-1mol/L、可溶性镍盐0.5-1.5mol/L、亚磷酸或次磷酸盐0.3-1.2mol/L、 络合剂10-30g/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；
所述的钴-镍-磷非晶合金制备工艺参数为：阳极采用石墨板，电刷镀纤维，电极相对运动速度为2-10m/min，滴定强酸溶液使镀液Ph值2-6，施镀温度为50-80℃。
5.权利要求2所述的电刷镀钴-镍-磷合金的溶液组成：可溶性钴盐1-3.5 mol/L、酸0.2-0.8 mol/L、可溶性镍盐0.3-1.2mol/L、亚磷酸或次磷酸盐0.2-1mol/L、 络合剂5-15g/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；
所述的钴-镍-磷合金的制备工艺参数为：阳极采用石墨板，电刷镀纤维，电极相对运动速度为10-20 m/min，滴定强酸溶液使镀液Ph值3-6，施镀温度为30-60℃。
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