CN106687416B - 用于电解氯化工艺的电极和其制造方法 - Google Patents
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Abstract
本发明涉及甚至在低温下仍适用于氯化钠稀溶液的电解处理的电极。该电极可用于在海洋压载水中产生活性氯基杀生物剂。电极具有钛基材,含有钽、钌和铱的氧化物的内催化涂层,以及含有钛、钌和镍、铁和钴中的至少一种的氧化物的外催化涂层。
Description
技术领域
本发明涉及适用于电解氯化电解槽的电极,例如用于海洋应用的压舱水的杀生物处理的电解槽。
发明背景
海水的电解或随活性氯产生而来的氯化钠的其它稀的水溶液,即次氯酸盐和其它氧化物质的混合物在工业中发现若干用途,其利用该产物的杀生物和消毒的性能。特别感兴趣的应用是在航海领域中使用的压载水的杀生物剂处理。其实如所知的,当船舶在港口被置换或在加载和卸载的操作过程中时在船舶上执行的压载和平衡程序,对存储在专用隔间中的海水的量进行,相应地排空或填充该隔间。为了避免来自不同环境的生物物种污染排放区域,强制性进行待排放水的预防杀菌处理,特别是消除所有种类的微生物。已知基于贵金属氧化物涂覆的钛基材的阳极制剂适用于从氯化钠产生活性氯;然而,在低氯化钠浓度,特别是在低温下(如同海水的情形)操作电解质时,已知的制剂的一般特征是差的选择性和效率。在未分离的电解氯化电解槽中活性氯的阳极产生(典型是电解氯化过程)还受到与局部碱度增加有关的氢的阴极产生的抗衡,这有利于阴极表面的快速结垢。在这一方面,通常用盐酸进行阴极的周期性洗涤;这样的过程带来了一些安全和环境问题。一种替代的方案由如下构成:相同制剂的两个电极之间进行电解,通过周期性地反转所施加的极性交替地将一个作为阳极操作,另一个作为阴极,并反之亦然:以这种方式,在后续阳极工作诱导的局部酸化的作用下获得了结垢阴极的自清洁效果。然而,现有技术的贵金属氧化物涂覆的钛阳极具有在阴极工作期间得到失活的倾向,因而不利地影响该技术的总成本。
因而,将期望提供克服现有技术的缺点的适合用于电解氯化电解槽的电极。
特别地,将提供即使在低温下仍在从氯化钠稀溶液产生活性氯中具有良好的选择性的电极,其即使受到其极性的周期性反转仍具有对于工业应用的合适的持续时间。
发明内容
在所附的权利要求中阐述本发明的各方面。
在一个方面,本发明涉及适用于电解氯化电解槽的电极,其包含:钛基材,施加于基材的含有钽、钌和铱的氧化物的混合物的第一内催化涂层,含有选自镍、铁和钴的至少一种元素和钛、钌的氧化物的混合物的附加外催化涂层。钛基材可以包含任选合金化的钛金属的固体片材或多孔结构(如穿孔的片材、板网或网状物)。在一个实施方案中,钛基材具有4-10μm的平均粗糙度值Ra,以便有利于催化涂层的优化锚固;可以通过在受控冶金条件下选择性蚀刻钛基材的晶界来获得此粗糙外形:这在宽范围的特定负载下可以有利于涂覆层的锚固,特别是关于与基材表面直接接触的内催化涂层。可以通过用轮廓曲线仪测量来控制所获得的粗糙外形,如本领域中公知的。在一个实施方案中,在内催化涂层中的总贵金属负载量表示为1至5g/m2的钌和铱的总和。这可具有如下优点:在整个电极的寿命周期中使贵金属利用最大化,对于给定的所施加贵金属负载使电极的特定持续时间最大化,如在广泛的测试运动周期(campaign)中观察到的那样。在一个实施方案中,外催化涂层的重量组成含有30-60%的Ru、35-70%的Ti、以及1-8%的Fe、Co和Ni的总和。已经证明在此范围内的制剂对于平衡电极的催化活性、其选择性和其工作寿命是优化的,尤其是用稀释的电解质(例如用浓度低于20克/升的NaCl)工作时,即使在低温下,例如低于20℃也是如此。为了确保在电解氯化电解槽中的优化工作的目的,也可以优选将贵金属分布在催化涂料的制剂中,使得它主要集中在最外层。对于给定的电极的成本,这可以具有在催化活性和耐久性方面提供更好性能的优点。在一个实施方案中,在外催化涂层中的钌含量与在内催化涂层中的表示为钌和铱中的总和的贵金属含量的重量比因此在3至10之间。
在另一个方面,本发明涉及一种用于制造如上所述的电极的方法,包括以下的顺序步骤:在酸性溶液中蚀刻钛基材以对其赋予受控的粗糙度外形,该外形通过轮廓曲线仪检测可核查;对蚀刻基材施加钽,钌和铱化合物的溶液,在高于400℃的温度下随后热分解和形成内催化涂层;向内催化涂层施加钛、钌和至少一种选自镍,铁和钴的元素的化合物的溶液;在高于400℃的温度下随后热分解,直至形成外催化涂层。在一个实施方案中,在80-90℃下在20-30重量%的硫酸中进行蚀刻步骤持续足以对基材赋予150-250g/m2的重量损失的时间。这可具有如下优点:在晶界处使钛基材的溶解局部化,有利于以更宽的特定负载的范围锚定催化涂层。
在另一个方面,本发明涉及一种用于氯化钠水溶液的杀生物处理的方法,例如用于海洋应用的压载水,其包括:在配有一对或多对如前文所述电极的电解槽中电解至少一部分溶液,且产生活性氯。在一个实施方案中,该方法包括电极极性的周期性反转。
包括下列实施例以说明本发明的特定实施方案,其实用性已在所要求保护的数值范围内得到很大程度的验证。本领域技术人员应该理解,在下面的实施例中公开的组合物和技术代表了发明人发现的在本发明的实践中很好地起作用的组合物和技术;然而,鉴于本公开内容,本领域技术人员应该理解,可以在所公开的具体实施方案中进行许多改变且仍然获得相同或类似的结果,而不脱离本发明的范围。
实施例1
在87℃下,在27重量%的H2SO4中,在15分钟的周期中对具有0.5m2的总面积的钛品级1的1mm厚的固体片材蚀刻持续总共五个循环,直到观察到175.5g/m2的重量损耗。所得到的粗糙度外形的特征在于位于晶界处的谷,如SEM调查所显示的,且发现平均粗糙度值Ra为8.6和10微米之间,如通过在表面的不同点的测量用轮廓曲线仪所测定的。由此获得的基材细分为130mm×110mm的样本。根据各种制剂提供具有催化涂层的不同样品,在表1中报告了其最显著的设置。对于所有报告的样品中,通过如下方式沉积内催化涂层:以5个涂次施加用盐酸酸化的RuCl3、H2lrCl6和TaCl5的水溶液,在50℃下中间干燥5分钟,且在每个涂次之后在480℃热分解15分钟。用相同的工序以多个(25-40)涂次沉积外催化涂层,在RuCl3、TiCl3、Fe(NO3)3、NiCl2和CoCl2之间选择相应的盐酸酸化的水溶液的前体。
实施例2
在85℃的温度和pH 2下,将实施例1的样品进行电解(electrodic)活性的标准测试,作为通过在220克/升NaCl中的频率响应分析(FRA)校正的电位的量度。结果发现所有样品对析氯是活性的,而阳极电势在1000A/m2下为1.35和1.36V之间。
在15℃的温度和1200A/m2的电流密度下,在17克/升的NaCl中对相同的样品进行标准感应电流效率测试。
样品A1、A2、A3、A4、A5和A6都显示了86和87%之间的效率,相比之下,样品C1为81.8%的值和样品C2为83.6%。
还使用标准加速试验测量了相同样品的持续时间的特性,在15℃的温度和2500A/m2的电流密度下在17克/升的NaCl中提供了它们的操作,始于阳极工作,每12小时反转极性。当其阳极电位比初始阳极电位高1伏时,认为电极是失活的。
编号为A1至A6样品显示了1200小时(样品A4)和1500小时(A3)之间的持续时间,而样品C1和C2分别显示了500和460小时的持续时间。
前面的说明不应视为限制本发明,其可根据不同的实施方案来使用而不脱离其范围,并且其程度仅通过所附的权利要求书来进行限定。
贯穿本申请的说明书和权利要求书,术语“包含(comprise)”及其变体例如“包括(comprising)”和“含有(comprises)”并不意欲排除其它元素、部件或额外的工艺步骤的存在。
仅出于提供本发明的上下文的目的在本申请文件中包含了文件、条例、材料、设备、制品等的讨论。这并没有暗示或代表任何或所有这些内容形成现有技术基础的一部分,或是在本申请的每个权利要求的优先权日前与本发明相关领域的普通常识。
Claims (10)
1.用于电解氯化的电解槽的电极,包含:
-钛基材
-施加到所述基材上的内催化涂层,其含钽、钌和铱的氧化物的混合物
-施加在所述内催化涂层顶部上的外催化涂层,其含有选自镍、铁和钴的至少一种元素和钛、钌的氧化物的混合物。
2.根据权利要求1所述的电极,其中所述钛基材具有4至10微米的平均粗糙度Ra的值。
3.根据权利要求1或2所述的电极,其中所述内催化涂层具有表示为钌和铱的总和的1至5g/m2的贵金属总负载。
4.根据权利要求1或2所述的电极,其中所述外催化涂层的重量组成包含30-60%的Ru、35-70%的Ti和1-8%的Fe、Co和Ni的总和。
5.根据权利要求1或2所述的电极,其中在所述外催化涂层中的钌含量与在所述内催化涂层中的以钌和铱的总和表示的贵金属含量的重量比为3至10。
6.生产根据权利要求1至5中任一项所述的电极的方法,包括以下顺序的步骤:
-在酸性溶液中蚀刻钛基材直到赋予受控的粗糙度外形;
-对蚀刻的基材施加钽、钌和铱的化合物的溶液,随后在高于400℃的温度下热分解和形成内催化涂层;
-向内催化涂层施加钛、钌和选自镍、铁和钴的至少一种元素的化合物的溶液,随后在高于400℃的温度下热分解且形成外催化涂层。
7.根据权利要求6所述的方法,其中所述酸性溶液包含20-30重量%的硫酸,且在80-90℃下进行所述蚀刻步骤直到获得150-250g/m2的所述基材的重量损失。
8.对氯化钠水溶液的杀生物处理的方法,包括:在配有根据权利要求1至5中任一项所述的一对电极的电解槽中电解溶液,形成活性氯。
9.根据权利要求8所述的方法,还包括所述对的电极的极性的周期性反转。
10.根据权利要求8或9所述的方法,其中所述氯化钠水溶液为用于海洋应用的压载水。
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PCT/EP2015/074609 WO2016066544A1 (en) | 2014-10-27 | 2015-10-23 | Electrode for electrochlorination processes and method of manufacturing thereof |
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WO2018147725A1 (en) * | 2017-02-07 | 2018-08-16 | Bright Spark B.V. | Device comprising a channel, a cathode, an anode and a power source, and method for the production of chlorine dioxide |
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RU2712545C2 (ru) | 2020-01-29 |
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CA2958328A1 (en) | 2016-05-06 |
RU2017118339A3 (zh) | 2019-03-20 |
KR20170077176A (ko) | 2017-07-05 |
CN106687416A (zh) | 2017-05-17 |
PH12017500512B1 (en) | 2017-08-07 |
PH12017500512A1 (en) | 2017-08-07 |
WO2016066544A1 (en) | 2016-05-06 |
MX2017005361A (es) | 2017-08-15 |
SG11201701888VA (en) | 2017-05-30 |
CA2958328C (en) | 2022-05-31 |
AU2015340814A1 (en) | 2017-03-09 |
RU2017118339A (ru) | 2018-11-29 |
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IL250589B (en) | 2019-09-26 |
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