CN112517009B - 一种改性多孔铜镍合金板及其制备方法和应用 - Google Patents
一种改性多孔铜镍合金板及其制备方法和应用 Download PDFInfo
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- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 25
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Abstract
本发明公开了一种改性多孔铜镍合金板及其制备方法和应用。该改性多孔铜镍合金板的制备方法包括:将包括聚合物粘结剂、粘度调节剂、铜粉、镍粉和有机溶剂的原料混匀后将涂覆在载体板上浸入浸泡液中,浸泡液为水或者水与乙醇的混合溶液,然后将制得的多孔铜镍合金板前驱体置于依次置于氧气或空气氛围以及氢气或一氧化碳氛围下加热,最后将制得的多孔铜镍合金板置于碳源气体氛围下加热制得。本发明提出的的新型催化材料制备简单,工业普及难度低,用于VOCs处理时的降解率和降解效率均得到了大幅提高,应用时也无需提供额外的能量提供装置,此外,与本发明的改性多孔铜镍合金板配套的装置结构简单,大大拓展了催化降解法的应用前景。
Description
技术领域
本发明涉及材料领域,具体涉及一种改性多孔铜镍合金板及其制备方法和应用。
背景技术
VOCs是指一系列具有挥发性的有机化合物,由于人类日常生活的不断丰富以及工业化的不断发展,生活废气和工业废气中VOCs的排放量也越来越高。而VOCs会对人体造成一定的伤害,轻则导致眼睛、鼻子和喉咙等部分发炎疼痛,使人恶心头晕,重则会增加得癌风险,尤其是肺癌和肝癌等。
现有技术中,一般都采用吸附法、燃烧法和催化降解等方法对VOCs进行降解处理;其中,吸附方法会产生一定的具有危害性的废物;燃烧法只适合处理高浓度的VOCs,适用范围窄,设备损耗大;而催化降解法,包括光催化降解法,虽然不会产生危害性废物,且适合处理高浓度和低浓度VOCs,但其成本高,效率低,需要外加能量提供装置,配套装置复杂,工业化普及困难大;此外,现有技术中的催化材料基本都采用颗粒或粉末,无法应对大批量处理的情况,无法在工业上广泛应用。这些缺陷极大限制了催化降解法的发展。
因此,提出一种适用范围广,成本低,效率高,配套装置简单,工业普及难度低的新型催化材料将十分有意义。
发明内容
本发明的目的在于至少解决上述技术问题之一,具体技术方案如下:
一种改性多孔铜镍合金板的制备方法,包括以下步骤:
步骤一、将包括聚合物粘结剂、粘度调节剂、铜粉、镍粉和有机溶剂的原料混匀得到预混液,然后将所述预混液涂覆在载体板上,然后浸入浸泡液中,制得多孔铜镍合金板前驱体;所述浸泡液为水,或者是水和乙醇的混合溶液;所述预混液中,所述聚合物粘结剂的质量百分比为3~6%,所述粘度调节剂的质量百分比为1~2%,所述有机溶剂的质量百分比为23~37%,所述铜粉和所述镍粉的总质量百分比为58~70%;
步骤二、将所述多孔铜镍合金板前驱体置于氧气或空气氛围下加热氧化,加热氧化温度为500~700℃;然后置于氢气或一氧化碳氛围下还原烧结1~3h,还原烧结温度为650~850℃;制得多孔铜镍合金板;
步骤三、将所述多孔铜镍合金板置于碳源气体氛围下加热40s~80s,制得所述改性多孔铜镍合金板;加热温度为400~1000℃。
本发明通过将聚合物粘结剂、粘度调节剂和有机溶剂混合形成聚合物溶液,并使其与铜粉和镍粉混匀得到铜粉和镍粉均匀分散的金属粉浆,将其刮涂在载体板上后浸入浸泡液中,浸泡液会将有机溶剂置换出来,使得整个体系发生相转换,转换后的材料会固化成型,从载体板上直接脱离,形成多孔铜镍合金板前驱体;然后将多孔铜镍合金板前驱体置于氧气或空气氛围下加热,烧掉其中的聚合物的同时也将其中的铜和镍氧化为氧化铜和氧化镍,然后置于氢气或一氧化碳氛围下加热还原;设计将铜和镍一同依次经历氧化和还原的过程,会使得金属铜和金属镍形成金属互化物,从而使得制得的多孔铜镍合金板具有更好的Cu8Ni3合金相,进一步提高材料的VOCs降解性能(Cu8Ni3合金相正是发挥材料VOCs降解性能的关键);最后将多孔铜镍合金板置于碳源气体的氛围下进行多孔铜镍合金板表面碳层的原位生长,使得多孔铜镍合金板的表面原位生长碳材料,最终制得本发明的改性多孔铜镍合金板。
其中,步骤一中,所述预混液涂覆在载体板上,然后浸入浸泡液中的浸泡时间为6~12h最为适宜;步骤二中,加热氧化的时间为2~5h最为适宜。
其中,步骤三中,加热温度(即碳层原位生长温度)为400~600℃时,多孔铜镍合金板的表面原位生长无定型碳;加热温度(即碳层原位生长温度)为800~1000℃时,多孔铜镍合金板的表面原位生长石墨烯;而加热温度(即碳层原位生长温度)为其它温度值时,多孔铜镍合金板的表面原位生长碳纳米管。
本发明的改性多孔铜镍合金板是一种全新的VOCs催化降解材料,首先,铜镍合金对于VOCs确实有催化降解的作用,但其降解效率较低,而本发明首先提出将制备的多孔铜镍合金用于VOCs催化降解处理,增大VOCs与合金的接触面积,提高其催化降解效果;另一方面通过在多孔铜镍合金表面原位生长碳材料(碳材料本身就具备一定的吸附性能,能够起到一定的固定VOCs的作用)大大提高了多孔铜镍合金的催化降解效果,同时,原位生长的碳层中会负载一定数量的铜镍合金,增加催化剂的降解效果;此外,在实际应用时,在改性多孔铜镍合金板上加持5~50V的直流电流,碳材料即可产生60~180℃的温度,提供足够的能量用于进一步提高VOCs的降解处理效果,也无需传统工艺中额外的外加能量和提供外加能量的装置。为了使用方便,在实际制备时,可以将上述步骤二中的多孔铜镍合金板放置于一个衬底(例如玻璃板等)上进行碳材料的原位生长,此时可以保证碳材料只在多孔铜镍合金板暴露于碳源气体的一面进行原位生长。
优选的,所述聚合物粘结剂包括聚砜、聚醚砜、聚醚酰亚胺和聚偏氟乙烯中的至少一种。
优选的,所述粘度调节剂包括吡咯烷酮、聚乙烯吡咯烷酮、乙基纤维素和聚乙二醇中的至少一种。所述粘度调节剂用以调节聚合物溶液,使铜粉、镍粉在金属粉浆中均匀分布。
优选的,所述有机溶剂包括N-甲基吡咯烷酮、N,N-二甲基甲酰胺、N,N-二甲基乙酰胺和二甲基亚砜中的至少一种。
优选的,所述载体板包括玻璃平板和陶瓷平板中的一种。
优选的,所述铜粉的粒径为800~1200μm,所述镍粉的粒径为400~600nm。铜粉和镍粉的粒径直接影响着制得的多孔铜镍合金板的孔径、孔隙率和空气渗透率。
优选的,所述铜粉与所述镍粉的质量比为10~20:1。根据发明人不断的研究发现,在此比例下比较利于多孔结构的成型,制得的多孔铜镍合金板中Cu8Ni3合金相占比较高,而Cu8Ni3合金相正是材料中降解处理VOCs的关键。
优选的,所述预混液涂覆在所述载体板上的厚度为0.2~2mm。
优选的,步骤三的具体过程为:将所述多孔铜镍合金板置于容器内,向容器内通入惰性气体和氢气,同时在400~1000℃的条件下加热15~25min,然后通入碳源气体,继续加热40~80s。预先将多孔铜镍合金板置于惰性气体和氢气的氛围下加热,可以防止少量金属氧化物的存在影响后期碳材料的原位生长,从而影响制得的改性多孔铜镍合金板的性能。
优选的,步骤三中,所述氢气、所述惰性气体和所述碳源气体的总气体流速为50~300mL/min。流速过快会使得多孔铜镍合金板表面的碳材料层厚度过大,影响气体通过效率;流速太慢则会使得碳材料层厚度过小,可能会使得多孔铜镍合金板表面覆盖不完全。
根据将上述制备方法制得的一种改性多孔铜镍合金板在VOCs降解领域中具有较大的应用前景。
本发明的有益效果为:本发明提出的用于VOCs降解处理的新型催化降解材料制备简单,工业普及难度低,用于VOCs处理时的降解率和降解效率较高,应用时也无需额外的加热源以及配套的能量提供装置,此外,与本发明的改性多孔铜镍合金板配套的装置结构简单,大大拓展了催化降解法的应用前景。
附图说明
图1为多孔铜镍合金板前驱体截面在400μm尺寸下的SEM照片;
图2为多孔铜镍合金板前驱体表面在10μm尺寸下的SEM照片;
图3为多孔氧化铜-氧化镍合金板表面在500nm尺寸下的SEM照片;
图4为多孔铜镍合金板截面在400μm尺寸下的SEM照片;
图5为多孔铜镍合金板表面在10μm尺寸下的SEM照片;
图6为改性多孔铜镍合金板表面在1μm尺寸下的SEM照片;
图7为实施例2中的一种VOCs降解处理装置的结构示意图;
图8为采用对比例1制得的合金板作为功能板时,甲醛气体和乙酸乙酯气体的降解率结果图;
图9为采用实验组1制得的合金板作为功能板时,甲醛气体和乙酸乙酯气体的降解率结果图;
图10为采用实施例1制得的合金板作为功能板时,甲醛气体和乙酸乙酯气体的降解率结果图。
具体实施方式
以下将结合实施例对本发明的构思及产生的技术效果进行清楚、完整的描述,以充分地理解本发明的目的、方案和效果。需要说明的是,在不冲突的情况下,本申请中的实施例及实施例中的特征可以相互组合。
实施例1:
一种改性多孔铜镍合金板的制备方法,包括以下步骤:
步骤一、将聚砜、吡咯烷酮(pvp)、铜粉(粒径1000μm)、镍粉(粒径500nm)和N-甲基吡咯烷酮(NMP)混匀,形成一定粘度的金属粉浆,其中,在金属粉浆中,铜粉的质量百分比为63%,镍粉的质量百分比为5%,聚砜的质量百分比为5.12%,所述粘度调节剂的质量百分比为1.45%,所述有机溶剂的质量百分比为25.43%;然后将金属粉浆静置于真空干燥箱中抽真空4h用于除去金属粉浆中的气泡,然后将金属粉浆刮涂在玻璃平板上,厚度控制在0.2~2mm之间,然后迅速浸入水中静置8h,制得多孔铜镍合金板前驱体,其电镜(SEM)照片如图1~2所示,其中,图1为多孔铜镍合金板前驱体截面在400μm尺寸下的SEM照片;
图2为多孔铜镍合金板前驱体表面在10μm尺寸下的SEM照片;图1~2能够说明多孔铜镍合金版前驱体成型良好,铜粉和镍粉分布均匀;
步骤二、将多孔铜镍合金板前驱体置于气氛炉中,通入氧气(100mL/min),在600℃的温度下加热氧化3h,得到多孔氧化铜-氧化镍合金板,图3为多孔氧化铜-氧化镍合金板表面在500nm尺寸下的SEM照片;降至室温后,再通入氢气(20mL/min),在750℃的温度下还原烧结2h,制得多孔铜镍合金板;其SEM照片如图4~5所示,其中,图4为多孔铜镍合金板截面在400μm尺寸下的SEM照片;图5为多孔铜镍合金板表面在10μm尺寸下的SEM照片;图4~5可以说明制得的确实是多孔铜镍合金板,经过检测,多孔铜镍合金板的空气渗透率为6*10- 6mol·m-2·s-1·pa-1,孔径为40μm,孔隙率为70%;
步骤三、将制得的多孔铜镍合金板置于气氛炉中,放置在玻璃衬底上,通入氩气(100mL/min)和氢气(100mL/min),并在700℃的温度下加热20min,然后继续加热的同时通入乙炔气体(10mL/min)60s,制得表面生长有碳纳米管的多孔铜镍合金板,即改性多孔铜镍合金板,图6为改性多孔铜镍合金板表面在1μm尺寸下的SEM照片,由图6表面的碳纳米管结构可知制得的确实是表面修饰有碳纳米管的多孔铜镍合金板。
实施例2:
将实施例1中步骤三的加热温度改为500℃,其余按照与实施例1中完全相同的步骤和条件,制得表面原位生长有无定型碳的多孔铜镍合金板作为实验组1;
设置对比例1:将设有若干个贯穿孔的普通铜镍合金板作为对比例1;
将实施例1、实验组1和对比例1制得的合金板分别用于VOCs的降解处理,具体过程如下:
首先,设计一种VOCs降解处理装置,其结构如图7所示,包括反应室100,反应室100的形状为长方体,长宽高分别为(1~2m)*(0.8~1.5m)*(0.8~1.5m),反应室100的材质为不锈钢,反应室100的内部设有若干功能板500,功能板500将反应室100的内部分隔为至少两个互不连通的子腔400,反应室100具有进气口200和出气口300,功能板500位于进气口200和出气口300之间,进气口200和出气口300分别连通不同的子腔400;相邻的功能板500之间设有阻流板600,使得相邻的功能板500之间的子腔400内形成往返通道。
功能板500分别采用实施例1、实验组1和对比例1制得的合金板进行VOCs降解处理实验,步骤如下:
将甲醛气体/乙酸乙酯气体通过进气口200进行输入,经过功能板500后,由于阻流板600的存在,甲醛气体/乙酸乙酯气体会在子腔400内的行进路线是往返的,增长了其行进路径,然后由于功能板500的多层降解处理,处理后的气体从出气口300排出,对处理后的气体进行检测,计算甲醛气体/乙酸乙酯气体的降解率。
其中,功能板500为实施例1和实验组1制得的合金板时,需要在常压下,在铜镍合金板层和碳纳米管层/无定型碳层上加持直流电压,直流电压5~50V,其中正极接多孔铜镍合金层,负极接碳纳米管层/无定型碳层,此时,由于加持了电流,碳纳米管层/无定型碳层会产生60~180℃的温度,提供能量使得甲醛气体/乙酸乙酯气体依次经过多孔铜镍合金层和碳纳米管层/无定型碳层时,能够共同作用将甲醛气体/乙酸乙酯气体催化降解为二氧化碳和水。
功能板500为对比例1制得的合金板时,同样在常压下,在合金板上加持4~10V的直流电压,正极和负极均接在合金板上。由于纯铜镍合金没有碳,电阻比较低,加持过高电压会产生很高的电流,仪器短路,而直接影响降解过程的是加持电压后产生的温度,故采用对比例1制得的合金板时,只加持了4~10V,保持对比例1、实验组1和实施例1的实验过程中温度相当即可。
此外,在一些实施情况中,反应室100可设计为长度为1~10m,底面直径为0.1~0.25m的圆柱体形状,即管状,此时,可以在加压的条件下进行降解处理过程,而在现有的所有工艺中,由于催化材料为粉末/颗粒状以及大批量处理的限制,一般都需要焊接金属部件组成大型的反应室,这种焊接而成的反应室没有办法保证其气密性,没有办法实现加压处理;而此时也无需设计阻流板600增加气体行进路径从而提高降解效率。
按照上述过程,测试的结果如图8~10所示,图8中a为采用对比例1制得的合金板作为功能板500时,甲醛气体的降解率结果图,b为采用对比例1制得的合金板作为功能板500时,乙酸乙酯气体的降解率结果图;图9中a为采用实验组1制得的合金板作为功能板500时,甲醛气体的降解率结果图,b为采用实验组1制得的合金板作为功能板500时,乙酸乙酯气体的降解率结果图;图10中a为采用实施例1制得的合金板作为功能板500时,甲醛气体的降解率结果图,b为采用实施例1制得的合金板作为功能板500时,乙酸乙酯气体的降解率结果图。
由图8~10可知,本发明制得的改性多孔铜镍合金板对于VOCs的降解率能够达到98%,高于对比例1,同时本发明首次提出板材类结构用于VOCs降解处理,相比于现有技术其工业普及难度极低,应用范围更广,此外,在降解处理过程中,只需要加持5~50V的直流电压即可完成能量的提供,无需任何额外的加热源,大大节省了成本,降低了装置的损耗,本实施例提出的配套的装置也因此十分简单,生产成本低,如果采用管式结构的反应室,可在加压条件下进行VOCs的降解处理,其降解速率会大大增加。
Claims (6)
1.一种改性多孔铜镍合金板的制备方法,其特征在于,包括以下步骤:
步骤一、将包括聚合物粘结剂、粘度调节剂、铜粉、镍粉和有机溶剂的原料混匀得到预混液,然后将所述预混液涂覆在载体板上,然后浸入浸泡液中,制得多孔铜镍合金板前驱体;所述浸泡液为水,或者是水和乙醇的混合溶液;所述预混液中,所述聚合物粘结剂的质量百分比为3~6%,所述粘度调节剂的质量百分比为1~2%,所述有机溶剂的质量百分比为23~37%,所述铜粉和所述镍粉的总质量百分比为58~70%;
步骤二、将所述多孔铜镍合金板前驱体置于氧气或空气氛围下加热氧化,加热氧化温度为500~700℃;然后置于氢气或一氧化碳氛围下还原烧结1~3h,还原烧结温度为650~850℃;制得多孔铜镍合金板;
步骤三、将所述多孔铜镍合金板置于容器内,向容器内通入惰性气体和氢气,同时在400~1000℃的条件下加热15~25min,然后通入碳源气体,继续加热40~80s;
所述铜粉的粒径为800~1200μm,所述镍粉的粒径为400~600nm;
所述铜粉与所述镍粉的质量比为10~20:1;
所述氢气、所述惰性气体和所述碳源气体的总气体流速为50~300mL/min。
2.根据权利要求1所述的制备方法,其特征在于,所述聚合物粘结剂包括聚砜、聚醚砜、聚醚酰亚胺和聚偏氟乙烯中的至少一种。
3.根据权利要求1所述的制备方法,其特征在于,所述粘度调节剂包括吡咯烷酮、聚乙烯吡咯烷酮、乙基纤维素和聚乙二醇中的至少一种。
4.根据权利要求1所述的制备方法,其特征在于,所述有机溶剂包括N-甲基吡咯烷酮、N,N-二甲基甲酰胺、N,N-二甲基乙酰胺和二甲基亚砜中的至少一种。
5.一种改性多孔铜镍合金板,其特征在于,由权利要求1至4任一项所述的制备方法制得。
6.权利要求5所述的一种改性多孔铜镍合金板在VOCs降解领域中的应用。
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