CN108889264A - 一种吸附分解甲醛的泡沫铜的制备方法 - Google Patents
一种吸附分解甲醛的泡沫铜的制备方法 Download PDFInfo
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Abstract
本发明是一种吸附分解甲醛的泡沫铜的制备方法,采用泡沫铜为原料,浸泡氧化剂溶液、沥干、烘干氧化,或者直接将泡沫铜加温氧化,在泡沫铜内外表面形成一层均匀的氧化膜,通过的气流就会与泡沫铜不规则的通孔内表面充分碰撞,提高气体中甲醛与泡沫铜表面的铜氧化物发生接触吸附、氧化还原反应而降解的概率,泡沫铜基材又具有良好的力学强度,可以直接制作空气过滤组件,是一种理想的吸附、降解空气中甲醛的过滤材料,满足不同需求,适合规模化生产。
Description
技术领域
本发明所公开的是一种吸附分解甲醛的泡沫铜的制备方法,特别是指可以用于吸附、反应和催化分解空气中甲醛的泡沫铜的制备方法,属于新型材料技术范畴。
背景技术
泡沫铜是一种成熟的产品,具有优良的导热性能、导电性能、高比表面积、高孔隙率,广泛用于电子元器件的导热散热、镍锌电池及双电层电容器的电极材料、过滤材料和吸音材料。也有利用泡沫铜作为载体,覆载纳米二氧化钛作为光催化材料。
纳米材料虽然具有优异特性,但对人类健康和环境安全,也可能存在潜在的危害。马萨诸塞州大学的研究者认为,一方面,纳米颗粒非常小,以至于可以穿透细胞膜和屏障,进入细胞内部;另一方面,纳米颗粒又足够大,以至于可以干扰细胞内聚集态的结构,从而影响生化反应和细胞的正常生长。据2008年3月英国《新科学家》杂志报道,纳米材料、转基因农作物、人造病毒和仿生机器人等25个因素将严重威胁未来的地球环境,其中纳米材料引起的污染和对健康威胁的问题排在第一位。因此,在没有足够的证据证明所采用的纳米组分——纳米氧化钛或其他氧化物的纳米粒子对人类健康和环境的安全不构成威胁之前,对应用于制备空气过滤器等关乎人身健康的产品的复合纳米粒子——通过涂敷、覆载而可能容易脱落进入空气的纳米氧化物,应该采取一定的保守态度。
目前针对除去空气中甲醛的材料,主要是采用高比表面积的吸附材料、以及可以分解甲醛的含有金红石或锐钛矿型的纳米二氧化钛的光触媒材料、吸附银离子和铜离子的活性碳或活性碳纤维毡,涂敷纳米二氧化钛的光触媒材料存在纳米颗粒脱落的负面因素,吸附银离子、铜离子的活性碳或活性碳纤维毡需要与其他材料复合以增加力学性能,自身无法直接制成空气过滤构件。
氧化亚铜、氧化铜均有吸附空气中的甲醛、直接与甲醛发生氧化还原反应、催化空气中的氧与甲醛反应而分解空气中的甲醛的性能,泡沫铜本身具有很大的比表面积,有良好的空隙率和通透性,与铜网相比直通的通孔比例较低。如果在泡沫铜内、外表面形成结合良好的氧化层,如氧化亚铜、氧化铜或二者的混合氧化物的氧化层,通过的气流就会与泡沫铜不规则的通孔内表面充分碰撞,气体中甲醛与泡沫铜表面的氧化铜和氧化亚铜发生接触吸附、直接发生氧化还原反应或被催化与空气中的氧反应而降解的概率就得以大幅提高,泡沫铜基材又具有良好的力学强度,可以直接制作空气过滤组件,是一种理想的吸附、降解空气中甲醛的过滤材料。
目前市场上销售的泡沫铜产品主要有两大类,一种是电沉积法生产的泡沫铜,以聚氨酯泡沫为基体,经预氧化处理聚氨酯泡沫、氯化亚锡敏化、化学沉积、电沉积和焚烧除去聚氨酯泡沫骨架,然后通氢气热还原工艺制备的泡沫铜,具有均匀分布三维网状孔结构、高空隙率(>95%)、高通透性且具有一定拉伸强度;另一种是烧结法泡沫铜,以铜粉和NaCl颗粒为原材料,采用烧结-脱溶技术制备通孔泡沫铜的方法,将NaCl颗粒与电解铜粉以及添加剂混合均匀后压制得生坯,在烧结炉中置于氩气气氛下烧结,得到的物品置于循环热水装置中将NaCl颗粒溶除,再用超声波水浴中洗涤和丙酮清洗,最后烘干制成,有三维相互连通的空间网络构成的开孔、孔隙率为50~81%、平均孔径为0.2~4mm,通透性相对较低。这些泡沫铜金属表面只有极少量因接触空气氧化而造成的氧化物,不具备对甲醛有良好的吸附、反应和催化氧化功能的氧化层;为解决上述问题,特完成本发明。
发明内容
本发明要解决的技术问题是,在泡沫铜内外表面形成结合良好的氧化层,氧化层可以是氧化亚铜、氧化铜或二者的混合氧化物,使其在空气通过时,具有吸附甲醛、直接与甲醛氧化还原反应、或催化空气中的氧与甲醛反应而净化空气的性能;并且不损害泡沫铜的力学强度,便于直接用于制作空气过滤组件;所形成的氧化层与泡沫铜基体结合紧密,在过滤空气过程中不至于脱落而形成纳米污染。
为解决这个技术问题,本发明的技术构思为:
方案一:将泡沫铜用氧化剂溶液浸泡,然后取出沥干,使其表面残留部分氧化剂溶液,进入烘箱控制合适的升温速度,到一定温度后恒温一定时间,促使氧化剂将泡沫铜内、外表面氧化,形成均匀的氧化膜。
这种方案,采用的氧化剂在加工之后,必须保证无残留,避免对产品的性能造成影响,可以选用的氧化剂有过氧化氢、硝酸、硫酸和过硫酸氨等,由于硝酸、硫酸会对设备产生腐蚀和造成环境污染,最适合的氧化剂溶液应该是过氧化氢和过硫酸氨。
过氧化氢或过硫酸铵的浓度以不低于5wt%为宜,浓度太低氧化能力弱,浸泡时间长,影响生产效率。
方案二:直接将泡沫铜在电阻炉中缓慢升温至一定温度,利用空气中的氧在加热条件下将泡沫铜的内外表面氧化成氧化亚铜形成氧化层,也可以实现。
这种方案,在制备过程中,温度较高,需要450~500℃,升温、恒温、冷却整个过程时间较长,需要7~8小时,对于空隙率高的泡沫铜,如ppi(Pores Per Linear Inch,孔隙密度:单位英寸长度上的平均孔数。)大于80的泡沫铜,高温氧化对导致其力学强度明显下降;但是整个工艺无污染,无药剂消耗。
所采用的泡沫铜,可以直接从市场上直接采购的高温通氢气还原退火之后的产品,也可以是未脱除聚氨酯泡沫骨架的电解沉积金属铜之后的“泡沫铜”,为加以区分,称之为“含有聚氨酯骨架的泡沫铜”。对于应用于吸附分解空气中甲醛的体系,泡沫铜内部存在的聚氨酯骨架并不影响其功能,可以省去常规泡沫铜制备过程中的焚烧除去聚氨酯泡沫骨架及通氢气热还原这两道工艺环节,节省成本;但是这种含有聚氨酯骨架的泡沫铜,在表面形成均匀氧化膜的处理工艺中,只能采用氧化剂溶液浸泡加烘干处理方案;否则,高温会导致聚氨酯骨架分解,产生的气体物质会导致结构丧失力学性能。
金属铜直接接触的表面,所形成的氧化物多为氧化亚铜,外层由于与空气中的水分和二氧化碳、氧气接触,会继续氧化现场Cu2(OH)2CO3(一般的铜绿),但不影响其吸附、氧化、催化氧化甲醛的功能。
综上所述,本发明的核心技术是:
提供一种吸附分解甲醛的泡沫铜的制备方法,包括以下步骤:
(1).将干净的泡沫铜用浓度不低于5wt%过氧化氢溶液或过硫酸铵溶液浸泡,取出后沥干,进入烘箱烘干;烘干温度不大于180℃,达到温度后,恒温1~3小时,自然冷却至室温;
(2).直接将市场采购的泡沫铜置于电阻炉中,升温至450~500℃,恒温1~3小时,自然冷却至室温。
本发明的优点和效果是:
以氧化剂溶液浸泡、沥干、烘箱恒温烘干方式,将泡沫铜内、外表面氧化,形成均匀的氧化膜泡沫铜,或直接将市场采购的泡沫铜升温氧化制备均匀的氧化膜泡沫铜,工艺简洁、无污染,保持泡沫铜的力学性能,赋予泡沫铜具有吸附、直接氧化还原反应、催化空气中的氧与甲醛反应而分解甲醛的性能,是一种良好的吸附、降解空气中甲醛的空气过滤材料。
附图说明
附图1:实施例1制备的一种催化分解甲醛的泡沫铜的俄歇电子能谱图。
具体实施方式
下面结合具体实施例和附图对本发明作进一步描述:
实施例1.取3块干净的100mmx100mm厚度2mm空隙密度为95ppi泡沫铜,用10wt%的过氧化氢溶液浸泡10分钟,然后取出斜靠于干净搪瓷盘中,沥干,置于烘箱中,设定30分钟升温至180℃,恒温2小时,自然冷却至室温;一块用于做光电子能谱(XPS)分析,采用VGScientific ESCALab220i-XL型光电子能谱仪,激发源为AlKαX射线,功率约300W,激发能量1486.6eV,电子结合能用碳的C1s峰(284.6eV)校正;另外两块用于做吸附分解甲醛效果分析,以未经处理的100mmx100mm厚度2mm空隙密度为95ppi泡沫铜原样做对比。
实施例2.取2块干净的100mmx100mm厚度5mm空隙密度为85ppi泡沫铜,用5wt%的过硫酸铵溶液浸泡15分钟,然后取出斜靠于干净搪瓷盘中,沥干,置于烘箱中,设定30分钟升温至150℃,恒温3小时,自然冷却至室温;用于做吸附分解甲醛效果分析,以未经处理的100mmx100mm厚度5mm空隙密度为85ppi泡沫铜原样做对比。
实施例3.取3块干净的100mmx100mm厚度5mm空隙密度为110ppi含有聚氨酯骨架的泡沫铜(从生产厂家订购),用10wt%的过氧化氢溶液浸泡3分钟,然后取出斜靠于干净搪瓷盘中,沥干,置于烘箱中,设定30分钟升温至150℃,恒温2小时,自然冷却至室温;用于做吸附分解甲醛效果分析,以未经处理的100mmx100mm厚度5mm空隙密度为110ppi含有聚氨酯骨架的泡沫铜原样做对比。
实施例4.取3块干净的100mmx100mm厚度4mm空隙密度为85ppi泡沫铜,置于马弗炉中,设定60分钟升温至450度,恒温3小时,自然冷却至室温;用于做吸附分解甲醛效果分析,以未经处理的100mmx100mm厚度4mm空隙密度为85ppi泡沫铜原样做对比。
所制备的样品的吸附分解甲醛的性能评价方法:
用有机玻璃制备一个1000mm(长)x 1000mm(宽)x 800mm(高)的透明容器,上面靠一侧有一个300mm x 300mm的开口,开口周边包覆硅橡胶条,用盖子压上可以保证密闭;在容器内离底部200mm处(用300mm x 200mm x 200mm有机玻璃盒子垫起),居中放置一个内尺寸为200mm x 105mm x 105mm的有机玻璃方管,方管的一端口内放置一个5W的直流风扇(电压12V,转速3300rpm),管壁与风扇之间的缝隙用硅橡胶胶条封严;方管的另一端口内,放置检测用的泡沫铜100mm x100mm样块,用尺寸与方管匹配的有机玻璃卡子固定,与管壁之间的间隙用硅橡胶条密合,避免从间隙漏气;离容器顶板200mm处,居中放置甲醛传感器。电源线及信号线引出口均用橡胶卡座密封。
在放置测试样或对照样评价之前,先将甲醛滴入一个蒸发皿中,置于容器底部,盖紧盖子,让风机运行30min,待传感器中甲醛浓度数值基本不变时,停止风机;打开盖子,迅速将准备好的样品或对照样置于方管一段,盖紧盖子,静置3分钟左右,甲醛浓度读数基本稳定时,读取甲醛初始浓度C0,开启风机循环30min,读取甲醛最终浓度Ct;结果列于表(1)。
从表(1)的结果中可以看出,经过氧化处理后的泡沫铜,与未经处理的原样相比,具有显著的去甲醛效果;而且,空隙密度高、厚度大的泡沫铜除甲醛效果更为明显,与其比表面积大小成正相关。
为了确认氧化处理后泡沫铜表面铜的价态,对实施例1的样品进行XPS分析,由于Cu(0)和Cu(I)的Cu2P3/2的结合能(binding energy)分别为933.4和933.6eV,非常接近,而且峰形相似,在XPS谱上很难分辩;但它们的俄歇电子峰分别为918.3和916.5eV,可以采用相应的俄歇(Auger)电子的动能谱来区分:
α=Eb+Ek (1)
其中:Eb为结合能(eV),Ek为俄歇电子动能(eV),α为校正后的俄歇参数,为1448eV。
如图1所示,从俄歇电子谱中可以看出,金属Cu(0)和Cu2O的俄歇电子峰分别对应于918.3和916.5eV,泡沫铜表面基本上是氧化亚铜Cu(I),与预测的一致。由于XPS的表面探测深度一般只有3nm,最多不超过5nm,因此可以断定经氧化处理后的泡沫铜表面有比较均匀的氧化亚铜氧化膜存在,如此厚度的氧化膜,出现纳米颗粒脱落的概率很低,不会出现纳米污染现象。
应当指出,以上所述具体实施方式可以使本领域的技术人员更全面地理解本发明,但不以任何方式限制本发明。因此,尽管本说明书和实施例对本发明已进行了详细的说明,但是,本领域技术人员应当理解,仍然可以对本发明进行修改或者等同替换;而一切不脱离本发明的精神和范围的技术方案及其改进,其均应涵盖在本发明专利的保护范围当中。
表1.不同实施例和对照样的吸附分解甲醛测试结果
Claims (1)
1.一种吸附分解甲醛的泡沫铜的制备方法,其特征在于:(a)将干净的泡沫铜用浓度不低于5wt%的氧化剂溶液浸泡,取出后沥干,进入烘箱烘干,温度不大于180℃恒温1~3小时,冷却;(b)将泡沫铜置于电阻炉中,升温至450~500℃,恒温1~3小时,冷却;其中:
(1)、所述的氧化剂溶液是浓度以不低于5wt%过氧化氢溶液或过硫酸铵溶液的一种。
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CN112604689B (zh) * | 2020-11-25 | 2022-03-15 | 电子科技大学 | 一种用于催化甲醛分解的多孔氧化铜骨架催化剂制备 |
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