CN101612667B - 一种表面修饰油溶性纳米铜的制备方法 - Google Patents

一种表面修饰油溶性纳米铜的制备方法 Download PDF

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CN101612667B
CN101612667B CN2009100650564A CN200910065056A CN101612667B CN 101612667 B CN101612667 B CN 101612667B CN 2009100650564 A CN2009100650564 A CN 2009100650564A CN 200910065056 A CN200910065056 A CN 200910065056A CN 101612667 B CN101612667 B CN 101612667B
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张晟卯
代闯
吕富山
吴志申
张治军
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Zhejiang Kepeier New Material Co ltd
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Henan University
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Abstract

本发明属于新型功能纳米材料制备技术领域，特别涉及一种表面修饰油溶性纳米铜的制备方法。以铜合金为原料，先加入含有修饰剂的有机溶液，然后加入可与合金金属反应的酸或碱溶液，于0-100℃的条件下充分反应6-24h，分离纯化即得所述表面修饰油溶性纳米铜。本制备方法具有工艺、设备简单、原料廉价易得、成本低，产率高等特点，适合大规模的工业生产。

Description

一种表面修饰油溶性纳米铜的制备方法
(一)技术领域
本发明属于新型功能纳米材料制备技术领域，特别涉及一种表面修饰油溶性纳米铜的制备方法。
(二)背景技术
铜纳米微粒在催化、电子、涂料、润滑等领域具有广泛的用途。文献表明，铜纳米微粒可望作为一种新型的修复型润滑添加剂用于润滑油工业。铜纳米微粒作为润滑油添加剂的前提是它在润滑油中有足够的稳定性、分散性，且其生产成本要足够低。目前，物理方法和化学方法制备铜纳米微粒都有报道。其中物理方法制备的铜纳米微粒表面洁净，适用于催化、电子等行业，但它们无法在溶剂中分散，或靠使用大量的表面活性剂将其分散于溶剂中且易沉降，无法彻底解决其分散性问题。目前所报道的化学方法即自下而上的方法-通过还原铜盐来制备纳米铜。例如，周静芳等发明了一种水醇混合体系中制备表面修饰铜纳米微粒的方法，虽然在一定程度上改善了铜纳米微粒的分散性，但尚不能彻底解决在高浓度和长时间条件下的分散性。王晓波等发明了一种基于浮选原理的铜纳米微粒的制备方法，较好的解决了其分散性问题，但存在制备过程较为复杂，且中间涉及到铜溶胶的制备。众所周知，胶体体系是热力学不稳定体系，其稳定性受到浓度等诸多因素的影响，这有可能导致其工艺不稳定且生产规模受到限制。
(三)发明内容
本发明的目的在于提供一种表面修饰油溶性纳米铜的制备方法，制得的纳米铜在有机溶剂中的单分散性好、稳定性高。
本发明采用的技术方案如下：
一种表面修饰油溶性纳米铜的制备方法，以铜合金为原料，先加入含有修饰剂的有机溶液，然后加入可与合金金属反应的酸或碱溶液，于0-100℃的条件下充分反应6-24h，分离纯化即得所述表面修饰油溶性纳米铜。
所述铜合金中铜质量含量为80-95％。
所述铜合金中的铜与修饰剂的物质的量比为1∶0.1-3。
修饰剂为烷基膦酸、烷基硫代磷酸、烷基羟肟酸、烷基水杨醛肟中的一种或两种以上的组合，所述烷基含有6-20个碳。
有机溶液的溶剂为氯仿、石油醚、甲苯、苯、液体石蜡中的一种或两种以上的组合，用量为1g合金加入80-100mL溶液。
修饰剂的有机溶液的浓度为0.03-0.10mol/L。
所述合金为CuSn合金。
使用的酸为盐酸、硫酸、硝酸、磷酸中的一种或两种以上的组合；使用的碱为氢氧化钠和/或氢氧化钾。
所用的酸或碱与Sn的物质的量比为0.6～4。
所述的分离纯化为静置，分层，分出有机溶剂层减压蒸馏即可。
本发明以铜合金为原料，将铜合金中除铜以外的其他组分在适当的条件下通过适当的化学反应去除掉，剩下的铜则生产铜纳米微粒，在形成纳米微粒的同时采用适当的修饰剂直接完成在纳米微粒表面的有机修饰，从而使得到的表面修饰铜纳米微粒具有良好的有机分散性，即油溶性。
本发明方法是基于一种自上而下的方法即从大的铜合金到纳米铜，区别于现有的多为自下而上的方法即从离子到纳米铜的方法，提供了制备纳米铜的一种新思路。本发明在体相铜变为纳米铜的同时完成原位表面修饰和从水相向有机相的转移，由于纳米铜形成的过程中，纳米铜表面包覆了一层有机修饰剂，因此制得的纳米铜在有机相中具有较好的分散性能；由于所得纳米铜颗粒粒径较小，因此能够以较高浓度稳定的停留于有机相中，具有较好的稳定性。
本制备方法具有工艺、设备简单、原料廉价易得、成本低，产率高等特点，适合大规模的工业生产。所制备出的表面修饰铜纳米微粒粒径均一，可以通过改变修饰剂的碳链长度来改变纳米微粒的粒径及形貌，调节反应温度来改变所得纳米微粒的粒径，一般较低的温度有利于形成较小的纳米颗粒；产品在空气中可以长期稳定存在，且能很好的分散于氯仿、甲苯和液体石蜡中，有广泛的工业用途。
(四)附图说明
图1为实施例1制得的O，O′-二辛基二硫代磷酸修饰的铜纳米微粒的透射电子显微镜图；
图2为实施例2制得的O，O′-二辛基二硫代磷酸修饰的铜纳米微粒的透射电子显微镜图；
图3为实施例1制得的O，O′-二辛基二硫代磷酸修饰的铜纳米微粒分散于有机溶剂中的光学照片，溶剂从右至左依次为：液体石蜡、石油醚、氯仿、二氯甲烷、甲苯、苯。
(五)具体实施方式：
以下以具体实施例来说明本发明的技术方案，但本发明的保护范围不限于此：
实施例1
向500mL单口烧瓶中加入0.91g的CuSn合金(Sn含量10％，300目)，磁力搅拌下加入2.73gO，O′-二辛基二硫代磷酸的氯仿溶液80mL，随即加入以20mL37％(wt)HCl溶于水制得的盐酸溶液80mL，室温磁力搅拌24h。停止搅拌，静置，过滤，滤液分两层，水层澄清透明，氯仿层红棕色，减压过滤后分出CHCl3层，减压蒸馏得到棕红色粘稠液体，即为O，O′-二辛基二硫代磷酸(C8DDP)修饰的铜纳米微粒，记为C8DDPCu；其透射电子显微镜图见图1，可知，所得产品粒径均匀，平均粒径约为20nm。其溶解于各种有机溶剂中的光学照片见图3(有机溶剂中的质量浓度为0.5％，静置时间为15天)，可知其在有机溶剂中有良好的分散性。
实施例2
向500mL单口烧瓶中加入0.91g的CuSn(Sn含量10％，300目)，磁力搅拌下加入2.73gO，O′-二辛基二硫代磷酸的氯仿溶液80mL，随即加入1.25mol/L的NaOH溶液80mL，20℃磁力搅拌24h。停止搅拌，减压过滤分出CHCl3层，减压蒸馏得到棕红色粘稠液体，即为O，O′-二辛基二硫代磷酸(C8DDP)修饰的铜纳米微粒，记为C8DDP-Cu。其透射电子显微镜图见图2，可知所得产品粒径均匀，平均粒径约为10nm。取所得铜纳米颗粒溶解于液体石蜡中质量浓度为1％，静置15天后无明显沉淀，稳定性好。
实施例3
向500mL单口烧瓶中加入0.91g的CuSn(Sn含量20％，300目)，磁力搅拌下加入0.37g O，O′-二辛基膦酸的甲苯溶液80mL，随即加入以20mL 37％(wt)HCl溶于水制得的盐酸溶液80mL，10℃下磁力搅拌6h。停止搅拌，减压过滤分出有机层，减压蒸馏得到棕红色粘稠液体，即为O，O′-二辛基膦酸修饰的铜纳米微粒。取所得铜纳米颗粒溶解于甲苯中浓度为0.3％，静置15天后无明显沉淀，稳定性好。
实施例4
向500mL单口烧瓶中加入0.91g的CuSn(Sn含量5％，300目)，磁力搅拌下加入6g O，O′-二辛基膦酸的苯溶液80mL，随即加入1.25mol/L的NaOH溶液80mL，40℃下磁力搅拌12h。停止搅拌，减压过滤分出有机层，减压蒸馏得到棕红色粘稠液体，即为O，O′-二辛基膦酸修饰的铜纳米微粒。取所得铜纳米颗粒溶解于二氯甲烷中浓度为0.8％，静置15天后无明显沉淀，稳定性好。
实施例5
向500mL单口烧瓶中加入0.91g的CuSn(Sn含量15％，300目)，磁力搅拌下加入7.71g 5-壬基水杨醛肟的石油醚溶液80mL，随即加入1.25mol/L的NaOH溶液80mL，30℃下室温磁力搅拌18h。停止搅拌，减压过滤分出有机层，减压蒸馏得到棕红色粘稠液体，即为5-壬基水杨醛肟修饰的铜纳米微粒。取所得铜纳米颗粒溶解于苯中浓度为1％，静置15天后无明显沉淀，稳定性好。
实施例6
向500mL单口烧瓶中加入0.91g的CuSn(Sn含量10％，300目)，磁力搅拌下加入3.85g 5-壬基水杨醛肟的氯仿溶液80mL，随即加入以20mL 37％(wt)HCl溶于水制得的盐酸溶液80mL，20℃下磁力搅拌24h。停止搅拌，减压过滤分出CHCl3层，减压蒸馏得到棕红色粘稠液体，即为5-壬基水杨醛肟修饰的铜纳米微粒。取所得铜纳米颗粒溶解于石油醚中浓度为0.5％，静置15天后无明显沉淀，稳定性好。
实施例7
向500mL单口烧瓶中加入0.91g的CuSn(Sn含量10％，300目)，磁力搅拌下加入2g辛基羟肟酸氯仿溶液80mL，随即加入以20mL 37％(wt)HCl溶于水制得的盐酸溶液80mL，室温磁力搅拌24h。停止搅拌，减压过滤分出有机层，减压蒸馏得到棕红色粘稠液体，即为辛基羟肟酸修饰的铜纳米微粒。取所得铜纳米颗粒溶解于甲苯中浓度为1％，静置15天后无明显沉淀，稳定性好。

Claims (5)

1.一种表面修饰油溶性纳米铜的制备方法，其特征在于，以铜合金为原料，先加入含有修饰剂的有机溶液，然后加入可与合金金属反应的酸或碱溶液，于0-100℃的条件下充分反应6-24h，分离纯化即得所述表面修饰油溶性纳米铜；其中，所述铜合金中铜质量含量为80-95％；修饰剂为烷基膦酸、烷基硫代磷酸、烷基羟肟酸、烷基水杨醛肟中的一种或两种以上的组合，所述烷基含有6-20个碳，所述铜合金中的铜与修饰剂的物质的量比为1∶0.1-3；有机溶液的溶剂为氯仿、石油醚、甲苯、苯、液体石蜡中的一种或两种以上的组合，用量为1g合金加入80-100mL溶液，修饰剂的有机溶液的浓度为0.03-0.10mol/L。
2.如权利要求1所述的表面修饰油溶性纳米铜的制备方法，其特征在于所述合金为CuSn合金。
3.如权利要求2所述的表面修饰油溶性纳米铜的制备方法，其特征在于使用的酸为盐酸、硫酸、硝酸、磷酸中的一种或两种以上的组合；使用的碱为氢氧化钠和/或氢氧化钾。
4.如权利要求3所述的表面修饰油溶性纳米铜的制备方法，其特征在于所用的酸或碱与Sn的物质的量比为0.6～4。
5.如权利要求1所述的表面修饰油溶性纳米铜的制备方法，其特征在于所述的分离纯化为静置，分层，分出有机溶剂层减压蒸馏即可。
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