CN113861496B - 一种聚酰亚胺/碳量子点/硫化锌量子点复合气凝胶及其制备方法 - Google Patents
一种聚酰亚胺/碳量子点/硫化锌量子点复合气凝胶及其制备方法 Download PDFInfo
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Abstract
本发明涉及一种聚酰亚胺/碳量子点/硫化锌量子点复合气凝胶及其制备方法,属于聚酰亚胺改性技术领域。制备方法为:通过水热法制备碳量子点;通过水热法制备硫化锌量子点;将碳量子点、硫化锌量子点、二酐和二胺单体在有机溶剂中混合,加入亚胺化试剂得到聚酰亚胺气凝胶前驱体;聚酰亚胺气凝胶前驱体进行老化,溶剂置换,最后超临界干燥得到复合气凝胶。本发明聚酰亚胺/碳量子点/硫化锌复合气凝胶具有较大的比表面积以及良好的光催化性能。
Description
技术领域
本发明涉及聚酰亚胺改性技术领域,尤其涉及一种聚酰亚胺/碳量子点/硫化锌量子点复合气凝胶及其制备方法。
背景技术
聚酰亚胺是主链上含有酰亚胺基团的一类聚合物。聚酰亚胺分子中含有稳定的芳杂环结构单元,具有优于其他高分子材料的耐热性能、良好的机械性能和电性能。聚酰亚胺优异的综合性能,使其在现代工业的各行各业都有广泛的应用,主要用途有柔性薄膜、涂料、先进复合材料、胶黏剂等。
近年来,无毒、低廉的具有高可见光活性和稳定的新型有机聚合物光催化剂成为当前光催化领域的研究热点。其中聚酰亚胺能够吸收可见光,引起了科学家广泛的兴趣。
文章1(“Facile green synthesis of crystalline polyimide photocatalystforhydrogen generation from water”,Chu,Journal of Materials Chemistry,2012,22,15519-15521”)公开了以三聚氰胺和均苯四甲酸二酐为原料采用固相热聚合的方法合成了聚酰亚胺,并发现其具有光催化分解水产氢活性。
文章2(“Bandgap modulation of polyimide photocatalyst for optimum H2 production activity under visible light irradiation”,Wang,Internationaljournalof hydrogen energy,2013,38,10768-10772)公开报道通过改变不同的煅烧温度得到不同聚合度的聚酰亚胺,从而研究其电子结构的变化对其光催化产氨活性的影响。随着煅烧温度的上升(250-350℃),聚合度逐渐增强,紫外-可见光吸收带边发生红移。在一系列样品中,325℃煅烧制得的样品在可见光(a>420nm)照射下,Pt作为助催化剂,10vol%甲醇水溶液中表现出最高的产氨活性。
然而,现阶段聚酰亚胺用作光催化剂时,对光的吸收效率较低,对载流子的传输效率较低,导致光生载流子的复合率高,导致光催化效率较低。
碳量子点是一类尺寸小于10nm的碳纳米材料,导电性优良,高量子产率,化学稳定性强以及量子点的特殊光电性能,成为现在的研究热点。碳量子点特有卓越的上转换性能,即以较低频率的激发光激发出较高频率的发射光,例如将可见光转换成紫外-近紫外光,使其可以被宽带隙的半导体吸收利用,提高光吸收效率。
文章3(“Preparation of carbon quantum dots/TiO2 nanotubes compositesand their visible light catalytic applications.”Pan,Journal of MaterialsChemistry A,2014,2,18082-18086”)公开报道使用简单的静电纺丝法和水热法,定向可控地制备了碳量子点/TiO2纳米复合体系,实验证明,该产物具有十分卓越的可见光催化效果,原因则主要归结于碳量子点特有的上转换效应以及可以有效的促进光生电子空穴对的产生和分离。
文章4(“Preparation and visible light photocatalytic activity ofcarbon quantum dots/TiO2 nanosheet composites."Yu,Carbon,2014,68,718-724.”)公开报道碳量子点/TiO2纳米片复合材料,研究证实碳量子点的上转换性能以及TiO2纳米片的高活性增强了复合材料的可见光催化性能。基于此,在催化领域引起了科学家的重视。
ZnS在紫外光下光分解水产氢的活性很早就被人们所熟知,其可以不需要助催化剂的存在就表现出很高的光催化活性。硫化锌优异的光催化性能取决它独特的光学性质:(1)紫外光激发下能够快速生成电子-空穴对;(2)被激发电子具有很低的负还原电位;(3)光激发下具有极强的稳定性,不易发生光腐蚀现象。但是,由于硫化锌的禁带宽度较大,只能被紫外光激发,而且电子-空穴对分离效率较低,大部分光生载流子并没有起到氧化还原的作用,这些都极大的限制了硫化锌作为光催化剂的实际应用。
发明内容
针对现有技术的不足,本发明提供了一种聚酰亚胺/碳量子点/硫化锌量子点复合气凝胶及其制备方法,本发明制备的聚酰亚胺/碳量子点/硫化锌量子点复合气凝胶具有良好的光催化性能。
本发明的技术方案如下:
一种聚酰亚胺/碳量子点/硫化锌量子点复合气凝胶的制备方法:
(1)通过水热法制备碳量子点;
(2)通过水热法制备硫化锌量子点;
(3)将碳量子点、硫化锌量子点、二酐和二胺单体在有机溶剂中混合,加入亚胺化试剂和交联剂得到聚酰亚胺气凝胶前驱体;
(4)聚酰亚胺气凝胶前驱体进行老化,溶剂置换,最后超临界干燥得到复合气凝胶。
进一步的,所述的碳量子点包括无掺杂碳量子点、氮掺杂碳量子点及氮硫掺杂碳量子点。
所述的无掺杂碳量子点利用蔗糖、聚乙烯醇、壳聚糖为原料;优选的,所述无掺杂碳量子点原料质量比为蔗糖或聚乙烯醇或壳聚糖:水=1:(10-100)。
所述的氮掺杂碳量子点利用葡萄糖和甘氨酸为原料,水热法制备;优选的,所述氮掺杂碳量子点制备原料质量比为葡萄糖:甘氨酸:水=1:(0.1-10):(10-100)。
本发明所述氮硫掺杂碳量子点采用苹果酸、乙二胺、L-半膀氨酸为原料制备;优选的,所述氮硫掺杂碳量子点制备原料质量比为苹果酸:乙二胺:L-半膀氨酸:水=1:(0.5-10):(0.1-10):(10-100)。
所述步骤(2)中水热法制备硫化锌量子点,是以醋酸锌和硫脲为反应物,物质的量比例为:1:(1-50);优选的,所述的水热法温度为120-200℃;时间为6-24h。
所述步骤(3)中二酐单体选自均苯四甲酸二酐PMDA、4,4'-联苯醚二酐ODPA、二苯甲酮四酸二酐BTDA或二苯醚四酸二酐BPDA中的任意一种。
所述二胺单体选自4,4-二氨基二苯醚(ODA)、3.4-二氨基二苯醚、对苯二胺、己二胺、2,2-双[3,5-二甲基-4-(4-氨基苯氧基)苯基]丙烷TBAPP或癸二胺中的任意一种。
所述步骤(3)中的有机溶剂选自N-甲基吡咯烷酮,二甲基甲酰胺或二甲基乙酰胺中的任意一种。
所述步骤(3)中亚胺化试剂为醋酸酐和三乙胺或吡啶。
所述步骤(4)中的聚酰亚胺酸中碳量子点:硫化锌量子点:溶剂的质量比例为(0.01-0.5):(0.01-0.5):100。
所述的交联试剂为1,3,5-苯三甲酰氯(BTC)或1,3,5-三(4-氨基苯氧基)苯或3-氨丙基三乙氧基硅烷。
所述步骤(4)中超临界干燥选自乙醇超临界干燥或二氧化碳超临界干燥;乙醇超临界条件为温度220-300℃,压强8-13MPa;二氧化碳超临界条件为温度40-80℃,压强6-12MPa。
本发明还包括通过上述方法获得的聚酰亚胺/碳量子点/硫化锌量子点复合气凝胶;所述聚酰亚胺/碳量子点/硫化锌量子点复合气凝胶为三维多孔的网状结构。
本发明与现有技术相比具有以下优点:
(1)本发明提供的聚酰亚胺/碳量子点/硫化锌量子点复合气凝胶具有较大的比表面积;
(2)本发明提供的聚酰亚胺/碳量子点/硫化锌量子点复合气凝胶具有良好的光催化性能。
附图说明
图1为PI,PI/CQDs/ZnS-0.5,PI/CQDs/ZnS-1和PI/CQDs/ZnS-3的红外光谱图;
图2为复合气凝胶放大50000倍的扫描电子显微镜照片;(a)PI,(b)PI/CQDs/ZnS-0.5,(c)PI/CQDs/ZnS-1,(d)PI/CQDs/ZnS-3;
图3为PI,PI/CQDs/ZnS-0.5,PI/CQDs/ZnS-1和PI/CQDs/ZnS-3的紫外可见光漫反射光谱图;
图4为PI,PI/CQDs/ZnS-0.5,PI/CQDs/ZnS-1和PI/CQDs/ZnS-3的荧光光谱图;
图5为光催化降解曲线图。
具体实施方式
下面结合具体实施例来进一步描述本发明,本发明的优点和特点将会随着描述而更为清楚。但实施例仅是范例性的,并不对本发明的范围构成任何限制。本领域技术人员应该理解的是,在不偏离本发明的精神和范围下可以对本发明技术方案的细节和形式进行修改或替换,但这些修改和替换均落入本发明的保护范围内。
实施例1
一种聚酰亚胺/碳量子点/硫化锌量子点复合气凝胶,通过如下方法制备:
(1)碳量子点的制备
蔗糖0.5g加入30ml水中,搅拌30min,转入50ml反应釜中,200℃5h,冷却,离心,透析,干燥。
(2)硫化锌量子点的制备:
1.6mmol醋酸锌和40mmol硫脲加入40mL去离子水中,室温下搅拌30分钟后,转入60mL的内衬聚四氟乙烯水热高压釜中,140℃下保温5小时,最后产物冷却,离心,60℃下干燥10小时。
(3)聚酰亚胺/碳量子点/硫化锌量子点复合气凝胶的制备
①聚酰亚胺/碳量子点/硫化锌量子点复合湿凝胶的制备:
将碳量子点0.073g分散于80mlNMP中,加入3gODA,溶解后加入4.31gBPDA,15分钟后,加入0.037g硫化锌量子点,加入11.07ml无水醋酸酐,搅拌均匀后,加入2.04ml三乙胺,15分钟后,加入溶有0.065gBTC的10mlNMP溶液,搅拌均与后,立刻转到模具中,15分钟成凝胶。
②聚酰亚胺/碳量子点/硫化锌量子点复合湿凝胶的老化:
待其凝胶并室温下老化1天。将老化后的凝胶浸泡在乙醇中进行溶剂置换(置换时间大约为1周,在此期间平均每天更换一次乙醇)。
③聚酰亚胺/碳量子点/硫化锌量子点复合气凝胶的制备
对上述置换后的凝胶进行二氧化碳超临界干燥,得到聚酰亚胺/碳量子点/硫化锌量子点复合气凝胶。二氧化碳超临界的条件:,压力为9.5MPa;温度40℃,干燥时间为6h。
实施例1产品命名为PI/CQDs/ZnS-0.5。
实施例2
一种聚酰亚胺/碳量子点/硫化锌量子点复合气凝胶,通过如下方法制备:
(1)碳量子点的制备
壳聚糖0.75g,加入30ml 2%冰醋酸中,搅拌30min,转入50ml反应釜中,180℃5h,冷却,离心,透析,干燥。
(2)硫化锌量子点的制备:
2.0mmol醋酸锌和40mmol硫脲加入40mL去离子水中,室温下搅拌30分钟后,转入60mL的内衬聚四氟乙烯水热高压釜中,140℃下保温5小时,最后产物冷却,离心,60℃下干燥10小时。
(3)聚酰亚胺/碳量子点/硫化锌量子点复合气凝胶的制备
①聚酰亚胺/碳量子点/硫化锌量子点复合湿凝胶的制备:
将碳量子点0.093g分散于80mlNMP中,加入4gODA,溶解后加入5.31gBPDA,15分钟后,加入0.093g硫化锌量子点,加入12.07ml无水醋酸酐,搅拌均匀后,加入3.04ml三乙胺,15分钟后,加入溶有0.085gBTC的10mlNMP溶液,搅拌均与后,立刻转到模具中,15分钟成凝胶。
②聚酰亚胺/碳量子点/硫化锌量子点复合湿凝胶的老化:
待其凝胶并室温下老化1天。将老化后的凝胶浸泡在乙醇中进行溶剂置换(置换时间大约为1周,在此期间平均每天更换一次乙醇)。
③聚酰亚胺/碳量子点/硫化锌量子点复合气凝胶的制备
对上述置换后的凝胶进行二氧化碳超临界干燥,得到聚酰亚胺/碳量子点/硫化锌量子点复合气凝胶。二氧化碳超临界的条件:压力为10.5MPa;温度45℃,干燥时间为8h。
实施例2产品命名为PI/CQDs/ZnS-1。
实施例3
一种聚酰亚胺/碳量子点/硫化锌量子点复合气凝胶,通过如下方法制备:
(1)碳量子点的制备
壳聚糖1.5g,加入35ml 2%冰醋酸中,搅拌30min,转入50ml反应釜中,160℃5h,冷却,离心,透析,干燥。
(2)硫化锌量子点的制备:
3.0mmol醋酸锌和35mmol硫脲加入40mL去离子水中,室温下搅拌30分钟后,转入60mL的内衬聚四氟乙烯水热高压釜中,160℃下保温10小时,最后产物冷却,离心,60℃下干燥10小时。
(3)聚酰亚胺/碳量子点/硫化锌量子点复合气凝胶的制备
①聚酰亚胺/碳量子点/硫化锌量子点复合湿凝胶的制备:
将碳量子点0.108g分散于80mlNMP中,加入5gODA,溶解后加入5.83gBPDA,15分钟后,加入0.324g硫化锌量子点,加入14.00ml无水醋酸酐,搅拌均匀后,加入4.03ml三乙胺,15分钟后,加入溶有0.100gBTC的15mlNMP溶液,搅拌均与后,立刻转到模具中,15分钟成凝胶。
②聚酰亚胺/碳量子点/硫化锌量子点复合湿凝胶的老化:
待其凝胶并室温下老化1天。将老化后的凝胶浸泡在乙醇中进行溶剂置换(置换时间大约为1周,在此期间平均每天更换一次乙醇)。
③聚酰亚胺/碳量子点/硫化锌量子点复合气凝胶的制备
对上述置换后的凝胶进行二氧化碳超临界干燥,得到聚酰亚胺/碳量子点/硫化锌量子点复合气凝胶。二氧化碳超临界的条件:压力为10.8MPa;温度50℃,干燥时间为10h。
实施例3产品命名为PI/CQDs/ZnS-3。
对比例1
一种聚酰亚胺气凝胶,其制备方法与实施例1的区别在于:不加入碳量子点和硫化锌量子点,直接由ODA和二酐反应制备气凝胶,具体包括如下步骤:
①聚酰亚胺湿凝胶的制备:80ml NMP加入3g ODA,4.31gBPDA,完全溶解后,搅拌15分钟,加入11.07ml无水醋酸酐,搅拌均匀后,加入2.04ml三乙胺,15分钟后,加入10ml溶有0.060gBTC的NMP,搅拌均匀后,转入模具,凝胶。
②聚酰亚胺湿凝胶的老化:待其凝胶并室温下老化1天。将老化后的凝胶浸泡在乙醇中进行溶剂置换(置换时间大约为1周,在此期间平均每天更换一次乙醇)。
③聚酰亚胺气凝胶的制备:二氧化碳超临界干燥获得聚酰亚胺气凝胶。
二氧化碳超临界的条件:压力为9.5MPa;温度40℃,干燥时间为6h。
对比例产品命名为PI。
BET测试结果:
实施例1产品比表面积为307m2/g,实施例2产品比表面积为434m2/g,实施例3产品比表面积为357m2/g,对比例1产品比表面积为249m2/g。比纯PI气凝胶相比,PI/CQDs/ZnS比表面积有了较大提高,最高可提高185m2/g。
图1给出了实施例1-3及对比例的XRD谱图,从图中可以看出纯聚酰亚胺气凝胶为无定形结构,加入量子点后,PI/CQDs/ZnS-0.5、PI/CQDs/ZnS-1以及PI/CQDs/ZnS-3中逐渐出现了ZnS的典型衍射峰,28.9°,47.6°和57.1°,且随着ZnS量子点的增加,三个衍射峰强度增大。注意到,聚酰亚胺的两个宽衍射峰变为一个宽衍射峰,主要是碳量子点加入影响了其晶体结构。
纯的聚酰亚胺气凝胶(a)和碳量子点添加1%,硫化锌量子点分别添加0.5%(b),1%(c),3%(d)的聚酰亚胺/碳量子点/硫化锌量子点复合气凝胶放大50000倍的扫描电子显微镜照片如图2所示,由图2可知,聚酰亚胺以及聚酰亚胺/碳量子点/硫化锌量子点气凝胶为三维多孔的结构;聚酰亚胺/碳量子点/硫化锌量子点气凝胶表面出现了量子点,随着量子点含量的增加,气凝胶中微粒数增多。图3给出了PI、PI/CQDs/ZnS-0.5、PI/CQDs/ZnS-1以及PI/CQDs/ZnS-3的紫外可见光漫反射光谱图。由图3可知,380nm-600nm间PI/CQDs/ZnS-0.5、PI/CQDs/ZnS-1以及PI/CQDs/ZnS-3光谱强度高于PI,说明碳量子点和硫化锌量子点的加入提高了聚酰亚胺气凝胶对可见光的吸收强度。注意到,当硫化锌量子点添加量为1%时,PI/CQDs/ZnS-1具有最大的可见光吸收强度。图4给出了PI、PI/CQDs/ZnS-0.5、PI/CQDs/ZnS-1以及PI/CQDs/ZnS-3的荧光光谱图。从图4中可以看出,PI/CQDs/ZnS-0.5、PI/CQDs/ZnS-1以及PI/CQDs/ZnS-3的荧光强度降低,表明电荷传递速率提高。由此说明,碳量子点和硫化锌量子点的加入提高了聚酰亚胺气凝胶的电荷传递速率,利于光生电子和空穴的分离。注意到,当添加量为1%时,PI/CQDs/ZnS-1具有最低的荧光强度,最快的电荷传递速率。
光催化降解曲线如图5所示,聚酰亚胺以及聚酰亚胺/碳量子点/硫化锌量子点气凝胶具有光催化性能,纯聚酰亚胺气凝胶的光催化降解后的溶液浓度为48%,光催化效率为52%,加入碳量子点/硫化锌量子点后,聚酰亚胺/碳量子点/硫化锌量子点气凝胶的光催化性能有了较大的提高,尤其是硫化锌量子点添加量为1%时,在180min后,降解效率最高,剩余浓度比为27%,光催化效率为73%,提高了21%。
Claims (13)
1.一种聚酰亚胺/碳量子点/硫化锌量子点复合气凝胶的制备方法:
(1)通过水热法制备碳量子点;
(2)通过水热法制备硫化锌量子点;
(3)将碳量子点、硫化锌量子点、二酐和二胺单体在有机溶剂中混合,加入亚胺化试剂以及交联剂得到聚酰亚胺气凝胶前驱体;
(4)聚酰亚胺气凝胶前驱体进行老化,溶剂置换,最后超临界干燥得到复合气凝胶;
所述的碳量子点包括无掺杂碳量子点、氮掺杂碳量子点及氮硫掺杂碳量子点。
2.根据权利要求1所述的制备方法,其特征在于,所述无掺杂碳量子点利用蔗糖、聚乙烯醇、壳聚糖为原料。
3.根据权利要求2所述的制备方法,其特征在于,所述无掺杂碳量子点原料质量比为蔗糖或聚乙烯醇或壳聚糖:水=1:(10-100)。
4.根据权利要求1所述的制备方法,其特征在于,所述氮掺杂碳量子点利用葡萄糖和甘氨酸为原料,水热法制备。
5.根据权利要求4所述的制备方法,其特征在于,所述氮掺杂碳量子点制备原料质量比为葡萄糖:甘氨酸:水=1:(0.1-10):(10-100)。
6.根据权利要求1所述的制备方法,其特征在于,所述氮硫掺杂碳量子点采用苹果酸、乙二胺、L-半膀氨酸为原料制备。
7.根据权利要求6所述的制备方法,其特征在于,所述氮硫掺杂碳量子点制备原料质量比为苹果酸:乙二胺:L-半膀氨酸:水=1:(0.5-10):(0.1-10):(10-100)。
8.根据权利要求1所述的制备方法,其特征在于,所述步骤(2)中水热法制备硫化锌量子点,是以醋酸锌和硫脲为反应物,物质的量比例为:1:(1-50)。
9.根据权利要求8所述的制备方法,其特征在于,所述步骤(2)中所述的水热法温度为120-200℃;时间为6-24h。
10.根据权利要求1所述的制备方法,其特征在于,所述步骤(3)中二酐单体选自均苯四甲酸二酐PMDA、4,4'-联苯醚二酐ODPA、二苯甲酮四酸二酐BTDA或二苯醚四酸二酐BPDA中的任意一种;所述二胺单体选自4,4-二氨基二苯醚(ODA)、3.4-二氨基二苯醚、对苯二胺、己二胺、2,2-双[3,5-二甲基-4-(4-氨基苯氧基)苯基]丙烷TBAPP或癸二胺中的任意一种;有机溶剂选自N-甲基吡咯烷酮,二甲基甲酰胺或二甲基乙酰胺中的任意一种;亚胺化试剂为醋酸酐和三乙胺或吡啶。
11.根据权利要求1所述的制备方法,其特征在于,所述步骤(4)中的聚酰亚胺气凝胶前驱体中碳量子点:硫化锌量子点:溶剂的质量比例为(0.01-0.5):(0.01-0.5):100;所述的交联剂为1,3,5-苯三甲酰氯(BTC)或1,3,5-三(4-氨基苯氧基)苯或3-氨丙基三乙氧基硅烷;所述步骤(4)中超临界干燥选自乙醇超临界干燥或二氧化碳超临界干燥;乙醇超临界条件为温度220-300℃,压强8-13MPa;二氧化碳超临界条件为温度40-80℃,压强6-12MPa。
12.如权利要求1-11任一项所述制备方法获得的聚酰亚胺/碳量子点/硫化锌量子点复合气凝胶。
13.如权利要求12所述聚酰亚胺/碳量子点/硫化锌量子点复合气凝胶,其特征在于,所述的复合气凝胶为三维多孔的网状结构。
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