CN108295678A - 一种污水处理膜材料及其制备方法 - Google Patents
一种污水处理膜材料及其制备方法 Download PDFInfo
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- CN108295678A CN108295678A CN201810179268.4A CN201810179268A CN108295678A CN 108295678 A CN108295678 A CN 108295678A CN 201810179268 A CN201810179268 A CN 201810179268A CN 108295678 A CN108295678 A CN 108295678A
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- C—CHEMISTRY; METALLURGY
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- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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Abstract
本发明公开了一种污水处理膜材料的制备方法,包括步骤:1)聚合型双[3‑(三乙氧基硅)丙基]胺盐的制备,2)膜材料的制备,3)碳量子点接枝膜材料,4)离子交换。本发明还公开了采用所述污水处理膜材料的制备方法制备得到的污水处理膜材料。本发明公开的污水处理膜材料机械力学性能好,具有较强的催化污水中有机物分解、吸附分离污水中重金属离子的能力,且回收分离方便易行。
Description
技术领域
本发明属于污水处理技术领域,涉及一种膜材料及其制备方法,具体地说,涉及一种污水处理膜材料及其制备方法。
背景技术
随着经济的发展及全球工业化进程的推进,环境问题日益突出,成为制约我国经济发展和社会进步的主要因素之一,其中,水污染是今年来环境污染中较为严重的污染之一,其对生态平衡及人们的身心健康造成了威胁。因此,寻求有效的污水处理技术成为当前业内亟待关注的焦点。
传统污水处理的方法主要有生物法,电解法,化学法和光催化法。生物法占地面积大,适用范围窄,效果也不理想;电解法虽然效果好于生物法,但是能源消耗大,推广困难;化学法在分解污染物的同时容易造成二次污染,无法将有机物完全转化为无毒无害的小分子,光催化法是利用光能进行物质转换的方法之一,能将有机物大分子降解为二氧化碳或其他小分子有机物以及水,其成本低、无二次污染,但其存在光量子效率和光活性较低的问题。除此以外,现有技术中的污水处理方法或多或少存在着需要昂贵的专用设备,耗能大,回收分离循环利用困难,运行费用高,特别对中小企业来说是个非常沉重的负担。
采用具有污水处理功能的膜材料来处理污水,是一种有效的污水处理方法,其成本低,回收分离容易,现有技术中的污水处理膜材料大多只是对污水起到过滤分离作用,没有催化污水中有机物分解、吸附分离重金属离子的能力,且它们机械力学性能有待进一步提高。
因此,开发一种机械力学性能更好,具有催化污水中有机物分解、吸附分离污水中重金属离子的能力的污水处理膜材料具有广泛的市场价值和应用前景。
发明内容
为了克服现有技术中的缺陷,本发明提供一种污水处理膜材料及其制备方法,该制备方法简单易行,原料易得,价格低廉,对设备要求不高,适合大规模生产;通过所述制备方法制备得到的污水处理膜材料机械力学性能更好,具有更强的催化污水中有机物分解、吸附分离污水中重金属离子的能力,且回收分离方便易行,有利于节能环保和降低成本。
为达到上述发明目的,本发明采用的技术方案是,一种污水处理膜材料的制备方法,包括如下步骤:
1)聚合型双[3-(三乙氧基硅)丙基]胺盐的制备:将4-乙烯基苄氯溶于有机溶剂中,并向其中加入双[3-(三乙氧基硅)丙基]胺,在氧气氛围下30-40℃下搅拌反应6-8小时,用乙醚洗涤产物3-5次后旋蒸除去溶剂;
2)膜材料的制备:将经过步骤1)制备得到的聚合型双[3-(三乙氧基硅)丙基]胺盐、2,4-二氨基-6-二烯丙氨基-1,3,5-三嗪、二(2-甲基-2-丙烯酸)2-羟基-1,3-丙二醇酯、纳米二氧化钛、光引发剂、乳化剂混合并超声10-15分钟,后放入模具内,在氮气或惰性气体氛围下,波长为220-250nm的紫外光下反应30-40分钟;
3)碳量子点接枝膜材料:将经过步骤2)制备得到的膜材料浸泡在70-80℃下的浓度为10mg/mL的碳量子点的水溶液中10-12小时,后取出并用水洗4-5次;
4)离子交换:将经过步骤3)制备得到的膜材料浸泡在温度为50-60℃质量分数为5-10%的二亚乙基三胺五乙酸二酐的水溶液中浸泡50-60小时,后取出再浸泡在水中10-15小时,后置于鼓风干燥箱50-60℃下烘8-12小时。
优选地,步骤1)中所述4-乙烯基苄氯、有机溶剂、双[3-(三乙氧基硅)丙基]胺的质量比为1:(5-10):1.4。
优选地,所述有机溶剂选自乙醚、乙酸乙酯、丙酮中的一种或几种。
优选地,步骤2)中所述聚合型双[3-(三乙氧基硅)丙基]胺盐、2,4-二氨基-6-二烯丙氨基-1,3,5-三嗪、二(2-甲基-2-丙烯酸)2-羟基-1,3-丙二醇酯、纳米二氧化钛、光引发剂、乳化剂的质量比为1:(1-2):1:(0.1-0.2):(0.03-0.05):(0.03-0.05);
优选地,所述光引发剂选自安息香、安息香双甲醚、安息香乙醚、安息香异丙醚、安息香丁醚、二苯甲酮、2,4-二羟基二苯甲酮中的一种或几种。
优选地,所述乳化剂选自十二烷基苯磺酸钠、聚氧丙烯聚乙烯甘油醚、壬基酚聚氧乙烯醚中的一种或几种。
优选地,所述惰性气体选自氖气、氦气、氩气中的一种或几种。
一种污水处理膜材料,采用所述污水处理膜材料的制备方法制备得到。
采用上述技术方案所产生的有益效果在于:
1)本发明提供的污水处理膜材料的制备方法,简单易行,原料易得,价格低廉,对设备要求不高,适合大规模生产。
2)本发明提供的污水处理膜材料,机械力学性能更好,抗紫外老化性能更优异,具有更强的催化污水中有机物分解、吸附分离污水中重金属离子的能力,且回收分离方便易行,有利于节能环保和降低成本。
3)本发明提供的污水处理膜材料,性能更稳定、光催化效率高、可见光响应范围宽、污水处理效果显著。
4)本发明提供的污水处理膜材料,分子链上含有三乙氧基硅结构与无机光催化剂二氧化钛的相容性和分散性好,分子链上还含有氨基结构,与碳量子点接枝,用利于碳量子点的分散及与有机聚合物膜的相容性;二氧化钛和碳量子点协同作用,能大大提高光催化效率,对有机污水处理效果更好、速率更快。
具体实施方式
为了使本技术领域人员更好地理解本发明的技术方案,并使本发明的上述特征、目的以及优点更加清晰易懂,下面结合实施例对本发明做进一步的说明。实施例仅用于说明本发明而不用于限制本发明的范围。
本发明下述实施例中所使用的所述碳量子点购自南京捷纳思新材料有限公司;其他原料来自于上海泉昕进出口贸易有限公司。
实施例1
一种污水处理膜材料的制备方法,包括如下步骤:
1)聚合型双[3-(三乙氧基硅)丙基]胺盐的制备:将4-乙烯基苄氯10g溶于乙醚50g中,并向其中加入双[3-(三乙氧基硅)丙基]胺14g,在氧气氛围下30℃下搅拌反应6小时,用乙醚洗涤产物3次后旋蒸除去溶剂;
2)膜材料的制备:将经过步骤1)制备得到的聚合型双[3-(三乙氧基硅)丙基]胺盐10g、2,4-二氨基-6-二烯丙氨基-1,3,5-三嗪10g、二(2-甲基-2-丙烯酸)2-羟基-1,3-丙二醇酯10g、纳米二氧化钛1g、安息香0.3g、十二烷基苯磺酸钠0.3g混合并超声10分钟,后放入模具内,在氮气氛围下,波长为220nm的紫外光下反应30分钟;
3)碳量子点接枝膜材料:将经过步骤2)制备得到的膜材料浸泡在70℃下的浓度为10mg/mL的碳量子点的水溶液中10小时,后取出并用水洗4次;
4)离子交换:将经过步骤3)制备得到的膜材料浸泡在温度为50℃质量分数为5%的二亚乙基三胺五乙酸二酐的水溶液中浸泡50小时,后取出再浸泡在水中10小时,后置于鼓风干燥箱50℃下烘8小时。
一种污水处理膜材料,采用所述污水处理膜材料的制备方法制备得到。
实施例2
一种污水处理膜材料的制备方法,包括如下步骤:
1)聚合型双[3-(三乙氧基硅)丙基]胺盐的制备:将4-乙烯基苄氯10g溶于乙酸乙酯65g中,并向其中加入双[3-(三乙氧基硅)丙基]胺14g,在氧气氛围下33℃下搅拌反应6.5小时,用乙醚洗涤产物4次后旋蒸除去溶剂;
2)膜材料的制备:将经过步骤1)制备得到的聚合型双[3-(三乙氧基硅)丙基]胺盐10g、2,4-二氨基-6-二烯丙氨基-1,3,5-三嗪12g、二(2-甲基-2-丙烯酸)2-羟基-1,3-丙二醇酯10g、纳米二氧化钛1.2g、安息香双甲醚0.35g、聚氧丙烯聚乙烯甘油醚0.32g混合并超声12分钟,后放入模具内,在氖气氛围下,波长为230nm的紫外光下反应33分钟;
3)碳量子点接枝膜材料:将经过步骤2)制备得到的膜材料浸泡在73℃下的浓度为10mg/mL的碳量子点的水溶液中10.5小时,后取出并用水洗5次;
4)离子交换:将经过步骤3)制备得到的膜材料浸泡在温度为53℃质量分数为7%的二亚乙基三胺五乙酸二酐的水溶液中浸泡54小时,后取出再浸泡在水中12小时,后置于鼓风干燥箱53℃下烘9小时。
一种污水处理膜材料,采用所述污水处理膜材料的制备方法制备得到。
实施例3
一种污水处理膜材料的制备方法,包括如下步骤:
1)聚合型双[3-(三乙氧基硅)丙基]胺盐的制备:将4-乙烯基苄氯10g溶于丙酮70g中,并向其中加入双[3-(三乙氧基硅)丙基]胺14g,在氧气氛围下35℃下搅拌反应7小时,用乙醚洗涤产物5次后旋蒸除去溶剂;
2)膜材料的制备:将经过步骤1)制备得到的聚合型双[3-(三乙氧基硅)丙基]胺盐10g、2,4-二氨基-6-二烯丙氨基-1,3,5-三嗪15g、二(2-甲基-2-丙烯酸)2-羟基-1,3-丙二醇酯10g、纳米二氧化钛1.5g、二苯甲酮0.4g、壬基酚聚氧乙烯醚0.4g混合并超声13分钟,后放入模具内,在氦气氛围下,波长为240nm的紫外光下反应36分钟;
3)碳量子点接枝膜材料:将经过步骤2)制备得到的膜材料浸泡在77℃下的浓度为10mg/mL的碳量子点的水溶液中11小时,后取出并用水洗4次;
4)离子交换:将经过步骤3)制备得到的膜材料浸泡在温度为56℃质量分数为8%的二亚乙基三胺五乙酸二酐的水溶液中浸泡57小时,后取出再浸泡在水中14小时,后置于鼓风干燥箱57℃下烘10小时。
一种污水处理膜材料,采用所述污水处理膜材料的制备方法制备得到。
实施例4
一种污水处理膜材料的制备方法,包括如下步骤:
1)聚合型双[3-(三乙氧基硅)丙基]胺盐的制备:将4-乙烯基苄氯10g溶于有机溶剂85g中,并向其中加入双[3-(三乙氧基硅)丙基]胺14g,在氧气氛围下37℃下搅拌反应7.5小时,用乙醚洗涤产物5次后旋蒸除去溶剂;所述有机溶剂是乙醚、乙酸乙酯、丙酮按质量比2:4:5混配而成。
2)膜材料的制备:将经过步骤1)制备得到的聚合型双[3-(三乙氧基硅)丙基]胺盐10g、2,4-二氨基-6-二烯丙氨基-1,3,5-三嗪18g、二(2-甲基-2-丙烯酸)2-羟基-1,3-丙二醇酯10g、纳米二氧化钛1.8g、光引发剂0.45g、乳化剂0.46g混合并超声14分钟,后放入模具内,在氩气氛围下,波长为245nm的紫外光下反应38分钟;所述光引发剂是安息香乙醚、2,4-二羟基二苯甲酮按质量比3:7混配而成;所述乳化剂是十二烷基苯磺酸钠、聚氧丙烯聚乙烯甘油醚、壬基酚聚氧乙烯醚按质量比1:2:4混配而成。
3)碳量子点接枝膜材料:将经过步骤2)制备得到的膜材料浸泡在78℃下的浓度为10mg/mL的碳量子点的水溶液中11.5小时,后取出并用水洗5次;
4)离子交换:将经过步骤3)制备得到的膜材料浸泡在温度为58℃质量分数为8%的二亚乙基三胺五乙酸二酐的水溶液中浸泡58小时,后取出再浸泡在水中14.5小时,后置于鼓风干燥箱58℃下烘11小时。
一种污水处理膜材料,采用所述污水处理膜材料的制备方法制备得到。
实施例5
一种污水处理膜材料的制备方法,包括如下步骤:
1)聚合型双[3-(三乙氧基硅)丙基]胺盐的制备:将4-乙烯基苄氯10g溶于乙醚100g中,并向其中加入双[3-(三乙氧基硅)丙基]胺14g,在氧气氛围下40℃下搅拌反应8小时,用乙醚洗涤产物5次后旋蒸除去溶剂;
2)膜材料的制备:将经过步骤1)制备得到的聚合型双[3-(三乙氧基硅)丙基]胺盐10g、2,4-二氨基-6-二烯丙氨基-1,3,5-三嗪20g、二(2-甲基-2-丙烯酸)2-羟基-1,3-丙二醇酯10g、纳米二氧化钛2g、安息香丁醚0.5g、十二烷基苯磺酸钠0.5g混合并超声15分钟,后放入模具内,在氮气氛围下,波长为250nm的紫外光下反应40分钟;
3)碳量子点接枝膜材料:将经过步骤2)制备得到的膜材料浸泡在80℃下的浓度为10mg/mL的碳量子点的水溶液中12小时,后取出并用水洗5次;
4)离子交换:将经过步骤3)制备得到的膜材料浸泡在温度为60℃质量分数为10%的二亚乙基三胺五乙酸二酐的水溶液中浸泡60小时,后取出再浸泡在水中15小时,后置于鼓风干燥箱60℃下烘12小时。
一种污水处理膜材料,采用所述污水处理膜材料的制备方法制备得到。
对比例
市售二氧化钛污水处理催化剂。
对上述实施例1-5以及对比例所得样品进行测试,测试结果见表1,测试方法如下:
1)染料降解率测试:染料降解率测试选择浓度为5mg/L的罗丹明B溶液。在石英试管中加入20mL罗丹明B溶液和0.05g所制备的样品,通空气搅拌,在400W紫外灯的照射下,每隔30min取一次溶液。采用紫外分光光度计测上层清夜的波长为553nm时的吸光度。染料的降解率可以通过下述方程进行计算:
R%(降解率)=(C0-Ct)/C0×100%
式中,C0是罗丹明B的起始浓度(mg/L),Ct是指在t时刻下的罗丹明B浓度。
2)分离回收率测试:将染料与样品的悬浮液过滤分离后,取固体部分、烘干。分离后样品的回收率可以通过下述方程计算:S%(分离回收率)=mt/m0×100%,式中,m0是初始投入样品的质量(mg),mt是分离烘干后剩余样品的质量。
表1实施例及对比例样品性能
染料降解率(%) | 分离回收(%) | |
实施例1 | 99.5 | 99.9 |
实施例2 | 99.7 | 100 |
实施例3 | 99.9 | 100 |
实施例4 | 100 | 100 |
实施例5 | 100 | 100 |
对比例 | 20 | 30 |
从上表可以看出,本发明实施例公开的污水处理膜材料,染料降解率99.5-100%,分离回收99.9-100%,而市售二氧化钛污水处理催化剂,染料降解率20%,分离回收30%。可见,本发明实施例公开的污水处理膜材料具有较好的污水处理效果,且分离回收方便。
以上显示和描述了本发明的基本原理和主要特征和本发明的优点。本行业的技术人员应该了解,本发明不受上述实施例的限制,上述实施例和说明书中描述的只是说明本发明的原理,在不脱离本发明精神和范围的前提下,本发明还会有各种变化和改进,这些变化和改进都落入要求保护的本发明范围内。本发明要求保护范围由所附的权利要求书及其等效物界定。
Claims (8)
1.一种污水处理膜材料的制备方法,其特征在于,包括如下步骤:
1)聚合型双[3-(三乙氧基硅)丙基]胺盐的制备:将4-乙烯基苄氯溶于有机溶剂中,并向其中加入双[3-(三乙氧基硅)丙基]胺,在氧气氛围下30-40℃下搅拌反应6-8小时,用乙醚洗涤产物3-5次后旋蒸除去溶剂;
2)膜材料的制备:将经过步骤1)制备得到的聚合型双[3-(三乙氧基硅)丙基]胺盐、2,4-二氨基-6-二烯丙氨基-1,3,5-三嗪、二(2-甲基-2-丙烯酸)2-羟基-1,3-丙二醇酯、纳米二氧化钛、光引发剂、乳化剂混合并超声10-15分钟,后放入模具内,在氮气或惰性气体氛围下,波长为220-250nm的紫外光下反应30-40分钟;
3)碳量子点接枝膜材料:将经过步骤2)制备得到的膜材料浸泡在70-80℃下的浓度为10mg/mL的碳量子点的水溶液中10-12小时,后取出并用水洗4-5次;
4)离子交换:将经过步骤3)制备得到的膜材料浸泡在温度为50-60℃质量分数为5-10%的二亚乙基三胺五乙酸二酐的水溶液中浸泡50-60小时,后取出再浸泡在水中10-15小时,后置于鼓风干燥箱50-60℃下烘8-12小时。
2.根据权利要求1所述的污水处理膜材料的制备方法,其特征在于,步骤1)中所述4-乙烯基苄氯、有机溶剂、双[3-(三乙氧基硅)丙基]胺的质量比为1:(5-10):1.4。
3.根据权利要求1所述的污水处理膜材料的制备方法,其特征在于,所述有机溶剂选自乙醚、乙酸乙酯、丙酮中的一种或几种。
4.根据权利要求1所述的污水处理膜材料的制备方法,其特征在于,步骤2)中所述聚合型双[3-(三乙氧基硅)丙基]胺盐、2,4-二氨基-6-二烯丙氨基-1,3,5-三嗪、二(2-甲基-2-丙烯酸)2-羟基-1,3-丙二醇酯、纳米二氧化钛、光引发剂、乳化剂的质量比为1:(1-2):1:(0.1-0.2):(0.03-0.05):(0.03-0.05)。
5.根据权利要求1所述的污水处理膜材料的制备方法,其特征在于,所述光引发剂选自安息香、安息香双甲醚、安息香乙醚、安息香异丙醚、安息香丁醚、二苯甲酮、2,4-二羟基二苯甲酮中的一种或几种。
6.根据权利要求1所述的污水处理膜材料的制备方法,其特征在于,所述乳化剂选自十二烷基苯磺酸钠、聚氧丙烯聚乙烯甘油醚、壬基酚聚氧乙烯醚中的一种或几种。
7.根据权利要求1所述的污水处理膜材料的制备方法,其特征在于,所述惰性气体选自氖气、氦气、氩气中的一种或几种。
8.一种采用权利要求1-7任一项所述的污水处理膜材料的制备方法制备得到的污水处理膜材料。
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