CN114797757A - 一种超疏水纳米材料的制备方法与应用 - Google Patents
一种超疏水纳米材料的制备方法与应用 Download PDFInfo
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- 239000002086 nanomaterial Substances 0.000 title claims abstract description 27
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 32
- 238000002156 mixing Methods 0.000 claims abstract description 27
- 238000003756 stirring Methods 0.000 claims abstract description 24
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 18
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 18
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 16
- 239000002893 slag Substances 0.000 claims abstract description 16
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 14
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- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000011863 silicon-based powder Substances 0.000 claims abstract description 12
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 9
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- 238000000576 coating method Methods 0.000 claims abstract description 7
- 239000007822 coupling agent Substances 0.000 claims abstract description 7
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims abstract description 6
- 230000032683 aging Effects 0.000 claims abstract description 6
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- RLQWHDODQVOVKU-UHFFFAOYSA-N tetrapotassium;silicate Chemical compound [K+].[K+].[K+].[K+].[O-][Si]([O-])([O-])[O-] RLQWHDODQVOVKU-UHFFFAOYSA-N 0.000 claims abstract description 3
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- 235000019353 potassium silicate Nutrition 0.000 claims description 8
- 229910001385 heavy metal Inorganic materials 0.000 claims description 7
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 6
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims description 6
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- FWDBOZPQNFPOLF-UHFFFAOYSA-N ethenyl(triethoxy)silane Chemical compound CCO[Si](OCC)(OCC)C=C FWDBOZPQNFPOLF-UHFFFAOYSA-N 0.000 claims description 4
- NKSJNEHGWDZZQF-UHFFFAOYSA-N ethenyl(trimethoxy)silane Chemical compound CO[Si](OC)(OC)C=C NKSJNEHGWDZZQF-UHFFFAOYSA-N 0.000 claims description 4
- 239000002351 wastewater Substances 0.000 claims description 4
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 claims description 3
- XDLMVUHYZWKMMD-UHFFFAOYSA-N 3-trimethoxysilylpropyl 2-methylprop-2-enoate Chemical compound CO[Si](OC)(OC)CCCOC(=O)C(C)=C XDLMVUHYZWKMMD-UHFFFAOYSA-N 0.000 claims description 3
- 229940073455 tetraethylammonium hydroxide Drugs 0.000 claims description 3
- LRGJRHZIDJQFCL-UHFFFAOYSA-M tetraethylazanium;hydroxide Chemical compound [OH-].CC[N+](CC)(CC)CC LRGJRHZIDJQFCL-UHFFFAOYSA-M 0.000 claims description 3
- BPSIOYPQMFLKFR-UHFFFAOYSA-N trimethoxy-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound CO[Si](OC)(OC)CCCOCC1CO1 BPSIOYPQMFLKFR-UHFFFAOYSA-N 0.000 claims description 3
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 2
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- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Substances [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims description 2
- 235000015320 potassium carbonate Nutrition 0.000 claims description 2
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 2
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- 239000004111 Potassium silicate Substances 0.000 description 6
- NNHHDJVEYQHLHG-UHFFFAOYSA-N potassium silicate Chemical compound [K+].[K+].[O-][Si]([O-])=O NNHHDJVEYQHLHG-UHFFFAOYSA-N 0.000 description 6
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Abstract
本发明公开一种超疏水纳米材料的制备方法,其是将钾水玻璃、结构导向剂、去离子水混合后,加热搅拌后将微硅粉分批加入到混合物中充分反应,得到硅溶胶,硅溶胶焙烧粉碎后得到纳米介孔二氧化硅;将硅烷偶联剂加入到无水乙醇中搅拌均匀,然后将纳米介孔二氧化硅加入到硅烷偶联剂‑乙醇溶液中,超声处理,室温陈化;将电石渣和铝灰焙烧后与FeS2混合破碎,并加入到无水乙醇溶液中搅拌混匀后,在超声下加入偶联剂搅拌混匀后,加入到陈化后的溶液中,混匀后得到超疏水纳米材料;本发明材料具有较好超疏水性能,在处理污染废水中有较强的吸附性能且容易分离再回收利用,用作防水涂层,其接触角>150°,滚动角<10°,且对污染气体具有较强的吸附性能。
Description
技术领域
本发明属于疏水材料与水污染处理技术领域,尤其涉及一种超疏水纳米材料的制备方法与应用。
背景技术
近年来超疏水纳米材料备受人们关注。超疏水是一种新型材料,在自然界中,许多植物叶表面、鸟禽羽毛都具有超疏水性的特点。我们将超疏水定义为材料表面稳定接触角>150°,滚动接触角<10°时的这类材料为超疏水材料。现如今,超疏水纳米材料因其优异的防水、防污、防腐蚀等性能已经被广泛用于油水分离领域、自清洁领域、医学领域、防覆冰领域等。目前,研究人员已经使用各种基材,如硅基、碳基、高分子基等材料来合成坚固、稳定和耐用的超疏水涂层。虽然关于超疏水材料研究已有很多报道,但大多数超疏水材料还存在原材料成本高、疏水性能差等问题无法工程化应用。
现在的纳米超疏水材料的制备中普遍存在成本高、改性剂价格昂贵,改性制剂有毒,存在污染环境的潜在风险,未达到超疏水性能要求且工艺繁琐等问题,极大的限制了其在一些行业的应用。
发明内容
针对传统疏水性材料具有防水性能差、制备成本较高、工艺繁琐,对环境具有一定污染风险等缺点,本发明提出了一种超疏水纳米材料的制备方法,该方法利用工业副产物微硅粉、电石渣、铝灰为主要原料制备超疏水纳米材料,应用于重金属污染废水的处理中,利用防水性能解决吸附材料和水难分离、二次再生困难等问题,或作为防水涂层净化污染气体,本发明可以增加工业副产物微硅粉、电石渣、铝灰的资源化利用途径,具有良好的生态效益和经济效益。
本发明超疏水纳米材料的制备方法步骤如下:
(1)将钾水玻璃、结构导向剂、去离子水混合后,在80~85℃下加热搅拌30~60min,然后将微硅粉分批加入到混合物中充分反应,得到硅溶胶,将硅溶胶置于450~550℃下焙烧4~6h,粉碎后得到纳米介孔二氧化硅;
所述钾水玻璃的添加量为微硅粉质量的20%~30%,结构导向剂为微硅粉质量的20%~30%;所述结构导向剂为十六烷基三甲基溴化铵、四乙基氢氧化铵、三乙胺中的一种或几种;
(2)将硅烷偶联剂加入到无水乙醇中搅拌均匀,然后将纳米介孔二氧化硅加入到硅烷偶联剂-乙醇溶液中,在50~60℃下超声处理30~60min,室温陈化;
硅烷偶联剂为γ-甲基丙烯酰氧基丙基三甲氧基硅烷、γ-氨丙基三乙氧基硅烷、γ-(2,3-环氧丙氧)丙基三甲氧基硅烷中的一种或几种,硅烷偶联剂的添加量为介孔二氧化硅质量的40%~50%;
(3)将电石渣和铝灰在800~900℃下焙烧1~3h后与FeS2混合破碎,并加入到无水乙醇溶液中搅拌混匀后,在超声下加入偶联剂搅拌混匀后,加入到步骤(2)陈化后的溶液中,混匀后得到超疏水纳米材料;
所述电石渣和铝灰的质量比为1:1~1.5,铝灰与FeS2的质量比为1:1.5~2.0,电石渣、铝灰、FeS2总质量: 偶联剂质量为1:0.5~1,电石渣添加量为介孔二氧化硅质量的12%~14%,偶联剂为乙烯基三乙氧基硅烷、乙烯基三甲氧基硅烷中的一种或几种。
所述微硅粉取自于硅冶炼行业,粒径为5nm~80nm,含水率为4%~6%;电石渣主要取自于能源厂,通过破碎筛分处理后粒径为20nm~30nm、含水率为2%~8%;铝灰主要取自于电解铝行业产生的二次铝灰,通过破碎筛分处理后粒径为15nm~60nm、含水率为3%~5%。
本发明另一目的是将上述方法制得的超疏水纳米材料应用在处理重金属污染废水、作为防水涂层净化污染气体中。
本发明超疏水纳米材料具有超疏水性能稳定持久、材料成本低、制备工艺简单、易将吸附材料与水分离、去除重金属和甲醛污染物等优点,其接触角大于154°,滚动角小于10°,对重金属、甲醛等污染物具有较强的吸附性能。
具体实施方式
下面通过实施例对本发明作进一步详细说明,但本发明保护范围不局限于所述内容。
实施例1:
(1)将2g钾水玻璃(硅酸钾)、2g十六烷基三甲基溴化铵(CTAB)、72g去离子水混合后,在80℃下加热搅拌30min,然后分批加入总量10g微硅粉充分反应得到硅溶胶,将硅溶胶置于450℃下焙烧6h,粉碎后得到纳米介孔二氧化硅;
(2)将4g的γ-甲基丙烯酰氧基丙基三甲氧基硅烷加入到10mL无水乙醇中100rpm下搅拌混匀,然后将纳米介孔二氧化硅10g加入到硅烷偶联剂-乙醇溶液中,在50℃、28kHz超声处理30min,室温陈化;
(3)将1.4g的电石渣、1.6g的铝灰在800℃高温下焙烧3h后,与3g的FeS2混合破碎,并加入15mL无水乙醇溶液中搅拌混匀后,在28kHz超声条件下加入4g的乙烯基三乙氧基硅烷搅拌混匀后,加入到步骤(2)陈化后的溶液中,混匀后得到超疏水纳米材料;
取上述制得超疏水纳米材料在85℃下干燥后,取10g放入含有50mg/L Cd2+、50mg/LMn2+、50mg/L Cd2+的重金属模拟废水100mL中,充分震荡反应4h;经检测,反应后模拟废水中Cd2+、Mn2+、Cd2+浓度均低于5mg/L,该超疏水纳米材料对重金属离子的去除率均大于90%,具有良好的重金属吸附能力。
实施例2:
(1)将4g钾水玻璃(硅酸钾)、4g十六烷基三甲基溴化铵(CTAB)、55g去离子水混合后,在83℃下加热搅拌45min,然后分批加入总量15g微硅粉充分反应得到硅溶胶,将硅溶胶在500℃下进行焙烧5h,粉碎后得到纳米介孔二氧化硅;
(2)将7g的γ-氨丙基三乙氧基硅烷加入到15mL无水乙醇中快速搅拌,然后将15g纳米介孔二氧化硅加入到硅烷偶联剂-乙醇溶液中,在55℃下40kHz超声处理45min,室温陈化;
(3)将2g的电石渣、2g的铝灰在850℃下焙烧2h后,与4g的FeS2混合破碎,并加入到15mL无水乙醇溶液中搅拌混匀后,在40kHz超声条件下加入7g的乙烯基三甲氧基硅烷搅拌混匀后,加入到步骤(2)的陈化后的溶液中,混匀后得到超疏水纳米材料;
在上述制得的100g纳米超疏水材料加入4g环氧树脂成膜剂,混匀后覆涂在木板上放入85℃烘干箱中干燥,利用接触角仪测试样品的接触角和滚动角,结果显示:原始木板为亲水性,覆涂上该材料后与水接触角为154°,滚动角为8°,使木板从亲水转化为疏水,具有良好的防水性能。
实施例3:
(1)将6g钾水玻璃(硅酸钾)、6g四乙基氢氧化铵、38g去去离子水混合后在85℃下加热搅拌60min,然后分批加入总量20g微硅粉充分反应得到硅溶胶,将硅溶胶在550℃高温下进行焙烧4h后,粉碎后得到纳米介孔二氧化硅;
(2)将10g的γ-(2,3-环氧丙氧)丙基三甲氧基硅烷加入到20mL无水乙醇中搅拌混匀,然后将20g纳米介孔二氧化硅加入到硅烷偶联剂-乙醇溶液中,在60℃、68kHz超声处理60min,室温陈化;
(3)将2.4g的电石渣、2.6g的铝灰在900℃下焙烧1h后,与5g的FeS2混合破碎,并加入20mL无水乙醇溶液中搅拌混匀后,在68kHz超声条件下加入5g的乙烯基三乙氧基硅烷和5g的乙烯基三甲氧基硅烷搅拌混匀后,加入到步骤(2)的陈化后的溶液中,混匀后得到超疏水纳米材料;
将上述制备的100g纳米超疏水材料加入4g丙烯酸树脂成膜剂后覆涂在50×50×50cm密闭木制盒子内壁,干燥后向盒子里注入1mg/m3的甲醛气体,反应4h后;检测结果显示反应后盒子中甲醛含量低于0.08mg/m3,该材料对甲醛的去除效率达90%以上,该材料的水接触角为154°,滚动角为9°,具有良好的甲醛吸附性能和防水性能。
应当理解的是本发明的应用不限于上述的举例,对本领域普通技术人员来说,可以根据上述说明加以改进或变换,所有这些改进和变换都应属于本发明所附权利要求的保护范围。
Claims (7)
1.一种超疏水纳米材料的制备方法,其特征在于,步骤如下:
(1)将钾水玻璃、结构导向剂、去离子水混合后,在80~85℃下加热搅拌30~60min,然后将微硅粉分批加入到混合物中充分反应,得到硅溶胶,将硅溶胶置于450~550℃下焙烧4~6h,粉碎后得到纳米介孔二氧化硅;
(2)将硅烷偶联剂加入到无水乙醇中搅拌均匀,然后将纳米介孔二氧化硅加入到硅烷偶联剂-乙醇溶液中,在50~60℃下超声处理30~60min,室温陈化;
(3)将电石渣和铝灰在800~900℃下焙烧1~3h后与FeS2混合破碎,并加入到无水乙醇溶液中搅拌混匀后,在超声下加入偶联剂搅拌混匀后,加入到步骤(2)陈化后的溶液中,混匀后得到超疏水纳米材料。
2.根据权利要求1所述的超疏水纳米材料的制备方法,其特征在于:钾水玻璃的添加量为微硅粉质量的20%~30%,结构导向剂为微硅粉质量的20%~30%。
3.根据权利要求1所述的超疏水纳米材料的制备方法,其特征在于:硅烷偶联剂为γ-甲基丙烯酰氧基丙基三甲氧基硅烷、γ-氨丙基三乙氧基硅烷、γ-(2,3-环氧丙氧)丙基三甲氧基硅烷中的一种或几种,硅烷偶联剂的添加量为介孔二氧化硅质量的40%~50%。
4.根据权利要求1所述的超疏水纳米材料的制备方法,其特征在于:电石渣和铝灰的质量比为1:1~1.5,铝灰与FeS2的质量比为1:1.5~2.0,电石渣、铝灰、FeS2总质量: 偶联剂质量为1:0.5~1,电石渣添加量为介孔二氧化硅质量的12%~14%,偶联剂为乙烯基三乙氧基硅烷、乙烯基三甲氧基硅烷中的一种或几种。
5.根据权利要求1所述的超疏水纳米材料的制备方法,其特征在于:微硅粉粒径为5nm~80nm,电石渣粒径为20nm~30nm,铝灰粒径为5nm~80nm。
6.根据权利要求1所述的超疏水纳米材料的制备方法,其特征在于:结构导向剂为十六烷基三甲基溴化铵、四乙基氢氧化铵、三乙胺中的一种或几种。
7.权利要求1-6任一项所述的超疏水纳米材料的制备方法制得的超疏水纳米材料在处理重金属污染废水、作为防水涂层净化污染气体中的应用。
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