CN110215915A - 一种蛭石/硅藻土基多孔陶瓷光催化板的制备方法 - Google Patents
一种蛭石/硅藻土基多孔陶瓷光催化板的制备方法 Download PDFInfo
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- 239000000919 ceramic Substances 0.000 title claims abstract description 58
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 56
- 239000010455 vermiculite Substances 0.000 title claims abstract description 49
- 229910052902 vermiculite Inorganic materials 0.000 title claims abstract description 49
- 235000019354 vermiculite Nutrition 0.000 title claims abstract description 47
- 230000001699 photocatalysis Effects 0.000 title claims abstract description 35
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 18
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- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 3
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- 230000015556 catabolic process Effects 0.000 description 6
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- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 4
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- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 2
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- 229910052710 silicon Inorganic materials 0.000 description 2
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- RBTBFTRPCNLSDE-UHFFFAOYSA-N 3,7-bis(dimethylamino)phenothiazin-5-ium Chemical group C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 RBTBFTRPCNLSDE-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 235000008331 Pinus X rigitaeda Nutrition 0.000 description 1
- 235000011613 Pinus brutia Nutrition 0.000 description 1
- 241000018646 Pinus brutia Species 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
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- IJKVHSBPTUYDLN-UHFFFAOYSA-N dihydroxy(oxo)silane Chemical compound O[Si](O)=O IJKVHSBPTUYDLN-UHFFFAOYSA-N 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
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- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 239000010977 jade Substances 0.000 description 1
- 238000010309 melting process Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- STZCRXQWRGQSJD-GEEYTBSJSA-M methyl orange Chemical compound [Na+].C1=CC(N(C)C)=CC=C1\N=N\C1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-GEEYTBSJSA-M 0.000 description 1
- 229940012189 methyl orange Drugs 0.000 description 1
- 229960000907 methylthioninium chloride Drugs 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 239000011941 photocatalyst Substances 0.000 description 1
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- DCKVNWZUADLDEH-UHFFFAOYSA-N sec-butyl acetate Chemical compound CCC(C)OC(C)=O DCKVNWZUADLDEH-UHFFFAOYSA-N 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
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- 239000000725 suspension Substances 0.000 description 1
- 239000012085 test solution Substances 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
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- 238000000870 ultraviolet spectroscopy Methods 0.000 description 1
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- 238000003911 water pollution Methods 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 1
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Abstract
本发明为一种蛭石/硅藻土基多孔陶瓷光催化板的制备方法。该方法包括以下步骤：将硅藻土、高岭土、白云石和蛭石球磨得到配料；将粘结剂聚乙烯醇和上步得到的配料依次加入到水中，得到浆料；将浆料倒入注浆、脱模后放入马弗炉中，升温得到蛭石/硅藻土基多孔陶瓷；将上步得到的蛭石/硅藻土基多孔陶瓷浸没入混合溶液中，浸渍‑烘干，得到负载有干胶的陶瓷；最后煅烧，得到蛭石/硅藻土基多孔陶瓷光催化板。本发明具有吸附协同光催化作用，解决光催化剂使用率低和单一吸附滤料饱和的问题，使其既具有吸附功能又具有光催化功能，用于印染废水终端，对其进行深度处理。
Description
技术领域
本发明属于印染废水脱色领域，具体为一种蛭石/硅藻土基多孔陶瓷光催化板的制备方法及其应用。
背景技术
随着我国社会工业化发展越来越迅速，随之而来的水污染问题也日趋严峻。印染废水作为水量大、难处理、难降解的废水种类之一，引起了人们的高度重视。我国的印染废水的处理主要有化学法、物理法和生物法(李炳金,易绍金,邓楚洲,等.印染废水处理技术研究[J].长江大学学报(自然科学版),2009,6:144-147.)。由于印染废水的复杂性，造成简单的某一种方法很难达到理想的处理效果。
S.N.Frank和A.J.Barden等人首次报道了，当用氙灯作为光照光源时，某些试剂如TiO2、ZnO、CdS、Fe2O3等能有效催化CN-和SO3 2-光解，这一结果的发现也使得光催化剂处理污水这一应用开始受到研究者的广泛关注。例如黄艳娥等(黄艳娥,琚行松.纳米二氧化钛光催化降解水中有机污染物的研究[J].现代化工,2001,4:45-48.)，Tanaka K(Tanaka,K.；Hisanaga,T.；Harada,K.,Photocatalytic degradation of organohalide compounds insemiconductor suspension with added hydrogen peroxide[J].New Journal OfChemistry.1989,13(1):5-7.)分别发现纳米TiO2可以用于多种有机废水的处理和降解Cr6 +,Hg3+等有毒金属重离子，至今发现二氧化钛在在紫外光照射下可以降解3000多种难处理的有机化合物。然而纳米TiO2颗粒在使用过程中，颗粒发生团聚现象，造成材料的浪费和环境污染，降低了催化效率。
国内外研究中大多将纳米二氧化钛负载在活性炭，多孔硅胶，天然多孔矿物如硅藻土等材料的粉体上，例如：李霞等(李霞，胡勤海，陈菊芬，等，纳米TiO2/硅藻土光催化降解废水中二甲胺[J].环境工程学报，2013，7(8)：3073-3078；)用溶胶凝胶法制备出了纳米TiO2/硅藻土复合材料，取3g/L的材料对浓度为400mg/L的二甲胺废水进行光催化处理，降解率为70％；虽然在一定程度上解决了光催化效率低的问题，但粉体难以回收的问题未得到解决。公开号为CN107398261的中国专利公开了一种基于硅藻土基多孔陶瓷复合催化剂的制备方法，虽然在一定程度上解决了粉体颗粒利用率低，但在制备多孔陶瓷过程中使用了造孔剂，造孔剂在烧结过程中的燃烧会造成二次污染，对环境有一定程度的影响。
为此针对上述问题，本发明提出一种蛭石/硅藻土基多孔陶瓷光催化板的制备方法，其能够解决现有制备技术中的环境污染问题和粉体利用率低及难以回收问题。
发明内容
本发明的目的为针对上述现有技术中存在的不足，提供一种蛭石/硅藻土基多孔陶瓷光催化板的制备方法。该材料使用具有自膨胀性能的蛭石，增大颗粒间的距离，在烧结助剂熔融过程中保护硅藻土原始孔洞；通过控制蛭石添加量，在不添加造孔剂的前提下，得到具有一定抗压强度、高孔隙率的蛭石/硅藻土基多孔陶瓷。采用溶胶凝胶法，将纳米二氧化钛负载在蛭石/硅藻土基多孔陶瓷上得到蛭石/硅藻土基多孔陶瓷光催化板的，使其具有吸附协同光催化作用，解决光催化剂使用率低和单一吸附滤料饱和的问题，使其既具有吸附功能又具有光催化功能，用于印染废水终端，对其进行深度处理。
本发明的技术方案为：
一种蛭石/硅藻土基多孔陶瓷光催化板的制备方法，该方法包括以下步骤：
(1)，蛭石/硅藻土基多孔陶瓷的配料制备：将硅藻土、高岭土、白云石和蛭石作为物料，放入球磨罐中，加入磨球，再加入无水乙醇浸润物料，以800r/min～1000r/min球磨1h～2h，然后烘干，得到配料；
其中，物料组成的质量百分比分别为：50％～80％的硅藻土，10％～40％的高龄土，2％～20％的白云石和1％～15％的蛭石；
所述的球磨步骤中，质量比为磨球：物料＝1～3：1；磨球按照直径尺寸分为三种，质量比为：3～5mm的磨球:5～8mm的磨球:8～10mm的磨球＝3：2：1；
(2)，蛭石/硅藻土基多孔陶瓷的成型和烧结：搅拌下，将粘结剂聚乙烯醇和上步得到的配料依次加入到60～70℃的去离子水中，然后继续搅拌1h～2h，得到浆料；将浆料倒入注浆模具中，自然条件下放至干燥；脱模后放入马弗炉中，升温至1000℃～1150℃后，保温1～2小时，随炉冷却至室温，得到蛭石/硅藻土基多孔陶瓷；
其中，每300g～600g配料加入600mL～1000mL去离子水；聚乙烯醇质量为配料质量的0.1％～2％；
所述的搅拌的转速为200r/min～300r/min；
所述的升温步骤优选为：以1℃/min～5℃/min的升温速率从室温升至500℃～800℃，保温1h～2h；然后以2℃/min～5℃/min的升温速率继续升温至1000℃～1150℃；
(3)，负载纳米TiO2：
将上步得到的蛭石/硅藻土基多孔陶瓷浸没入混合溶液中，在恒温气浴振荡器上25～35℃恒温震荡1h～2h，将陶瓷取出80℃～105℃烘干0.5～1.5h；重复“浸渍-烘干”过程3～10次，得到负载有干胶的陶瓷；最后将带有干胶的陶瓷置于马弗炉中700℃～900℃煅烧1～3h，得到蛭石/硅藻土基多孔陶瓷光催化板；
所述的混和溶液的制备方法，包括如下步骤：将溶液A用滴加到溶液B中，磁力搅拌30min～60min而成；其中，体积比为溶液B：溶液A＝2～6：1；所述A溶液的组成为无水乙醇和去离子水，体积比为1～10：1；并用硝酸调节至pH＝1～3；所述溶液B的组成为钛酸丁酯、无水乙醇和冰乙酸，体积比为：钛酸丁酯：无水乙醇：冰乙酸＝10～20：15～40：5～20。
本发明的有益效果为：
本发明的蛭石/硅藻土基多孔陶瓷的1000℃烧结时气孔率高于65％，抗压强度高于14MPa,气孔率和抗压强度随温度的变化曲线见图1，负载纳米TiO2后的蛭石/硅藻土基多孔陶瓷光催化板的SEM图见图2。在固定光源波长253.7nm、功率20W～200W，反应温度为25℃条件下对拟配印染污水进行光催化实验，其结果优于纯吸附滤料的处理效果，污染物去处率提高了20％～30％，并且可重复利用。
附图说明
图1为本发明的未负载纳米TiO2蛭石/硅藻土基多孔陶瓷的气孔率和抗压强度随温度的变化曲线
图2为本发明实施例1制备的蛭石/硅藻土基多孔陶瓷光催化板的SEM图
图3为本发明实施例1制备蛭石/硅藻土基多孔陶瓷光催化板进行光催化反应后的SEM图；
图4为本发明实施例1制备的样品对拟配印染废水去除率对比图
图5为本发明实施例1制备的蛭石/硅藻土基多孔陶瓷光催化板的多次使用的对比图
具体实施方式
实施例1
取质量分数70％硅藻土和21％高龄土等作为骨料，4％白云石作为烧结助剂加入5％的蛭石作为改性剂，(硅藻土，高岭土，白云石和蛭石均来自天津弘喜泰化工贸易有限公司)。每个球磨罐中放入100g物料；按照磨球与物料质量比为3：1，加入直径为3～5mm的磨球150g,5～8mm的磨球100g,8～10mm的磨球50g，再加入无水乙醇至没过配料，以1000r/min的转速对配料球磨，球磨时间为1h,完成后烘干，打散，得到配料。采用注浆成形的方法，取6g聚乙烯醇粘结剂，放入分散容器内，加入900ml温度为65℃的去离子水中，搅拌至凝胶状；在300r/min的转速下再在分散容器内加入磨好的配料600g，分散1h。分散好的浆料倒入矩形注浆模具中，自然条件下放至干燥。脱模，放入马弗炉中烧制。从30℃开始，以1℃/min的升温速率升至800℃，保温1h；然后以2℃/min的升温速率继续升温到1150℃，保温2h。得到大小为5cm*5cm*0.8cm的蛭石/硅藻土基多孔陶瓷。再制备溶胶溶液：将用硝酸调节pH＝1.5的A溶液(无水乙醇52mL,去离子水20mL)用恒压管以1mL/min的速度滴加用滴加到酸液B(钛酸丁酯45mL、无水乙醇81mL和冰乙酸30mL)中，磁力搅拌40min。然后对微孔陶瓷进行浸渍：将洗净并干燥的自制多孔陶瓷和A和B的混合溶液加入到烧杯中，将烧杯在恒温气浴振荡器上30℃恒温震荡1h，将陶瓷取出105℃烘干1h，将浸渍和烘干过程重复5次。将带有干胶的陶瓷置于马弗炉中700℃煅烧2h，得到蛭石/硅藻土基多孔陶瓷光催化板。
在固定光源波长253.7nm、功率200W，光照强度8mW·cm-2，光照距离为10cm，反应温度为25℃条件下，采用一块大小为5cm*5cm*0.8cm的蛭石/硅藻土基多孔陶瓷光催化板对600mL，COD浓度为220mg/L的拟配印染废水(主要成分为亚甲基蓝和甲基橙)进行吸附和光催化降解。采用紫外-可见分光光度计测试溶液的吸光度，反应印染废水被降解的程度。得到的去除效果见图4。一次实验后将陶瓷板在100℃下烘干，再重复上述实验，重复使用次数效果见图5。
实施例2
其他步骤同实施例1，不同之处为蛭石的添加量替换为10％，硅藻土添加量替换为65％，其余物料的添加量不变。得到的催化板催化降解效果接近实施例1。
实施例3
其他步骤同实施例1，不同之处为将陶瓷板的烧结温度升至1100℃。得到的催化板催化降解效果接近实施例1。
由图4可知曲线从上到下分别为蛭石/硅藻土基多孔陶瓷光催化板的光催化结果，未负载纳米二氧化钛的多孔陶瓷的吸附结果，负载纳米二氧化钛的吸附结果。分析三条曲线，可知不接受紫外光照射时材料只有吸附作用，且未负载的蛭石/硅藻土基多孔陶瓷比蛭石/硅藻土基多孔陶瓷光催化板对印染尾水的吸附去除率高；接受紫外光照射后，蛭石/硅藻土基多孔陶瓷光催化板对印染尾水的降解率最高，且40分钟后印染尾水的去除率接近100％。蛭石/硅藻土基多孔陶瓷光催化板使用不同次数后对印染尾水的去除率如图5所示。由图可知，随着蛭石/硅藻土基多孔陶瓷光催化板使用次数的增加，印染尾水的去除率降低。在重复使用5次后，印染尾水的去除率接近于90％。
显然，上述实施例仅仅是为清楚说明所做的举例，并非对实施方式的限定。这里无需也无法对所有的实施方式予以举例，而由此所引伸出的显而易见的变化或变动仍处于本发明创造的保护范围之中。
本发明未尽事宜为公知技术。
Claims (4)
1.一种蛭石/硅藻土基多孔陶瓷光催化板的制备方法，其特征为该方法包括以下步骤：
（1）蛭石/硅藻土基多孔陶瓷的配料制备：将硅藻土、高岭土、白云石和蛭石作为物料，放入球磨罐中，加入磨球，再加入无水乙醇浸润物料，以800r/min~1000r/min球磨1h~2h，然后烘干，得到配料；
其中，物料组成的质量百分比分别为：50%~80%的硅藻土，10%~40%的高龄土，2%~20%的白云石和1%~15%的蛭石；
（2）蛭石/硅藻土基多孔陶瓷的成型和烧结：搅拌下，将粘结剂聚乙烯醇和上步得到的配料加入到60~70℃的去离子水中，然后继续搅拌1h~2h，得到浆料；将浆料倒入注浆模具中，自然条件下放至干燥；脱模后放入马弗炉中，升温至1000℃~1150℃后，保温1~2小时，随炉冷却至室温，得到硅藻土基多孔陶瓷；
其中，每300g~600g配料加入600mL~1000mL去离子水；聚乙烯醇质量为配料质量的0.1%~2%；
（3）负载纳米TiO2：
将上步得到的蛭石/硅藻土基多孔陶瓷浸没入混合溶液中，在恒温气浴振荡器上25~35℃恒温震荡1h~2h，将陶瓷取出80℃~105℃烘干0.5~1.5h；重复“浸渍-烘干”过程3~10次，得到负载有干胶的陶瓷；最后将带有干胶的陶瓷置于马弗炉中700℃~900℃煅烧1~3h，得到蛭石/硅藻土基多孔陶瓷光催化板；
所述的混和溶液的制备方法，包括如下步骤：将溶液A用滴加到溶液B中，磁力搅拌30min~60min而成；其中，体积比为溶液B：溶液A=2~6：1；所述A溶液的组成为无水乙醇和去离子水，体积比为1~10：1；并用硝酸调节至pH=1~3；所述溶液B的组成为钛酸丁酯、无水乙醇和冰乙酸，体积比为：钛酸丁酯：无水乙醇：冰乙酸=10~20：15~40：5~20。
2.如权利要求1所述的蛭石/硅藻土基多孔陶瓷光催化板的制备方法，其特征为所述的步骤（1）中球磨步骤中，质量比为磨球：物料=1~3：1；磨球按照直径尺寸分为三种，质量比为：3~5mm的磨球:5~8mm的磨球:8~10mm的磨球=3：2：1。
3.如权利要求1所述的蛭石/硅藻土基多孔陶瓷光催化板的制备方法，其特征为所述的步骤（2）中搅拌的转速为200r/min~300r/min。
4.如权利要求1所述的蛭石/硅藻土基多孔陶瓷光催化板的制备方法，其特征为所述的步骤（2）中升温步骤优选为：以1℃/min~5℃/min的升温速率从室温升至500℃~800℃，保温1h~2h；然后以2℃/min~5℃/min的升温速率继续升温1000℃~1150℃。
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