CN113104995A - 一种磁性聚氨酯光生耦合填料及其制备方法 - Google Patents
一种磁性聚氨酯光生耦合填料及其制备方法 Download PDFInfo
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Abstract
本发明创造提供了一种磁性聚氨酯光生耦合填料及其制备方法,所述填料为表面负载有光催化材料的磁性聚氨酯海绵,所述光催化复合材料为溶胶‑凝胶方法制备而得的光催化剂/改性磁粉复合材料。本发明创造所述的磁性聚氨酯光生耦合填料具有磁性、亲水性、粗糙、光催化活性,将氧化和生化两个工艺融为一体,为处理低浓度难降解废水提供新思路。
Description
技术领域
本发明创造属于水处理行业技术领域,尤其是涉及一种磁性聚氨酯光生耦合填料及其制备方法。
背景技术
聚氨酯具有良好的稳定性、加工工艺简单、吸附力强以及成本低廉的优点,可以制成多种聚氨酯材料,其中聚氨酯海绵具有三维多孔结构、柔韧性强等优点,在废水生物处理过程中,为了强化生物处理的效果,聚氨酯海绵常被用作微生物固定化的载体材料。
研究发现,稳恒弱磁场可以有效地刺激微生物活性菌的生长,缩短其生长周期,提高微生物活性,故在聚氨酯海绵中添加磁粉等磁性物质进行改性,使整个聚氨酯海绵内外均带有微弱的磁场,如专利申请CN1263054A中将塑料材料、磁性材料和助剂加工制作成磁性纤丝,在将磁性纤丝制成三维结构的磁性填料,是其在进行水质净化过程中形成磁场来提高生物膜内的微生物活性;专利申请CN101070425A还在其中加入了反应性磁性粒子,以利用其产生的稳恒弱磁场来提高废水的生物降解效率。但是当该复合磁性聚氨酯泡沫载体用于生物流化床的实际处理过程中,由于磁性颗粒与聚氨酯海绵的结合的强度差,容易脱落,造成净化效果变差。
发明内容
有鉴于此,本发明创造旨在克服现有技术中的缺陷,提出一种高效率和高稳定性的磁性聚氨酯光生耦合填料。
为达到上述目的,本发明创造的技术方案是这样实现的:
一种磁性聚氨酯光生耦合填料,所述填料为表面负载有光催化复合材料的磁性聚氨酯海绵,所述光催化复合材料为溶胶-凝胶方法制备而得的光催化剂/改性磁粉复合材料。
优选的,所述光催化剂/改性磁粉复合材料中改性磁粉的质量占比为8-15%。
优选的,所述磁性聚氨酯海绵中的复合有磁粉或改性磁粉,所述磁粉或改性磁粉的质量占磁性聚氨酯海绵总质量的3-8%。
优选的,所述光催化剂为TiO2、C3N4、铋化物中的一种;
优选的,所述改性磁粉为四氧化三铁、钡铁氧体、钴铁氧体、γ-三氧化二铁、α-三氧化二铁、汝铁硼微粒材料中的至少一种经改性后制得。
优选的,所述光催化剂/改性磁粉复合材料的制备方法为:
a、将改性磁粉、无水乙醇与水混合均匀形成A液备用,并调节A液的pH值为3-5,其中,无水乙醇与水的体积比为2:1-4:1;
b、在搅拌状态下将光催化剂缓慢加到无水乙醇中形成B液,B液继续搅拌或超声分散1-3h;
c、将B液缓慢滴入A液中并继续搅拌1-3h,滴加A液的时间控制在30-60min,陈化后取出凝胶并沥去表面多余的溶胶80-120℃烘干得到干凝胶;
d、将干凝胶洗涤后放入管式炉中350-600°C煅烧2-4h即得光催化剂/改性磁粉复合材料。
优选的,所述光催化剂为钛源,所述钛源为钛酸酯类化合物,优选为钛酸四丁酯或钛酸四异丙酯。
优选的,所述改性磁粉的制备方法为:将磁粉与水混合均匀后制成悬浊液;加入醇的水溶液和偶联剂后至完全反应,再从反应介质中分离出磁粉,用醇的水溶液对分离出的磁粉清洗后干燥即得改性磁粉。
优选的,所述偶联剂为硅烷偶联剂、硅酸酯偶联剂、铝酸酯偶联剂中的至少一种。
优选的,所述填料由溶于溶剂的光催化剂/改性磁粉采用喷射法喷涂或浸渍法浸渍磁性聚氨酯泡沫表层,烘干后制得。
本发明还提供一种磁性聚氨酯光生耦合填料的制备方法,包括如下步骤:
S1:制备改性磁粉
称取磁粉与水混合超声分散后制成磁粉悬浊液;向磁粉悬浮液中加入醇的水溶液和偶联剂,混合后至完全反应,再从反应介质中分离出磁粉,用醇的水溶液对分离出的磁粉用醇的水溶液清洗后干燥即得改性磁粉;
S2:制备光催化剂/改性磁粉复合材料
具体步骤为:
a、将改性磁粉、无水乙醇与水混合均匀形成A液备用,并调节A液的pH值为3-5,其中,无水乙醇与水的体积比为2:1-4:1;
b、在搅拌状态下将光催化剂缓慢加到无水乙醇中形成B液,B液继续搅拌或超声分散1-3h;
c、将B液缓慢滴入A液中并继续搅拌1-3h,滴加A液的时间控制在30-60min,陈化后取出凝胶并沥去表面多余的溶胶80-120℃烘干得到干凝胶;
d、将干凝胶洗涤后放入管式炉中350-600°C煅烧2-4h即得光催化剂/改性磁粉复合材料;
S3:制备磁性聚氨酯填料
将磁粉或改性磁粉加入至聚氨酯填料的原料中后采用常规方法制备得到磁性聚氨酯填料;
S4:制备磁性聚氨酯光生耦合填料
将光催化剂/改性磁粉复合材料溶于溶剂中后,采用喷射法喷涂或浸渍法浸渍至磁性聚氨酯填料表层,烘干后得到成品。
优选的,步骤S1中醇的水溶液为体积浓度为50%的乙醇水溶液。
优选的,所述磁性聚氨酯填料中磁粉或改磁粉的质量百分比为3-8%。
相对于现有技术,本发明创造具有以下优势:
(1)使用本发明创造所述的磁性聚氨酯光生耦合填料只需一个设备即可完成光催化氧化开链和生化矿化有机污染物;
(2)本发明的填料的磁性和亲水性在填料雏形期间就已形成,磁性光催化剂与磁性填料相互结合使填料内的磁粉不易脱落,持久性强,具有污染物磁化预处理功能,同时在磁场的作用下生物增殖性能更佳;
(3)相对高级氧化-生物降解联用技术,本发明的磁性聚氨酯光生耦合填料具有空间利用集约及调控更为简易的特点,在抑制性废水处理领域极具吸引力。通过改变光照环境和光催化强度,可达到保护微生物活性以强化生物降解作用,解决了高效率(煅烧法会碳化聚氨酯填料)和稳定性(浸渍法稳定性差)相互矛盾不可兼得的技术问题。
附图说明
图1为本发明创造实施例所述的磁性聚氨酯光生耦合填料的工作原理示意图。
图中:1、光源;2、磁性聚氨酯光生耦合填料;3、微生物;4、光催化剂/改性磁粉;5、改性磁粉或磁粉;6、污染物。
具体实施方式
除有定义外,以下实施例中所用的技术术语具有与本发明创造所属领域技术人员普遍理解的相同含义。以下实施例中所用的试验试剂,如无特殊说明,均为常规生化试剂;所述实验方法,如无特殊说明,均为常规方法。
下面结合实施例来详细说明本发明创造。
实施例1
一种磁性聚氨酯光生耦合填料的制备工艺,包括如下步骤:
(1)称取Fe3O4和MiNi Q水超声分散后制成Fe3O4悬浮液;加入50%的乙醇-水溶液,同时加入KH550,水浴锅中快速机械揽拌,反应完全化。从反应介质中磁分离,并用50%的乙醇-水溶液对其清洗,干燥备用得到改性Fe3O4。
(2)称取水溶性聚酯多元醇固体真空脱水2小时,冷却备用。
(3)称取改性Fe3O4加入到六亚甲基二异氰酸酯中,80℃下机械搅拌0.5 h,再加入麻风树脂油基多元醇(JOL)和二月桂酸二丁基锡继续反应。反应2h后,降温到65℃后加入二羟甲基丙酸,继续升温到80℃反应1h后降低温度到40℃,并加入丙酮降低反应物粘度,然后加入三乙胺中和10min,将得到的预聚体倒入分散桶中,加水高速剪切分散,制备分散液,将分散于倒入聚四氟乙烯的模具中,真空干燥,改性Fe3O4的质量占磁性聚氨酯海绵总质量的4%。
(4)采用溶胶-凝胶方法制备二氧化钛/改性四氧化三铁复合材料(TiO2/Fe3O4) :以钛酸四丁酯为钛源,以无水乙醇为溶剂,制备TiO2溶胶具体制备步骤如下:将无水乙醇、水(1:2)和混合均匀组成A液备用,并用冰乙酸或硝酸调节溶液pH3.5,在磁力搅拌下将Ti(OC4H9)4缓慢加到无水乙醇中组成B液,B液继续磁力搅拌(也可以采用超声)2 h拌。B液缓慢滴入A液并继续搅拌3h,滴加B液的时间控制在30~60min左右,然后慢慢取出凝胶并沥去表面多余的溶胶80℃烘干。洗涤后将负载后TiO2/Fe3O4放入管式炉中。在空气气氛下,550℃煅烧2~4h后即得 TiO2/Fe3O4复合材料,TiO2/Fe3O4复合材料中改性Fe3O4的质量占比为10%。
(5)煅烧后的TiO2/Fe3O4溶于溶剂(醇、水混合物)采用喷射法喷涂或浸渍法浸渍磁性聚氨酯泡沫表层,烘干后得到成品。
实施例2
一种磁性聚氨酯光生耦合填料的制备工艺,包括如下步骤:
(1)称取γ- Fe2O3和MiNi Q水超声分散后制成γ- Fe2O3悬浮液;加入50%的乙醇-水溶液,同时加入KH550,水浴锅中超声分散,反应完全化。从反应介质中磁分离,并用50%的乙醇-水溶液对其清洗,干燥备用得到改性γ- Fe2O3。
(2)称取水溶性聚酯多元醇固体真空脱水2小时,冷却备用。
(3)称取改性γ- Fe2O3加入到六亚甲基二异氰酸酯中,80℃下机械搅拌0.5 h,再加入麻风树脂油基多元醇(JOL)和二月桂酸二丁基锡继续反应。反应2h后,降温到65℃后加入二羟甲基丙酸,继续升温到80℃反应1h后降低温度到40℃,并加入丙酮降低反应物粘度,然后加入三乙胺中和10min,将得到的预聚体倒入分散桶中,加水高速剪切分散,制备分散液,将分散于倒入聚四氟乙烯的模具中,真空干燥,改性γ- Fe2O3的质量占磁性聚氨酯海绵总质量的3%。
(4)采用溶胶-凝胶方法制备二氧化钛/改性γ- Fe2O3复合材料(TiO2/γ- Fe2O3):以钛酸四异丙酯为钛源,以无水乙醇为溶剂,制备TiO2溶胶具体制备步骤如下:将无水乙醇、水(1:2)和混合均匀组成A液备用,并用冰乙酸或硝酸调节溶液pH3.5,在磁力搅拌下将钛酸四异丙酯缓慢加到无水乙醇中组成B液,B液继续磁力搅拌(也可以采用超声)2 h拌。B液缓慢滴入A液并继续搅拌3h,滴加B液的时间控制在30~60min左右,然后慢慢取出凝胶并沥去表面多余的溶胶80℃烘干。洗涤后将负载后TiO2/γ- Fe2O3放入管式炉中。在空气气氛下,550℃煅烧2~4h后即得 TiO2/γ- Fe2O3复合材料,TiO2/γ- Fe2O3复合材料中改性Fe3O4的质量占比为8%。
(5)煅烧后的TiO2/γ-Fe2O3溶于溶剂(醇、水混合物)采用喷射法喷涂或浸渍法浸渍磁性聚氨酯泡沫表层,烘干后得到成品。
实施例3
一种磁性聚氨酯光生耦合填料的制备工艺,包括如下步骤:
(1)称取α-Fe2O3和MiNi Q水超声分散后制成α- Fe2O3悬浮液;加入50%的乙醇-水溶液,同时加入KH550,水浴锅中快速机械揽拌,反应完全化。从反应介质中磁分离,并用50%的乙醇-水溶液对其清洗,干燥备用得到改性α-Fe2O3。
(2)称取水溶性聚酯多元醇固体真空脱水2小时,冷却备用。
(3)称取改性α-Fe2O3加入到六亚甲基二异氰酸酯中,80℃下机械搅拌0.5 h,再加入麻风树脂油基多元醇(JOL)和二月桂酸二丁基锡继续反应。反应2h后,降温到65℃后加入二羟甲基丙酸,继续升温到80℃反应1h后降低温度到40℃,并加入丙酮降低反应物粘度,然后加入三乙胺中和10min,将得到的预聚体倒入分散桶中,加水高速剪切分散,制备分散液,将分散于倒入聚四氟乙烯的模具中,真空干燥,改性α-Fe2O3的质量占磁性聚氨酯海绵总质量的8%。
(4)采用溶胶-凝胶方法制备二氧化钛/改性四氧化三铁复合材料(TiO2/α-Fe2O3):以钛酸四丁酯为钛源,以无水乙醇为溶剂,制备TiO2溶胶具体制备步骤如下:将无水乙醇、水(1:2)和混合均匀组成A液备用,并用冰乙酸或硝酸调节溶液pH3.5,在磁力搅拌下将Ti(OC4H9)4缓慢加到无水乙醇中组成B液,B液继续磁力搅拌(也可以采用超声)2h拌。B液缓慢滴入A液并继续搅拌3h,滴加B液的时间控制在30~60min左右,然后慢慢取出凝胶并沥去表面多余的溶胶80℃烘干。洗涤后将负载后TiO2/α-Fe2O3放入管式炉中。在空气气氛下,550℃煅烧2~4h后即得 TiO2/α-Fe2O3复合材料,TiO2/α-Fe2O3复合材料中改性α-Fe2O3的质量占比为15%。
(5)煅烧后的TiO2/α-Fe2O3溶于溶剂(醇、水混合物)采用喷射法喷涂或浸渍法浸渍磁性聚氨酯泡沫表层,烘干后得到成品。
实施例4 负载微生物
接种使用的活性污泥种源来自污水处理厂A2/O 工艺好氧段,采用浸泡吸附的方式将活性污泥接种至实施例1-3制得的磁性聚氨酯泡沫上。将磁性聚氨酯泡沫载体浸泡在活性污泥中并曝气 24 h后进行常规挂膜。挂膜后海绵载体的内部孔道和外表面有一定的生物量,将磁性聚氨酯泡沫放入全混合式连续流反应器(CAFB)中进行培养。CAFB 采用连续流进低浓度稀释后废水,后续逐步升高进水污染物浓度。在反应器底部有曝气装置,溶解氧控制在 2 mg/L以上。在培养过程中全程采用紫外灯光辐照磁性聚氨酯泡沫表面,所用的紫外灯的相应光能的爱因斯坦常数为紫外强度为3.93 × 10−7 einstein/(L·s)。
表1. 磁性聚氨酯泡沫载体挂膜人工配水组分
主要成分 | 含量(mg/L) | 微量元素 | 含量(mg/L) |
NaAc·3H<sub>2</sub>O | 330 | H<sub>3</sub>BO<sub>3</sub> | 2.86 |
NH<sub>4</sub>Cl | 28.66 | MnCl<sub>2</sub> | 1.86 |
K<sub>2</sub>HPO<sub>4</sub>·3H<sub>2</sub>O | 12 | CuSO<sub>4</sub> | 0.08 |
NaH<sub>2</sub>PO<sub>4</sub>·2H<sub>2</sub>O | 4 | ZnSO<sub>4</sub> | 0.22 |
CaCl<sub>2</sub> | 2 | Na<sub>2</sub>MoO<sub>4</sub> | 0.39 |
MgSO<sub>4</sub>·7H<sub>2</sub>O | 2 |
人工配水组分如上表所示,其中 C:N:P 约为 100:5:1,进水 CODCr 保持在130mg/L,每天监测进出水中 CODCr 和 DO(溶解氧)等指标,并观察载体中生物膜的生长及分布情况,7天左右待出水 CODCr 稳定后即可,此时生物膜会稳定的附着于磁性聚氨酯泡沫载体。
试验例1 处理苯酚废水
当进水苯酚浓度10mg/L时,光催化的矿化程度COD去除率小于50%,生化反应下COD几乎没有去除,使用本发明实施例1-3制得的磁性聚氨酯光生耦合填料COD去除率分别提高至70%、73%和60%。可见本发明的磁性聚氨酯光生耦合填料处理苯酚废水的能力大于生化反应处理印染废水的能力。
试验例2 处理印染废水
当印染废水进水的COD约1500 mg/L,分别采用固定光催化剂、固定光合细菌以及实施例1-3制得的磁性聚氨酯光生耦合填料分析其降解COD能力。实验结果表明:使用本发明实施例1-3制得的磁性聚氨酯光生耦合填料COD去除率分别提高至81%、85%和75%,而固定光催化剂的COD去除率约为25%,固定光合细菌的COD去除率约为45%。可见本发明的磁性聚氨酯光生耦合填料处理印染废水的能力大于固定光催化剂与固定光合细菌处理印染废水的能力。
试验例3 处理磺胺类废水
当磺胺类废水进水中COD约为10mg/L时,光催化的矿化程度COD去除率小于30%,生化反应下COD几乎没有去除,使用本发明实施例1-3制得的磁性聚氨酯光生耦合填料COD去除率提高至67%、70%、61%。可见本发明的磁性聚氨酯光生耦合填料处理磺胺类废水的能力大于光催化剂处理磺胺类废水的能力。
试验例4
将相同质量的使用本发明实施例1-3制得的磁性聚氨酯光生耦合填料和常规浸渍TiO2的聚氨酯填料放入等体积水溶液中,旋转搅拌48h,测得浸出液的Ti的含量分别为19ug/L、53ug/L、2ug/L和226ug/L。可见,本发明的磁性聚氨酯光生耦合填料中的光催化材料与聚氨酯海绵中的磁粉相互结合,牢固且不易脱落,增加了耦合填料的稳定性和使用寿命。
以上所述仅为本发明创造的较佳实施例而已,并不用以限制本发明创造,凡在本发明创造的精神和原则之内,所作的任何修改、等同替换、改进等,均应包含在本发明创造的保护范围之内。
Claims (10)
1.一种磁性聚氨酯光生耦合填料,其特征在于:所述填料为表面负载有光催化复合材料的磁性聚氨酯海绵,所述光催化复合材料为溶胶-凝胶方法制备而得的光催化剂/改性磁粉复合材料。
2.根据权利要求1所述的磁性聚氨酯光生耦合填料,其特征在于:所述光催化剂/改性磁粉复合材料中改性磁粉的质量占比为8-15%;所述磁性聚氨酯海绵中的复合有磁粉或改性磁粉,所述磁粉或改性磁粉的质量占磁性聚氨酯海绵总质量的3-8%。
3.根据权利要求1所述的磁性聚氨酯光生耦合填料,其特征在于:所述光催化剂为TiO2、C3N4、铋化物中的一种;所述改性磁粉为四氧化三铁、钡铁氧体、钴铁氧体、γ-三氧化二铁、汝铁硼微粒材料中的至少一种经改性后制得。
4.根据权利要求1所述的磁性聚氨酯光生耦合填料,其特征在于:所述光催化剂/改性磁粉复合材料的制备方法为:
a、将改性磁粉、无水乙醇与水混合均匀形成A液备用,并调节A液的pH值为3-5,其中,无水乙醇与水的体积比为2:1-4:1;
b、在搅拌状态下将光催化剂缓慢加到无水乙醇中形成B液,B液继续搅拌或超声分散1-3h;
c、将B液缓慢滴入A液中并继续搅拌1-3h,滴加A液的时间控制在30-60min,陈化后取出凝胶并沥去表面多余的溶胶80-120℃烘干得到干凝胶;
d、将干凝胶洗涤后放入管式炉中350-600°C煅烧2-4h即得光催化剂/改性磁粉复合材料。
5.根据权利要求1所述的磁性聚氨酯光生耦合填料,其特征在于:所述光催化剂为钛源,所述钛源为钛酸酯类化合物。
6.根据权利要求1所述的磁性聚氨酯光生耦合填料,其特征在于:所述改性磁粉的制备方法为:将磁粉与水混合均匀后制成悬浊液;加入醇的水溶液和偶联剂后至完全反应,再从反应介质中分离出磁粉,用醇的水溶液对分离出的磁粉清洗后干燥即得改性磁粉。
7.根据权利要求6所述的磁性聚氨酯光生耦合填料,其特征在于:所述偶联剂为硅烷偶联剂、硅酸酯偶联剂、铝酸酯偶联剂中的至少一种。
8.根据权利要求1所述的磁性聚氨酯光生耦合填料,其特征在于:所述填料由溶于溶剂的光催化剂/改性磁粉采用喷射法喷涂或浸渍法浸渍磁性聚氨酯泡沫表层,烘干后制得。
9.权利要求1-8任一所述的磁性聚氨酯光生耦合填料的制备方法,其特征在于:包括如下步骤:
S1:制备改性磁粉
称取磁粉与水混合超声分散后制成磁粉悬浊液;向磁粉悬浮液中加入醇的水溶液和偶联剂,混合后至完全反应,再从反应介质中分离出磁粉,用醇的水溶液对分离出的磁粉用醇的水溶液清洗后干燥即得改性磁粉;
S2:制备光催化剂/改性磁粉复合材料
具体步骤为:
a、将改性磁粉、无水乙醇与水混合均匀形成A液备用,并调节A液的pH值为3-5,其中,无水乙醇与水的体积比为2:1-4:1;
b、在搅拌状态下将光催化剂缓慢加到无水乙醇中形成B液,B液继续搅拌或超声分散1-3h;
c、将B液缓慢滴入A液中并继续搅拌1-3h,滴加A液的时间控制在30-60min,陈化后取出凝胶并沥去表面多余的溶胶80-120℃烘干得到干凝胶;
d、将干凝胶洗涤后放入管式炉中350-600°C煅烧2-4h即得光催化剂/改性磁粉复合材料;
S3:制备磁性聚氨酯填料
将磁粉或改性磁粉加入至聚氨酯填料的原料中后采用常规方法制备得到磁性聚氨酯填料;
S4:制备磁性聚氨酯光生耦合填料
将光催化剂/改性磁粉复合材料溶于溶剂中后,采用喷射法喷涂或浸渍法浸渍至磁性聚氨酯填料表层,烘干后得到成品。
10.权利要求9所述的磁性聚氨酯光生耦合填料的制备方法,其特征在于:步骤S1中醇的水溶液为体积浓度为50%的乙醇水溶液;所述磁性聚氨酯填料中磁粉或改磁粉的质量百分比为3-8%。
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