CN114150438B - 酿酒废水处理的石墨烯人工水草及其制备方法 - Google Patents
酿酒废水处理的石墨烯人工水草及其制备方法 Download PDFInfo
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Abstract
本发明属于石墨烯人工水草处理污水技术领域,具体涉及一种酿酒废水处理的石墨烯人工水草及其制备方法。针对现有缺乏一种成本低、吸附效果好、使用寿命长的人工水草的问题,本发明提供了一种酿酒废水处理的石墨烯人工水草,其结构包括:石墨烯改性树脂发泡材料、石墨烯改性无纺布和绒毛,所述石墨烯改性无纺布附着于石墨烯改性树脂发泡材料的上、下表面,所述绒毛位于石墨烯改性无纺布上。本发明还提供了上述人工水草的制备方法。本发明采用石墨烯改性树脂发泡材料作为填充物,外层包围石墨烯改性无纺布,石墨烯自身比表面积大、吸附能力强,还具有无污染、零排放、低成本的优势。同时,还提高了人工水草的使用寿命,应用前景广阔。
Description
技术领域
本发明属于石墨烯人工水草处理污水技术领域,具体涉及一种酿酒废水处理的石墨烯人工水草及其制备方法。
背景技术
酿酒废水是指从白酒生产到贮存陈化过程中所产生的工业废水,富含淀粉、还原糖、有机酸、酯类、醇类等,这些大分子物质难以降解,是引起污染的主要原因。此外,由于我国白酒种类多样,在原材料、酿造工艺和主体香气成分上的差异,这也很大程度上导致了酿酒废水的不同。当前,水资源严重短缺,水污染形势日益严峻,废水排放标准更加严格,而酿酒废水性质独特不一,因此酿酒废水的治理需要追根溯源、统筹把控和技术整合,废水预处理成为一个重要研究方向。
人工水草修复技术属于生物-生态修复技术,在我国的应用尚处于起步阶段,它是一种生物膜载体技术,采用耐酸碱、耐污、柔韧性很强的仿水草材料,通过模拟污水处理中的植物净化原理和优化生物填料以利于生物膜的形成和再生,不受透明度、光照等限制,从而大大提高污水处理的效果。
现有人工水草使用的材料主要包括合成纤维、碳纤维等。合成纤维主要是由聚氯乙烯、维尼纶、聚烯烃等高分子材料制备而成,其孔隙发达,微孔较多,吸附作用强,性能优良,可有效的去除有害污染物。
碳纤维是由调制沥青和淀粉塑料以及α-甲基纤维素混合制得,具有吸附面积大、可降解的作用。现有的人工水草中,大多采用碳纤维材料,除了碳纤维本身具有吸附性外,还会添加复合微生物菌剂,在人工水草表面快速形成生物膜,提高吸附效果。但碳纤维材料制备的人工水草存在更换频率较高、使用寿命短的缺点。
目前,有研究发现,可将石墨烯材料用于制备人工水草。
专利CN109092281A提供了一种在人工水草表面附着石墨烯光催化剂的方法,该专利采用的是现有的人工水草,在现有人工水草上镀一层石墨烯改性光催化剂膜,其达到的效果是提高人工水草与光催化剂膜之间的吸附力,使光催化剂不易脱落,提高人工水草的去污能力。该方法镀膜的操作较为复杂,镀膜成本高,不适宜规模化生产。
专利CN112850691A提供了一种石墨烯改性材料及制备方法和应用,该专利提供了一种用于药物提取纯化、稀土元素分离纯化及污水的重金属处理等领域的改性石墨烯材料,先制备得到氧化石墨烯@Fe3O4材料,然后对氧化石墨烯表面进行还原处理,得到改性石墨烯,最后于改性石墨烯表面在活化剂的作用下,接枝弱酸性聚丙烯酸树脂,得到石墨烯改性材料。该专利制备的改性石墨烯材料主要应用于药物提取纯化、稀土元素分离纯化及污水的重金属处理中,无法处理污水中的其他污染物,因此不适宜用在酿酒废水的处理中。
综上可见,在采用人工水草处理酿酒废水的领域,目前还无法提供一种成本低、吸附效果好、使用寿命长的人工水草,亟待开发。
发明内容
本发明要解决的技术问题为:在酿酒废水处理时,还缺乏一种成本低、吸附效果好、使用寿命长的人工水草的问题。
本发明解决上述技术问题的技术方案为:提供一种酿酒废水处理的石墨烯人工水草的制备方法。该方法包括以下步骤:
a、将氧化石墨烯与聚丙烯按重量比0.1-5:100混合,得到石墨烯改性聚丙烯;将石墨烯改性聚丙烯、反应助剂、引发剂按重量比100:0.4-60:0.01-10混合后,在150-260℃下熔融,利用双螺杆挤出装置挤出成型,得到发泡聚丙烯材料;
b、将石墨烯加入氧化石墨烯的水分散液中,通过乳化均质机进行分散,得到氧化石墨烯分散液;将分散液置于水热反应釜中,150-200℃下反应1-3h,冷却至室温,干燥,得到石墨烯复合添加剂;
c、将步骤b得到的石墨烯复合添加剂与聚丙烯按重量比1-10:100预混,经过熔喷设备连续制备带绒毛的石墨烯改性无纺布;
d、在步骤a得到的发泡材料上、下表面分别粘结一层步骤c制备得到的石墨烯改性无纺布,制备成细绳状的石墨烯人工水草。
其中,上述酿酒废水处理的石墨烯人工水草的制备方法中,步骤a所述的反应助剂主要成分包括烯烃和烷烃。
其中,所述烷烃、烯烃的比例范围为100:1-40之间。
其中,上述酿酒废水处理的石墨烯人工水草的制备方法中,步骤a所述的引发剂为过氧化苯甲酸叔丁酯或过氧化二异丙苯。
其中,上述酿酒废水处理的石墨烯人工水草的制备方法中,步骤a所述的双螺杆挤出装置的参数设置为:加料段温度设置为160℃-210℃,反应段温度为170-220℃,挤出段温度为140℃-220℃,机头温度为100-200℃。
其中,上述酿酒废水处理的石墨烯人工水草的制备方法中,步骤b所述的石墨烯与氧化石墨烯分散液质量比为5-40:100。
其中,上述酿酒废水处理的石墨烯人工水草的制备方法中,步骤b所述的氧化石墨烯的水分散液中,氧化石墨烯浓度为1-20wt%。
其中,上述酿酒废水处理的石墨烯人工水草的制备方法中,步骤c所述的聚丙烯为片状的聚丙烯。
其中,上述酿酒废水处理的石墨烯人工水草的制备方法中,步骤d所述的发泡材料厚度为2-3mm,石墨烯改性无纺布厚度为1-1.5mm,改性无纺布上附着有长度2-5mm的绒毛。
本发明还提供了一种上述方法直接制备得到的酿酒废水处理的石墨烯人工水草。
具体的,本发明的酿酒废水处理的石墨烯人工水草,其结构包括:石墨烯改性树脂发泡材料、石墨烯改性无纺布和绒毛,所述石墨烯改性无纺布附着于石墨烯改性树脂发泡材料的上、下表面,所述绒毛位于石墨烯改性无纺布上。
本发明还提供了一种上述酿酒废水处理的石墨烯人工水草的使用方法,将石墨烯人工水草组合成石墨烯人工水草帘,固定在聚乙烯支架上,置于废水中进行酿酒废水的处理。
在使用时,采用聚乙烯制作架台固定支架,聚乙烯管材具备链接功能,固定支架可根据酿酒企业内废水收集池的尺寸调节大小;采用多根细绳状石墨烯人工水草进行组合成为石墨烯人工水草帘,然后固定在支架上,固定支架上可放置多个石墨烯人工水草帘;将固定支架放置多根绳索,然后将固定支架放置于酿酒废水收集池内,便于后续管理和维护。
本发明的有益效果为:
本发明提供了一种用于酿酒废水处理的石墨烯人工水草及其制备方法,采用石墨烯改性树脂发泡材料作为填充物,外层包围石墨烯改性无纺布,利用石墨烯材料自身比表面积大、吸附能力强的特性,具有无污染、零排放、低成本、可回收的优势。本发明将石墨烯水草制备成石墨烯改性发泡材料和石墨烯改性无纺布的形式,可以增强人工水草表面粗糙度,有利于增加微生物与人工水草间的接触面积,缩减挂膜时间,吸附效果更好。此外,由于石墨烯优异的增韧特质,石墨烯人工水草机械强度更大,在水体里飘浮耐冲击,稳定性强,使用寿命比普通人工水草长。本发明的石墨烯人工水草无需再增设其他辅助设备,利用聚乙烯做固定支架,形成架台结构,连接处采用螺栓装置,便于人工水草的放置和后期维修管理,具有经济可行性。
附图说明
图1所示为本发明酿酒废水处理的石墨烯人工水草结构图,结构包括石墨烯改性树脂发泡材料、石墨烯改性无纺布和绒毛,石墨烯改性无纺布附着于石墨烯改性树脂发泡材料的上、下表面,绒毛位于石墨烯改性无纺布上;
图2所示为制备人工水草的流程图,将石墨烯人工水草经过裁剪,组合收卷,可以得到细绳状石墨烯人工水草;
图3所示为石墨烯人工水草组成的石墨烯人工水草帘,多根细绳状石墨烯人工水草进行组合成为石墨烯人工水草帘;
图4所示为石墨烯人工水草帘的固定结构示意图,石墨烯人工水草帘固定在支架上,架台上的多个支架上可对应放置多个石墨烯人工水草帘。
具体实施方式
本发明主要针对酿酒废水开发一种净化水质的人工水草,由于酿酒行业的特殊性,酿酒废水与其他生活污水或其他污染废水中的杂质存在不同,采用现有的人工水草除杂效果普通,并且现有的人工水草使用寿命偏短,不利于长期使用。在中国白酒谱系中,有酱香型、浓香型、清香型、米香型、凤香型、芝麻香型、豉香型、特香型、老白干香型、兼香型、馥郁香型等不同种类的白酒,每种类型白酒的制备方法不同,产生的废水中的COD、氨氮、总氮、总磷也各不相同。但是污水处理厂对酿酒废水入水是有要求的,酿酒企业必须经过预处理后,达到相应指标才可排入污水处理厂进行处理。其中要求:污水中的化学需氧量排放限值为40mg/L,氨氮排放限值为2.0mg/L,总磷排放限值为0.4mg/L。
为了达到上述酿酒废水的处理效果,本发明提供了一种酿酒废水处理的石墨烯人工水草的制备方法,包括以下步骤:
a、将氧化石墨烯与聚丙烯按重量比0.1-5:100混合,得到石墨烯改性聚丙烯;将石墨烯改性聚丙烯、反应助剂、引发剂按重量比100:0.4-60:0.01-10混合后,在150-260℃下熔融,利用双螺杆挤出装置挤出成型,得到发泡聚丙烯材料;
b、将石墨烯加入氧化石墨烯的水分散液中,通过乳化均质机进行分散,得到氧化石墨烯分散液;将分散液置于水热反应釜中,150-200℃下反应1-3h,冷却至室温,干燥,得到石墨烯复合添加剂;
c、将步骤b得到的石墨烯复合添加剂与聚丙烯按重量比1-10:100预混,经过熔喷设备连续制备带绒毛的石墨烯改性无纺布;
d、在步骤a得到的发泡材料上、下表面分别粘结一层步骤c制备得到的石墨烯改性无纺布,制备成细绳状的石墨烯人工水草。
本发明还提供了一种上述方法制备得到的石墨烯人工水草,其结构包括:石墨烯改性树脂发泡材料1、石墨烯改性无纺布2和绒毛3,所述石墨烯改性无纺布附着于石墨烯改性树脂发泡材料的上、下表面,所述绒毛位于石墨烯改性无纺布上。
本发明的石墨烯人工水草的特殊结构,让人工水草与废水的接触面更大了,可承载更高密度的好氧菌、厌氧菌、兼性好氧(厌氧)菌、原生动物以及藻类,更有利于处理废水中的主要污染物;废水池内的水并非静止状态,绒毛状更有利于随水飘浮,加速反应(意思类似于曝气),因此本发明的石墨烯人工水草除杂效果更好,并且使用寿命更长。
本发明还提供了一种上述酿酒废水处理的石墨烯人工水草的使用方法,将石墨烯人工水草组合成石墨烯人工水草帘,固定在聚乙烯支架上,置于废水中进行酿酒废水的处理。
在使用时,采用聚乙烯制作架台固定支架,聚乙烯管材具备链接功能,固定支架可根据酿酒企业内废水收集池的尺寸调节大小;采用多根细绳状石墨烯人工水草进行组合成为石墨烯人工水草帘,然后固定在支架上,固定支架上可放置多个石墨烯人工水草帘;将固定支架放置多根绳索,然后将固定支架放置于酿酒废水收集池内,便于后续管理和维护。
本发明采用石墨烯人工水草采用石墨烯改性树脂发泡材料作为填充物,石墨烯是已知强度最高的材料之一,同时还具有很好的韧性,因此采用石墨烯改性树脂发泡材料作为填充物,不仅能增强耐用性,提高寿命;同时还能降低重量,更利于在水体里飘浮。填充物不局限于本发明上述方法制备得到的改性树脂发泡材料,可替换成其他性能优异的发泡材料,比如PE、EVA等。
本发明石墨烯水草的关键是在于石墨烯改性无纺布的制备和使用,那么在无纺布的制备上,本发明采用石墨烯复合添加剂与聚丙烯切片共同制备改性无纺布,由于聚丙烯具有耐腐蚀等优异性能,采用其作为原料制作的人工水草具有良好韧性和强度。同时,经过大量的筛选,本发明发现当石墨烯复合添加剂与聚丙烯切片的重量比设置为1-10:100时效果最好,石墨烯复合添加剂含量过低,起不到增韧和增加强度的作用,但不是含量越高,效果越好,实验显示添加量过高时,反而会起到相反的作用。
本发明制备得到的石墨烯人工水草比表面积大,一方面可承载更高密度的好氧菌、厌氧菌、兼性好氧(厌氧)菌、原生动物以及藻类;另一方面吸附效果好,表面粗糙,可迅速挂膜(生物膜),让水草系统更快开展工作,因此,草比其他现有的水草对杂质的去除效果更好。同时,由于石墨烯增强材料的韧性和强度,本发明的人工水草使用寿命更长,本发明人工水草的使用寿命可达到12-14年;现有大概为8-10年,提高40%。
下面将通过实施例对本发明的具体实施方式做进一步的说明,但不表示将本发明的保护范围限制在实施例所述范围内。
实施例1采用本发明方法制备酿酒废水处理的石墨烯人工水草
具体的操作步骤如下:
a.首先将氧化石墨烯与聚丙烯按1:100比例进行混合均匀,将石墨烯改性聚丙烯、反应助剂和引发剂按100:30:8的重量比例均匀混合在一起,得到原料。
b.将原料混合熔融,利用双螺杆挤出装置挤出成型,加料段温度设置为195℃,反应段温度为210℃,挤出段温度为200℃,机头温度为195℃。得到发泡聚丙烯材料。
c.将10份石墨烯加入50质量份氧化石墨烯的水分散液,通过乳化均质机进行分散,得到氧化石墨烯分散液,使得石墨烯的质量浓度为4%。
d.将步骤c所得分散液置于水热反应釜中,180℃下反应2h,冷却至室温后取出反应物干燥,得到石墨烯复合添加剂。
e.将步骤d所得石墨烯复合添加剂与聚丙烯切片预混,经过熔喷设备连续制备带绒毛的石墨烯改性无纺布。石墨烯基复合添加剂和聚丙烯的质量比为5:100。
f.在发泡材料表面粘结一层带绒毛的石墨烯改性无纺布,经过裁剪制成5cm长细绳状的石墨烯人工水草(如图1、图2所示)。
g.将8根细绳状石墨烯人工水草组合成石墨烯人工水草帘,固定在聚乙烯支架上(如图3-图4所示),则可以投入使用。
实施例2采用本发明方法制备酿酒废水处理的石墨烯人工水草
与实施例1的区别在于,裁剪的长细绳状石墨烯人工水草长为10cm。
实施例3采用本发明方法制备酿酒废水处理的石墨烯人工水草
与实施例1的区别在于,裁剪的长细绳状石墨烯人工水草长为10cm。石墨烯的质量浓度为2%。
实施例4采用本发明方法制备酿酒废水处理的石墨烯人工水草
与实施例1的区别在于,裁剪的长细绳状石墨烯人工水草长为10cm。石墨烯的质量浓度为3%。
实施例5采用本发明方法制备酿酒废水处理的石墨烯人工水草
与实施例1的区别在于,裁剪的长细绳状石墨烯人工水草长为10cm。石墨烯的质量浓度为5%。
对比例1不采用本发明方法制备酿酒废水处理的石墨烯人工水草
与实施例1的区别在于,采用石墨烯阿科曼生态基技术制备的人工水草,参与污染物去除的对比。
对比例2不采用本发明方法制备酿酒废水处理的石墨烯人工水草
与实施例1的区别在于,采用石墨烯超细立体纤维人工水草,参与污染物去除的对比。
对实施例和对比例制备得到的人工水草对于废水中的杂志去除率进行比较,结果如下所示。
不同形态的人工水草对白酒酿酒废水中主要污染物的去除率如表1所示。
表1不同形态的人工水草对白酒酿酒废水中主要污染物的去除率对比
由表1可看出:采用本发明方法制备成的石墨烯人工水草对白酒酿酒废水中的主要污染物去除率都要优于现有的人工水草(对比例1的石墨烯阿科曼生态基和对比例2的石墨烯超细立体纤维人工水草),而石墨烯人工水草的长度也会影响吸附效果,其中10cm人工水草对白酒酿酒废水中的主要污染物去除率优于5cm人工水草。
而当石墨烯人工水草的长度均为10cm时,不同的石墨烯比例也会影响到去除效果。下表2所示为不同石墨烯比例的人工水草对白酒酿酒废水中主要污染物去除效果的影响。
表2不同石墨烯比例的人工水草对白酒酿酒废水主要污染物的去除率对比
下表3所示为不同石墨烯比例的人工水草对人工配制污水中主要污染物去除效果的影响。
表3不同石墨烯比例的人工水草对人工配制污水中主要污染物去除率对比
由表2、表3的数据可看出:在石墨烯人工水草长度相同(10cm)的情况下,实施例4(石墨烯的质量浓度为3%的石墨烯人工水草)对污染物的综合去除效果最好。
石墨烯人工水草采用石墨烯改性树脂发泡材料作为填充物,外层包围石墨烯改性无纺布。通过和其他方案对比,石墨烯人工水草对污染水体中的污染物去除具有优异的效果,对酿酒废水中的主要污染物具有较强的去除能力。
Claims (7)
1.酿酒废水处理的石墨烯人工水草的制备方法,其特征在于,包括以下步骤:
a、将氧化石墨烯与聚丙烯按重量比1:100混合,得到石墨烯改性聚丙烯;将石墨烯改性聚丙烯、反应助剂、引发剂按重量比100:30:8混合后,在195℃下熔融,利用双螺杆挤出装置挤出成型,得到发泡聚丙烯材料;所述的反应助剂主要是由烯烃和烷烃混合而成,烷烃、烯烃的比例为100:1-40;所述的引发剂为过氧化苯甲酸叔丁酯或过氧化二异丙苯;
b、将石墨烯加入氧化石墨烯的水分散液中,通过乳化均质机进行分散,得到氧化石墨烯分散液;将分散液置于水热反应釜中,180℃下反应2h,冷却至室温,干燥,得到石墨烯复合添加剂;
c、将步骤b得到的石墨烯复合添加剂与聚丙烯按重量比5:100预混,经过熔喷设备连续制备带绒毛的石墨烯改性无纺布;
d、在步骤a得到的发泡材料上、下表面分别粘结一层步骤c制备得到的石墨烯改性无纺布,制备成细绳状的石墨烯人工水草;所述的发泡材料厚度为2-3mm,石墨烯改性无纺布厚度为1-1.5mm,改性无纺布上附着有长度2-5mm的绒毛。
2.根据权利要求1所述的酿酒废水处理的石墨烯人工水草的制备方法,其特征在于:步骤a所述的双螺杆挤出装置的参数设置为:加料段温度设置为195℃,反应段温度为210℃,挤出段温度为200℃,机头温度为195℃。
3.根据权利要求1所述的酿酒废水处理的石墨烯人工水草的制备方法,其特征在于:步骤b所述的石墨烯与氧化石墨烯分散液质量比为5-40:100。
4.根据权利要求1所述的酿酒废水处理的石墨烯人工水草的制备方法,其特征在于:步骤b所述的氧化石墨烯的水分散液中,氧化石墨烯浓度为1-20wt%。
5.根据权利要求1所述的酿酒废水处理的石墨烯人工水草的制备方法,其特征在于:步骤c所述的聚丙烯为片状的聚丙烯。
6.权利要求1-5任一项所述的酿酒废水处理的石墨烯人工水草的制备方法制备得到的酿酒废水处理的石墨烯人工水草。
7.根据权利要求6所述的酿酒废水处理的石墨烯人工水草,其特征在于,结构包括:石墨烯树脂发泡材料、石墨烯改性无纺布和绒毛,所述石墨烯改性无纺布附着于石墨烯树脂发泡材料的上、下表面,所述绒毛位于石墨烯改性无纺布上。
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