CN108299564A - 一种用于混凝处理含丝多组分面料印染废水的疏水纤维素基絮凝材料的制备方法 - Google Patents
一种用于混凝处理含丝多组分面料印染废水的疏水纤维素基絮凝材料的制备方法 Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
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Abstract
本发明公开了一种用于混凝处理含丝多组分面料印染废水的疏水纤维素基絮凝材料的制备方法。采用方法的要点是将毛竹纤维素经高碘酸钾处理将其醛基化,然后采用硅烷疏水改性醛基化纤维素,制备可用于混凝处理含丝多组分面料印染废水的纤维素基絮凝材料。该方法快速、高效,特别适用于混凝处理含丝多组分面料印染废水的纤维素基絮凝材料制备。本发明在制备纤维素基絮凝材料的纤维原料中引入毛竹资源,扩充了其原料范围,可切实提高我国竹区农民的经济收入;该絮凝材料在混凝印染废水中悬浮性污染物的同时,还可实现其有机污染物的去除,具有重要的环境效益。
Description
技术领域
本发明涉及一种絮凝材料的制备方法,特别涉及一种用于混凝处理含丝多组分面料印染废水的疏水纤维素基絮凝材料的制备方法,属于有机高分子材料技术领域。
背景技术
随着工业发展的加剧,工业废水排放造成了严重的环境和生态破坏,特别是印染废水,由于印染过程中会使用到活性、酸性染料以及大量印染助剂、染料溶剂,在印染废水中不可避免地会含有大量有机污染物,如:苯及酚类、胺类、酯类、醇类、烷烃、烯烃、醛类、酮类等。用于废水处理过程中,有很多种方法,如离子交换法、生化法、电渗析法、絮凝沉淀法、化学氧化法、吸附法、膜过滤法等等,而其中成本最低、工艺最简单的是絮凝沉淀法,尤其在去除那些含有悬浮颗粒,染料和重金属离子的废水中特别起作用。但传统的絮凝剂难以实现对水体中有机污染物的高效去除。因此,迫切需要能够有效地去除水体中有机污染物的絮凝材料。
近来,鉴于其成本低,可更新性,生物相容性,无毒性和可生物降解性等因素,天然高分子材料如纤维素已被用作去除有机物的材料。纤维素作为自然界含量最丰富的天然有机高分子化合物,具有可再生、易降解等特性,是由D-脱水葡萄糖基重复单元通过β-1,4-苷键联接形成的线性均一聚糖。在每个D-脱水葡萄糖基单元的C2、C3、C6上均存在一个活性羟基(-OH),这为纤维素的功能化改性提供了可能。但是,由于天然纤维素分子链上含有亲水性基团,导致纤维素基絮凝剂具有很高的亲水性能。一方面,这些亲水性的极性基团可以促进絮凝剂与工业废水中的极性悬浮或微溶性污染物通过电中和机理结合,达到絮凝沉淀目的;但另一方面,若纤维素基絮凝剂的亲水性过高,难以实现对水体中有机污染物的吸附,因此,需对纤维素进行表面修饰降低表面能,以平衡两者之间的关系。基于上述原因,研制开发疏水可控、高效安全的新型纤维素基絮凝材料,已成为提升絮凝剂在工业废水中去除有机污染物效率的必要手段。
在纤维素基絮凝剂制备领域,中国专利(ZL 201710906907.8)“一种聚合氯化铝-壳聚糖复合絮凝剂及其制备方法与应用”首先采用铝灰、水、浓盐酸制的聚合氯化铝,然后将壳聚糖/乙酸溶液滴加到多聚磷酸钠溶液中搅拌,最后加入聚合氯化铝,制得聚合氯化铝-壳聚糖复合絮凝剂。并对使用制得聚合氯化铝-壳聚糖复合絮凝剂处理生活污水的效果做出来说明;中国专利(ZL201710872400.5)“一种磁性疏水改性阳离子聚丙烯酰胺除油絮凝剂的制备方法”采用十二烷基葡萄苷、二甲基二烯丙基氯化铵、丙烯酰胺、光引发剂在氮气、低压紫外光照条件下制得乳色胶体,再添加磁性纳米颗粒和硫酸铵,最后制得了除油絮凝剂;美国专利(US 20090137720A1)“Flocculant composition and method formanufacturing the same”通过利用交联水溶性聚合物和线性水溶性聚合物的优点并根据污泥的粒度分布的形式改变交联水溶性聚合物与线性水溶性聚合物的配合比而获得的粒子,絮凝剂组合物具有优异的粘附到悬浮颗粒的能力,不会引起污泥粘度的增加,在机械脱水过程中提供良好的排水能力;美国专利(US 20130299433A1)“Plant-derivedflocculant,flocculant mixture,method of flocculation,and method for preparingplant-derived flocculant”公开了具有较高絮凝能力的植物来源的絮凝剂和絮凝剂混合物,所述植物来源的絮凝剂包括黄麻的干物质,秋海棠的干物质,香蕉的干物质和黄麻的干物质中的至少一种,有良好的絮凝能力。截至目前,还未见到利用毛竹作为纤维素来源物,用以制备用于高效处理含丝多组分面料印染废水的纤维素基絮凝剂的相关工艺技术出现。
毛竹属于速生植物资源,具有生长速度快、成材周期短、纤维含量高等优点,其纤维形态和纤维细胞含量接近甚至高于一般阔叶木。充分利用我国丰富的毛竹资源,制备高附加值全降解纤维素基絮凝材料,切实提高我国竹区农民经济收入;该絮凝材料在混凝含丝多组分面料印染废水中悬浮性污染物的同时,还可实现其有机污染物的去除,具有重要的环境效益。
发明内容
为了实现絮凝剂在混凝含丝多组分面料印染废水中悬浮性污染物的同时,去除其有机污染物,并克服目前制备纤维素基絮凝剂存在的纤维原料供给不足、价格昂贵、生长周期较长等问题,本发明的目的是提供一种用于混凝处理含丝多组分面料印染废水的疏水纤维素基絮凝材料的制备方法。
为实现上述目的,本发明的技术方案是采用以下步骤:
一种用于混凝处理含丝多组分面料印染废水的疏水纤维素基絮凝材料的制备方法,其特征在于,包括以下步骤:
1)将毛竹浆板采用植物粉碎机粉碎,经50目筛网过滤,得到粒径小于等于0.30mm的毛竹粉末;
2)将步骤1)中得到的2g粒径小于等于0.30mm的毛竹粉末溶解于氢氧化钾和硫脲溶液中,在机械搅拌作用下使其均匀分散,得到毛竹纤维素溶液;
3)将步骤2)中得到的毛竹纤维素溶液在-15℃中冷冻120-200min,得到毛竹纤维素均相溶液;
4)称取1-2g高碘酸钾加入到步骤3)中得到的毛竹纤维素均相溶液中,在机械搅拌作用下,置于75-85℃反应240-360min,滴加2mL乙二醇终止反应,用蒸馏水洗涤至溶液呈中性,进行冷冻干燥,得到醛化毛竹纤维素粉末;
5)将步骤4)中得到的1g醛化毛竹纤维素粉末溶解于氢氧化钾水溶液中,在机械搅拌作用下,使其均匀分散,得到醛化纤维素溶液;
6)将步骤5)中得到的醛化纤维素溶液置于65-75℃下,氮气氛围下机械搅拌15min,加入0.3-0.9g硅烷,反应120-240min,用蒸馏水洗涤至溶液呈中性,进行冷冻干燥,最终得到疏水纤维素基絮凝材料。
所述的氢氧化钾和硫脲溶液为12wt%氢氧化钾和20wt%硫脲溶液,毛竹粉末在12wt%氢氧化钾和20wt%硫脲溶液中的质量分数为4-6wt%;氢氧化钾水溶液的质量分数为5wt%,醛化纤维素在5wt%氢氧化钾水溶液中的质量分数为2-4wt%。
所述的硅烷为十六烷基三甲氧基硅烷、正辛基三乙氧基硅烷、氨基丙基乙氧基硅烷中的一种。
与背景技术相比,本发明具有的有益效果是:
本发明在制备疏水纤维素基絮凝材料的纤维原料中引入毛竹资源,提出高值化利用毛竹资源的一条创新思路,符合国家发展循环经济政策,可切实提高我国竹区农民的经济收入;该絮凝材料在混凝含丝多组分面料印染废水中悬浮性污染物的同时,还可实现其有机污染物的去除。
具体实施方式
下面结合具体实施例对本发明作进一步说明。
实施例1:
1)将毛竹浆板采用植物粉碎机粉碎,经50目筛网过滤,得到粒径小于等于0.30mm的毛竹粉末;
2)将步骤1)中得到的2g粒径小于等于0.30mm的毛竹粉末溶解于质量分数分别为12wt%氢氧化钾和20wt%硫脲的溶液中,在机械搅拌作用下使其均匀分散,得到毛竹纤维素溶液;
3)将步骤2)中得到的毛竹纤维素溶液在-15℃中冷冻120min,得到质量分数为4wt%的毛竹纤维素均相溶液;
4)称取1g高碘酸钾加入到步骤3)中得到的毛竹纤维素均相溶液中,在机械搅拌作用下,置于75℃反应280min,滴加2mL乙二醇终止反应,用蒸馏水洗涤至溶液呈中性,进行冷冻干燥,得到醛化毛竹纤维素粉末;
5)将步骤4)中得到的1g醛化毛竹纤维素粉末溶解于质量分数为5wt%的氢氧化钾水溶液中,在机械搅拌作用下,使其均匀分散,得到质量分数为2wt%的醛化纤维素溶液;
6)将步骤5)中得到的醛化纤维素溶液置于65℃下,氮气氛围下机械搅拌15min,加入0.3g正辛基三乙氧基硅烷,反应180min,用蒸馏水洗涤至溶液呈中性,进行冷冻干燥,最终得到疏水纤维素基絮凝材料(a)。
实施例2:
1)将毛竹浆板采用植物粉碎机粉碎,经50目筛网过滤,得到粒径小于等于0.30mm的毛竹粉末;
2)将步骤1)中得到的2g粒径小于等于0.30mm的毛竹粉末溶解于质量分数分别为12wt%氢氧化钾和20wt%硫脲的溶液中,在机械搅拌作用下使其均匀分散,得到毛竹纤维素溶液;
3)将步骤2)中得到的毛竹纤维素溶液在-15℃中冷冻160min,得到质量分数为5wt%的毛竹纤维素均相溶液;
4)称取1.5g高碘酸钾加入到步骤3)中得到的毛竹纤维素均相溶液中,在机械搅拌作用下,置于80℃反应360min,滴加2mL乙二醇终止反应,用蒸馏水洗涤至溶液呈中性,进行冷冻干燥,得到醛化毛竹纤维素粉末;
5)将步骤4)中得到的1g醛化毛竹纤维素粉末溶解于质量分数为5wt%的氢氧化钾水溶液中,在机械搅拌作用下,使其均匀分散,得到质量分数为3wt%的醛化纤维素溶液;
6)将步骤5)中得到的醛化纤维素溶液置于70℃下,氮气氛围下机械搅拌15min,加入0.6g氨基丙基乙氧基硅烷,反应180min,用蒸馏水洗涤至溶液呈中性,进行冷冻干燥,最终得到疏水纤维素基絮凝材料(b)。
实施例3:
1)将毛竹浆板采用植物粉碎机粉碎,经50目筛网过滤,得到粒径小于等于0.30mm的毛竹粉末;
2)将步骤1)中得到的2g粒径小于等于0.30mm的毛竹粉末溶解于质量分数分别为12wt%氢氧化钾和20wt%硫脲的溶液中,在机械搅拌作用下使其均匀分散,得到毛竹纤维素溶液;
3)将步骤2)中得到的毛竹纤维素溶液在-15℃中冷冻200min,得到质量分数为5wt%的毛竹纤维素均相溶液;
4)称取1.5g高碘酸钾加入到步骤3)中得到的毛竹纤维素均相溶液中,在机械搅拌作用下,置于80℃反应240min,滴加2mL乙二醇终止反应,用蒸馏水洗涤至溶液呈中性,进行冷冻干燥,得到醛化毛竹纤维素粉末;
5)将步骤4)中得到的1g醛化毛竹纤维素粉末溶解于质量分数为5wt%的氢氧化钾水溶液中,在机械搅拌作用下,使其均匀分散,得到质量分数为2wt%的醛化纤维素溶液;
6)将步骤5)中得到的醛化纤维素溶液置于75℃下,氮气氛围下机械搅拌15min,加入0.6g十六烷基三甲氧基硅烷,反应120min,用蒸馏水洗涤至溶液呈中性,进行冷冻干燥,最终得到疏水纤维素基絮凝材料(c)。
实施例4:
1)将毛竹浆板采用植物粉碎机粉碎,经50目筛网过滤,得到粒径小于等于0.30mm的毛竹粉末;
2)将步骤1)中得到的2g粒径小于等于0.30mm的毛竹粉末溶解于质量分数分别为12wt%氢氧化钾和20wt%硫脲的溶液中,在机械搅拌作用下使其均匀分散,得到毛竹纤维素溶液;
3)将步骤2)中得到的毛竹纤维素溶液在-15℃中冷冻180min,得到质量分数为6wt%的毛竹纤维素均相溶液;
4)称取2g高碘酸钾加入到步骤3)中得到的毛竹纤维素均相溶液中,在机械搅拌作用下,置于85℃反应300min,滴加2mL乙二醇终止反应,用蒸馏水洗涤至溶液呈中性,进行冷冻干燥,得到醛化毛竹纤维素粉末;
5)将步骤4)中得到的1g醛化毛竹纤维素粉末溶解于质量分数为5wt%的氢氧化钾水溶液中,在机械搅拌作用下,使其均匀分散,得到质量分数为4wt%的醛化纤维素溶液;
6)将步骤5)中得到的醛化纤维素溶液置于70℃下,氮气氛围下机械搅拌15min,加入0.9g氨基丙基乙氧基硅烷,反应240min,用蒸馏水洗涤至溶液呈中性,进行冷冻干燥,最终得到疏水纤维素基絮凝材料(d)。
测定实施例1、2、3、4制备的疏水纤维素基絮凝材料应用于嵊州某企业含丝多组分面料印染废水的混凝处理过程,并测定其浊度和COD去除率数据,表1为实施例1、2、3、4制备的疏水纤维素基絮凝材料处理嵊州某企业含丝多组分面料印染废水的浊度和COD去除率测定结果。由表1可看出,制备的疏水纤维素基絮凝材料对含丝多组分面料印染废水的浊度去除率在96%-98%,COD去除率在85%-87%,浊度和COD去除效果显著,表明该疏水纤维素基絮凝材料对含丝多组分面料印染废水混凝工段具有较好的处理效果,有望替代传统的印染废水絮凝剂应用于企业的含丝多组分面料印染废水混凝工段。
表1
以上列举的仅是本发明的具体实施例。本发明不限于以上实施例,还可以有许多变形。本领域的普通技术人员能从本发明公开的内容直接导出或联想到的所有变形,均应认为是本发明的保护范围。
Claims (3)
1.一种用于混凝处理含丝多组分面料印染废水的疏水纤维素基絮凝材料的制备方法,其特征在于,包括以下步骤:
1)将毛竹浆板采用植物粉碎机粉碎,经50目筛网过滤,得到粒径小于等于0.30mm的毛竹粉末;
2)将步骤1)中得到的2g粒径小于等于0.30mm的毛竹粉末溶解于氢氧化钾和硫脲溶液中,在机械搅拌作用下使其均匀分散,得到毛竹纤维素溶液;
3)将步骤2)中得到的毛竹纤维素溶液在-15℃中冷冻120-200min,得到毛竹纤维素均相溶液;
4)称取1-2g高碘酸钾加入到步骤3)中得到的毛竹纤维素均相溶液中,在机械搅拌作用下,置于75-85℃反应240-360min,滴加2mL乙二醇终止反应,用蒸馏水洗涤至溶液呈中性,进行冷冻干燥,得到醛化毛竹纤维素粉末;
5)将步骤4)中得到的1g醛化毛竹纤维素粉末溶解于氢氧化钾水溶液中,在机械搅拌作用下,使其均匀分散,得到醛化纤维素溶液;
6)将步骤5)中得到的醛化纤维素溶液置于65-75℃下,氮气氛围下机械搅拌15min,加入0.3-0.9g硅烷,反应120-240min,用蒸馏水洗涤至溶液呈中性,进行冷冻干燥,最终得到疏水纤维素基絮凝材料。
2.根据权利要求1所述的一种用于混凝处理含丝多组分面料印染废水的疏水纤维素基絮凝材料的制备方法,其特征在于:所述的氢氧化钾和硫脲溶液为12wt%氢氧化钾和20wt%硫脲溶液,毛竹粉末在12wt%氢氧化钾和20wt%硫脲溶液中的质量分数为4-6wt%;氢氧化钾水溶液的质量分数为5wt%,醛化纤维素在5wt%氢氧化钾水溶液中的质量分数为2-4wt%。
3.根据权利要求1所述的一种用于混凝处理含丝多组分面料印染废水的疏水纤维素基絮凝材料的制备方法,其特征在于:所述的硅烷为十六烷基三甲氧基硅烷、正辛基三乙氧基硅烷、氨基丙基乙氧基硅烷中的一种。
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