CN106552592A - 一种木质素磺酸钠氧化改性的水体重金属吸附剂及其制备方法 - Google Patents

一种木质素磺酸钠氧化改性的水体重金属吸附剂及其制备方法 Download PDF

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CN106552592A
CN106552592A CN201611078208.0A CN201611078208A CN106552592A CN 106552592 A CN106552592 A CN 106552592A CN 201611078208 A CN201611078208 A CN 201611078208A CN 106552592 A CN106552592 A CN 106552592A
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尤为
杨燕宗
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Wuxi Longying Environmental Protection Technology Co Ltd
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Abstract

本发明公开了一种木质素磺酸钠氧化改性的水体重金属吸附剂及其制备方法,由以下组分按重量份数配比组成:木质素磺酸钠19~38份、硫酸亚铁12~32份、尿素8~19份、双氧水13~28份、无水乙醇8~17份、甲醛7~18份、氯化锌3~11份、氯化铜4~12份、马来酸酐8~19份、戊二醛8~17份。(1)本发明所述木质素磺酸钠氧化改性的水体重金属吸附剂能够针对性的吸附造纸污水中的重金属污染物,达到富集、絮凝和沉淀的作用;(2)本发明所述木质素磺酸钠氧化改性的水体重金属吸附剂处理后的污水可直接进行二次使用。

Description

一种木质素磺酸钠氧化改性的水体重金属吸附剂及其制备 方法
技术领域
本发明属于环境保护领域,涉及一种水体重金属修复技术,尤其涉及一种木质素磺酸钠氧化改性的水体重金属吸附剂及其制备方法。
背景技术
纤维素被人类利用已有数千年的历史,纤维素在为人类所利用的同时,却伴随着产生了大量废弃的木质素,而木质素至今没有得到普遍、广泛地利用。这不但引起资源的浪费,还严重地污染和影响了环境。我国制衆造纸废水在全国工业废水的所占的比例比较大,工业化学制架的副产物是构成工业木质素主要的来源之一,其自然降解的时间相对比较长,如果进行排放则对环境造成不利的影响,随环境资源问题的日益突出、人类对环境污染和资源危机等问题的认识不断深入和木质素来源丰富,加上其本身优良的物理化学特性,对木质素的充分利用越来越受到人们的重视。
工业木质素目前主要来源于制聚造纸工业的蒸煮废水,木质素的结构类似于苯酚结构,具有在天然条件下不易降解和降低的特点,致使造纸废水难以处理,木质素大多数的用途都是通过燃烧给造纸厂供热给造纸厂,利用形式单一且容易产生温室效应。近年来,由于世界各国对环境保护和能源危机的日益重视,以及天然高分子所具有的可再生、可降解性等性质日益受到重视。木质素这一巨大自然资源的循环利用,更加能促使世界各国引起高度的重视。
研究较经济的提取木质素方法和多样性的改性方法对造纸废液中木质素进行回收和综合利用,是减少污染、增加效益的有效途径。木质素的来源之丰富、日益短缺的能源、对木质素研究的日渐深入决定木质素的经济效益的可持续发展性,因此,对木质素进行接枝等化学改性,对木质素产品的功能进行全面有效开发,是解决造纸黑液作为供热这一单一形式的利用最有效的手段。
木质素磺酸盐同木质素一样,木质素磺酸钠是分子量从几百到几百万的高分子聚合物,其本身的擴酸基团决定了其具有较好的水溶性,可溶于各种不同性质的水溶液,但不溶于乙醇、丙酮等有机溶剂。木质素磺酸盐结构与木质素大致相同,不过也存在差异,木质素磺酸盐大分子环的脂肪侧碳上则多了磺酸盐,由于多了易溶于水的磺酸基而能溶于水,反之,木质素不能溶于水。重金属废水污染与其他的污染有所不用:微量的重金属,可以产生巨大的毒性,能够引起人类和动物患上疾病,这种长期性、持续性毒性的效果非常显著,所以国标要求达标排放的重金属浓度都是非常低的。在微生物潜在作用下,水体中某些重金属离子还进而变成了危害更大的毒瘤;在食物链中,重金属容易富集,这样带来的结果就是危害会成倍地增加。从环境内流入到生物底重金属,会在体内引起高度富集,其富集的倍数以成千上百万倍来计算,这种现象已经出现过的重金属污染重大事件中得到了验证。重金属然后经过食物迸入人体,不同种类的重金属引起的症状都不同,但都是致命的,危害人的身心健康。这种生物浓缩、生物富集、生物放大的特点在重金属废水污染中益突出的。重金属不能被生物所降解,不能凭空消失或转化掉,只能改变其有机化合物种类或者化合价态。由于重金属只能在环境中进行各种形态的相互转化,直接或间接地造成人类和动物的永久性中毒,对人类可谓危害极大。
发明内容
本发明解决的技术问题:为了克服现有技术的缺陷,结合木质素自身的优势,开发其一种新用途,有效处理造纸污水中的重金属污染物,使其达到排放标准,适于二次应用,本发明提供了一种一种木质素磺酸钠氧化改性的水体重金属吸附剂及其制备方法。
技术方案:一种木质素磺酸钠氧化改性的水体重金属吸附剂,由以下组分按重量份数配比组成:木质素磺酸钠19~38份、硫酸亚铁12~32份、尿素8~19份、双氧水13~28份、无水乙醇8~17份、甲醛7~18份、氯化锌3~11份、氯化铜4~12份、马来酸酐8~19份、戊二醛8~17份。
优选的,所述木质素磺酸钠氧化改性的水体重金属吸附剂由以下组分按重量份数配比组成:木质素磺酸钠32份、硫酸亚铁28份、尿素13份、双氧水21份、无水乙醇13份、甲醛13份、氯化锌8份、氯化铜9份、马来酸酐12份、戊二醛14份。
一种木质素磺酸钠氧化改性的水体重金属吸附剂的制备方法,包含以下步骤:
(1)吸附剂基体制备:将硫酸亚铁、尿素、氯化锌和氯化铜混合后,粉碎研磨,至粒径为100~130目,置于烘箱中90~105℃处理65~90分钟;
(2)第一次改性:将木质素磺酸钠加入吸附剂基体中,置于坩埚中加热,边加热边滴加8~25%的硫酸溶液,呈糊状后停止加热;
(3)第二次改性:将双氧水、无水乙醇和甲醛加入经第一次改性后的吸附剂基体中,混合均匀后,26~32℃反应1~3.5小时,坩埚继续加热,至水分完全挥发停止加热;
(4)交联反应:向第二次改性后的吸附剂基体中加入马来酸酐和戊二醛,4~8℃反应40~85分钟;
(5)成品:经交联反应后的产物置于烘箱中,90~105℃反应1~3.5小时即可制得。
优选的,步骤(1)吸附剂基体制备:将硫酸亚铁、尿素、氯化锌和氯化铜混合后,粉碎研磨,至粒径为110目,置于烘箱中100℃处理86分钟。
优选的,步骤(2)第一次改性:将木质素磺酸钠加入吸附剂基体中,置于坩埚中加热,边加热边滴加20%的硫酸溶液,呈糊状后停止加热。
优选的,步骤(3)第二次改性:将双氧水、无水乙醇和甲醛加入经第一次改性后的吸附剂基体中,混合均匀后,30℃反应3小时,坩埚继续加热,至水分完全挥发停止加热。
优选的,步骤(4)交联反应:向第二次改性后的吸附剂基体中加入马来酸酐和戊二醛,7℃反应65分钟。
优选的,步骤(5)成品:经交联反应后的产物置于烘箱中,98℃反应3小时即可制得。
有益效果:(1)本发明所述木质素磺酸钠氧化改性的水体重金属吸附剂能够针对性的吸附造纸污水中的重金属污染物,达到富集、絮凝和沉淀的作用;(2)本发明所述木质素磺酸钠氧化改性的水体重金属吸附剂处理后的污水可直接进行二次使用。
具体实施方式
实施例1
一种木质素磺酸钠氧化改性的水体重金属吸附剂,由以下组分按重量份数配比组成:木质素磺酸钠19份、硫酸亚铁12份、尿素8份、双氧水13份、无水乙醇8份、甲醛7份、氯化锌3份、氯化铜4份、马来酸酐8份、戊二醛8份。
一种木质素磺酸钠氧化改性的水体重金属吸附剂的制备方法,包含以下步骤:
(1)吸附剂基体制备:将硫酸亚铁、尿素、氯化锌和氯化铜混合后,粉碎研磨,至粒径为100目,置于烘箱中90℃处理65分钟;
(2)第一次改性:将木质素磺酸钠加入吸附剂基体中,置于坩埚中加热,边加热边滴加8%的硫酸溶液,呈糊状后停止加热;
(3)第二次改性:将双氧水、无水乙醇和甲醛加入经第一次改性后的吸附剂基体中,混合均匀后,26℃反应1小时,坩埚继续加热,至水分完全挥发停止加热;
(4)交联反应:向第二次改性后的吸附剂基体中加入马来酸酐和戊二醛,4℃反应40分钟;
(5)成品:经交联反应后的产物置于烘箱中,90℃反应1小时即可制得。
实施例2
一种木质素磺酸钠氧化改性的水体重金属吸附剂,由以下组分按重量份数配比组成:木质素磺酸钠32份、硫酸亚铁28份、尿素13份、双氧水21份、无水乙醇13份、甲醛13份、氯化锌8份、氯化铜9份、马来酸酐12份、戊二醛14份。
一种木质素磺酸钠氧化改性的水体重金属吸附剂的制备方法,包含以下步骤:
(1)吸附剂基体制备:将硫酸亚铁、尿素、氯化锌和氯化铜混合后,粉碎研磨,至粒径为110目,置于烘箱中100℃处理86分钟;
(2)第一次改性:将木质素磺酸钠加入吸附剂基体中,置于坩埚中加热,边加热边滴加20%的硫酸溶液,呈糊状后停止加热;
(3)第二次改性:将双氧水、无水乙醇和甲醛加入经第一次改性后的吸附剂基体中,混合均匀后,30℃反应3小时,坩埚继续加热,至水分完全挥发停止加热;
(4)交联反应:向第二次改性后的吸附剂基体中加入马来酸酐和戊二醛,7℃反应65分钟;
(5)成品:经交联反应后的产物置于烘箱中,90~105℃反应1~3.5小时即可制得。
优选的,步骤(4)交联反应:经交联反应后的产物置于烘箱中,98℃反应3小时即可制得。
实施例3
一种木质素磺酸钠氧化改性的水体重金属吸附剂,由以下组分按重量份数配比组成:木质素磺酸钠38份、硫酸亚铁32份、尿素19份、双氧水28份、无水乙醇17份、甲醛18份、氯化锌11份、氯化铜12份、马来酸酐19份、戊二醛17份。
一种木质素磺酸钠氧化改性的水体重金属吸附剂的制备方法,包含以下步骤:
(1)吸附剂基体制备:将硫酸亚铁、尿素、氯化锌和氯化铜混合后,粉碎研磨,至粒径为130目,置于烘箱中105℃处理90分钟;
(2)第一次改性:将木质素磺酸钠加入吸附剂基体中,置于坩埚中加热,边加热边滴加25%的硫酸溶液,呈糊状后停止加热;
(3)第二次改性:将双氧水、无水乙醇和甲醛加入经第一次改性后的吸附剂基体中,混合均匀后,32℃反应3.5小时,坩埚继续加热,至水分完全挥发停止加热;
(4)交联反应:向第二次改性后的吸附剂基体中加入马来酸酐和戊二醛,8℃反应85分钟;
(5)成品:经交联反应后的产物置于烘箱中,105℃反应3.5小时即可制得。
对实施例1~3制备获得的木质素磺酸钠氧化改性的水体重金属吸附剂的性能进行检测,结果如下表所示:
实施例1 实施例2 实施例3
Pb去除率/% 95.3 98.5 96.2
Cu去除率/% 93.2 98.9 97.4
Ni去除率/% 21.4 39.8 36.2
Zn去除率/% 32.1 43.2 38.2
Mn去除率/% 13.2 21.3 19.4
Cd去除率/% 16.4 29.4 23.8

Claims (8)

1.一种木质素磺酸钠氧化改性的水体重金属吸附剂,其特征在于,由以下组分按重量份数配比组成:木质素磺酸钠19~38份、硫酸亚铁12~32份、尿素8~19份、双氧水13~28份、无水乙醇8~17份、甲醛7~18份、氯化锌3~11份、氯化铜4~12份、马来酸酐8~19份、戊二醛8~17份。
2.根据权利要求1所述的一种木质素磺酸钠氧化改性的水体重金属吸附剂,其特征在于,由以下组分按重量份数配比组成:木质素磺酸钠32份、硫酸亚铁28份、尿素13份、双氧水21份、无水乙醇13份、甲醛13份、氯化锌8份、氯化铜9份、马来酸酐12份、戊二醛14份。
3.权利要求1所述的一种木质素磺酸钠氧化改性的水体重金属吸附剂的制备方法,其特征在于,包含以下步骤:
(1)吸附剂基体制备:将硫酸亚铁、尿素、氯化锌和氯化铜混合后,粉碎研磨,至粒径为100~130目,置于烘箱中90~105℃处理65~90分钟;
(2)第一次改性:将木质素磺酸钠加入吸附剂基体中,置于坩埚中加热,边加热边滴加8~25%的硫酸溶液,呈糊状后停止加热;
(3)第二次改性:将双氧水、无水乙醇和甲醛加入经第一次改性后的吸附剂基体中,混合均匀后,26~32℃反应1~3.5小时,坩埚继续加热,至水分完全挥发停止加热;
(4)交联反应:向第二次改性后的吸附剂基体中加入马来酸酐和戊二醛,4~8℃反应40~85分钟;
(5)成品:经交联反应后的产物置于烘箱中,90~105℃反应1~3.5小时即可制得。
4.根据权利要求3所述的一种木质素磺酸钠氧化改性的水体重金属吸附剂的制备方法,其特征在于,步骤(1)吸附剂基体制备:将硫酸亚铁、尿素、氯化锌和氯化铜混合后,粉碎研磨,至粒径为110目,置于烘箱中100℃处理86分钟。
5.根据权利要求3所述的一种木质素磺酸钠氧化改性的水体重金属吸附剂的制备方法,其特征在于,步骤(2)第一次改性:将木质素磺酸钠加入吸附剂基体中,置于坩埚中加热,边加热边滴加20%的硫酸溶液,呈糊状后停止加热。
6.根据权利要求3所述的一种木质素磺酸钠氧化改性的水体重金属吸附剂的制备方法,其特征在于,步骤(3)第二次改性:将双氧水、无水乙醇和甲醛加入经第一次改性后的吸附剂基体中,混合均匀后,30℃反应3小时,坩埚继续加热,至水分完全挥发停止加热。
7.根据权利要求3所述的一种木质素磺酸钠氧化改性的水体重金属吸附剂的制备方法,其特征在于,步骤(4)交联反应:向第二次改性后的吸附剂基体中加入马来酸酐和戊二醛,7℃反应65分钟。
8.根据权利要求3所述的一种木质素磺酸钠氧化改性的水体重金属吸附剂的制备方法,其特征在于,步骤(5)成品:经交联反应后的产物置于烘箱中,98℃反应3小时即可制得。
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