CN109331773B - 一种污水除磷剂及其制备方法 - Google Patents

一种污水除磷剂及其制备方法 Download PDF

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CN109331773B
CN109331773B CN201811218240.3A CN201811218240A CN109331773B CN 109331773 B CN109331773 B CN 109331773B CN 201811218240 A CN201811218240 A CN 201811218240A CN 109331773 B CN109331773 B CN 109331773B
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CN109331773A (zh
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付登强
杨伟波
刘小玉
余凤玉
孙彦涛
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Coconut Research Institute of Chinese Academy of Tropical Agricultural Sciences
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/0203Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
    • B01J20/0225Compounds of Fe, Ru, Os, Co, Rh, Ir, Ni, Pd, Pt
    • B01J20/0229Compounds of Fe
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/0203Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
    • B01J20/0274Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04 characterised by the type of anion
    • B01J20/0281Sulfates of compounds other than those provided for in B01J20/045
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/10Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
    • B01J20/103Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate comprising silica
    • B01J20/106Perlite
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/28Treatment of water, waste water, or sewage by sorption
    • C02F1/281Treatment of water, waste water, or sewage by sorption using inorganic sorbents
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00Nature of the contaminant
    • C02F2101/10Inorganic compounds
    • C02F2101/105Phosphorus compounds

Abstract

本发明涉及一种污水除磷剂及其制备方法,该方法以膨胀珍珠岩颗粒生产过程中的副产物——膨胀珍珠岩微粉为载体,利用其疏松多孔、比表面积大,化学性质稳定的特点,采用硫酸亚铁进行表面热改性,制备了一种低成本、高效率的污水除磷剂。本发明的污水除磷剂对pH为3~6的污水具有较高的除磷能力,除磷速度快,充分接触条件下10min即可完成吸附,吸附后污水不发黄。当模拟污水磷浓度为50mg.L‑1时,添加本发明的污水除磷剂25g.L‑1的磷去除率达99.3%,污水残磷浓度为0.35mg.L‑1,含磷量符合国家城镇污水处理厂污染物排放标准(GB 18918)的一级A类排放标准(≤0.5mg.L‑1)。本发明的污水除磷剂在酸性、高磷污水的快速除磷处理中具有一定的应用潜力。

Description

一种污水除磷剂及其制备方法
技术领域
本发明属于环境吸附材料技术领域,具体为一种污水除磷剂及其制备方法。
背景技术
吸附法是污水除磷的有效方法,目前常用的吸附剂主要包括土壤、炉渣、沸石、活性炭、膨润土、蛭石、凹凸棒石等,这些材料很难兼顾成本和除磷效率。珍珠岩微粉是生产膨胀珍珠岩颗粒的副产物,价格低廉,其比表面积大,但主要化学成分为二氧化硅,缺少离子吸附位点。铁、铝试剂是常用的污水除磷剂,铁试剂有三价铁和二价铁,三价的聚合硫酸铁成本较高,二价铁试剂价格较低,但需要氧化成三价铁才能更好的发挥除磷作用。
发明内容
解决的技术问题:珍珠岩微粉具备多孔结构,但化学成分主要为二氧化硅,对磷的吸附能力弱;聚合硫酸铁成本高,且过量的铁离子会导致水的颜色发黄、腐蚀管路和设备;硫酸亚铁成本低,但需要将二价铁离子转化为三价铁离子才能发挥除磷作用。本发明将硫酸亚铁附着在珍珠岩微粉的表面上,通过高温将其亚铁离子转化为铁离子并固定,是一种变废为宝、成本低廉的新型除磷剂制备技术。
技术方案:
一种污水除磷剂及其制备方法,包括以下步骤:
(1)制备饱和硫酸亚铁溶液;
(2)搅拌吸附:在1L所述饱和硫酸亚铁溶液中加入125~167g珍珠岩微粉进行搅拌,搅拌5~10分钟,静置后去掉浮粉,得到固液混合物;
(3)固液分离:将所述固液混合物进行固液分离,分离得到沉淀物;
(4)高温改性:将所述沉淀物在300~400℃下,加热1~2h,冷却后即得到所述污水除磷剂。
优选地,所述饱和硫酸亚铁溶液的具体制备步骤为:在25~30℃的1L水中加入550~570g七水合硫酸亚铁,即制得所述饱和硫酸亚铁溶液。
优选地,所述步骤(3)中,将所述混合液用200目滤网进行真空抽滤。
有益效果:硫酸亚铁热改性珍珠岩微粉除磷剂对pH为3~6的污水具有较高的除磷能力,除磷速度快,充分接触条件下10min即可完成吸附,吸附后污水不发黄。当模拟污水磷浓度为50mg.L-1时,添加25g.L-1改性微粉的磷去除率达99.3%,污水残磷浓度为0.35mg.L-1,含磷量符合国家城镇污水处理厂污染物排放标准(GB 18918)的一级A类排放标准(≤0.5mg.L-1)。本发明的污水除磷剂在酸性、高磷废水的快速除磷处理中具有一定的应用潜力。
附图说明
图1为本发明的工艺流程图;
图2为珍珠岩微粉与本发明除磷剂的磷吸附等温线;
图3为pH值对本发明除磷剂磷去除效果的影响。
具体实施方式
以下结合实例对本发明作进一步的描述:
实施例1:在1L 25℃的水中加入七水合硫酸亚铁550g,搅拌溶解后得到饱和硫酸亚铁溶液,取饱和硫酸亚铁溶液1L,加入珍珠岩微粉167g,搅拌10分钟,静置10分钟,去掉浮粉后用真空抽滤机(200目滤网)抽滤,抽滤后的滤液回收用于配置饱和硫酸亚铁溶液,抽滤后的沉淀物放入马弗炉300℃条件下处理2小时,冷却后得到162g改性珍珠岩微粉,即污水除磷剂。用珍珠岩微粉做对照,测试本实施例除磷剂的磷吸附等温线,结果如图2所示。本实施例的除磷剂的磷吸附能力显著提高,在80mg/L的磷溶液中加入25g/L本实施例的除磷剂,磷的去除率为97.86%。不同pH条件对除磷效果的影响如图3所示,在pH为3~6范围内,磷的去除率均超过90%,pH为5时去除率最高。
实施例2:在1L 30℃的水中加入七水合硫酸亚铁570g,搅拌溶解后得到饱和硫酸亚铁溶液,取饱和硫酸亚铁溶液1L,加入珍珠岩微粉125g,搅拌5分钟,静置10分钟,去掉浮粉后用真空抽滤机(200目滤网)抽滤,抽滤后的滤液回收用于配置饱和硫酸亚铁溶液,抽滤后的沉淀物放入马弗炉400℃条件下处理1小时,冷却后得到123g改性珍珠岩微粉,即污水除磷剂。当模拟污水磷浓度为50mg.L-1时,添加本发明除磷剂25g.L-1的磷去除率达99.3%,污水残磷浓度为0.35mg.L-1,含磷量符合国家城镇污水处理厂污染物排放标准(GB 18918)的一级A类排放标准(≤0.5mg.L-1)。
实施例3:在1L 28℃的水中加入七水合硫酸亚铁560g,搅拌溶解后得到饱和硫酸亚铁溶液,取饱和硫酸亚铁溶液1L,加入珍珠岩微粉140g,搅拌8分钟,静置10分钟,去掉浮粉后用真空抽滤机(200目滤网)抽滤,抽滤后的滤液回收用于配置饱和硫酸亚铁溶液,抽滤后的沉淀物放入马弗炉350℃条件下处理1.5小时,冷却后得到136g改性珍珠岩微粉,即污水除磷剂。在含磷量为100mg.L‐1的模拟污水中添加25g.L‐1本发明除磷剂,搅拌10min后,磷去除率可达98%以上。

Claims (3)

1.一种污水除磷剂的 制备方法,其特征在于,包括以下步骤:
(1)制备饱和硫酸亚铁溶液;
(2)搅拌吸附:在1L所述饱和硫酸亚铁溶液中加入125~167g珍珠岩微粉进行搅拌,搅拌5~10分钟,静置后去掉浮粉,得到固液混合物;
(3)固液分离:将所述固液混合物进行固液分离,分离得到沉淀物;
(4)高温改性:将所述沉淀物在300~400℃下,加热1~2h,冷却后即得到所述污水除磷剂。
2.如权利要求1所述的一种污水除磷剂的 制备方法,其特征在于,所述饱和硫酸亚铁溶液的具体制备步骤为:在25~30℃的1L水中加入550~570g七水合硫酸亚铁,即制得所述饱和硫酸亚铁溶液。
3.如权利要求1所述的一种污水除磷剂的 制备方法,其特征在于,所述步骤(3)中,将所述固液混合物用200目滤网进行真空抽滤。
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