CN112811914A - 一种利用铬泥和镁法脱硫渣制备纳米铬镁尖晶石的方法 - Google Patents

一种利用铬泥和镁法脱硫渣制备纳米铬镁尖晶石的方法 Download PDF

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CN112811914A
CN112811914A CN202110248739.4A CN202110248739A CN112811914A CN 112811914 A CN112811914 A CN 112811914A CN 202110248739 A CN202110248739 A CN 202110248739A CN 112811914 A CN112811914 A CN 112811914A
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方得安
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Abstract

本发明属于固体废弃物资源化利用技术领域，具体涉及一种利用铬泥和镁法脱硫渣制备纳米铬镁尖晶石的方法。本发明利用镁法烟气脱硫渣及化学沉淀法产生的铬泥为原料，在酸性条件下将二者溶解，溶液过滤后调节pH至中性，生成铬镁共沉淀；将沉淀物脱水干燥后，将其于马弗炉中焙烧；将焙烧后的样品经过稀盐酸洗涤，过滤干燥得到粒径为80‑500的纳米级铬镁尖晶石粉体。本发明将铬泥及烟气脱硫废弃物做为制备铬镁尖晶石的原料，对废弃物无害化处理的同时，实现废弃物的资源化利用，从而产生明显的经济效益、社会效益及环境效益。

Description

一种利用铬泥和镁法脱硫渣制备纳米铬镁尖晶石的方法
技术领域
本发明属于固体废弃物资源化利用技术领域，具体涉及一种利用铬泥和镁法脱硫渣制备纳米铬镁尖晶石的方法。
背景技术
铬镁尖晶石MgCr2O4是MgO-Cr2O3系统唯一的化合物，属典型的尖晶石结构，立方晶系，熔点约2350℃，莫氏硬度5.5，线膨胀系数(25-900℃)为5.7-8.55×10-6，具有耐高温，抗腐蚀等优良性能，是优质耐火材料。广泛应用于各种热工窑炉及作为湿敏元件和电子陶瓷。目前主要采用烧结反应法，电熔反应法及共沉淀法合成。
本发明采用铬泥及烟气脱硫废弃物为原料，合成纳米级铬镁尖晶石粉体，流程简单，成本低廉，实现废弃物的资源化利用。
发明内容
本发明提供一种利用铬泥和镁法脱硫渣制备纳米铬镁尖晶石的方法，该方法采用铬泥及烟气脱硫废弃物为原料，对废弃物无害化处理的同时，实现废弃物的资源化利用。从而产生明显的经济效益、社会效益及环境效益。
实现本发明目的的技术方案按照以下步骤进行：
一种利用铬泥和镁法脱硫渣制备纳米铬镁尖晶石的方法，其特征在于按照以下步骤进行：
（1）利用镁法脱硫渣作为镁源，含铬废水处理过程中产生的含铬绿泥作为铬源，按一定比例加入到自来水中，以无机酸调节溶液pH=2.0-4.5持续搅拌溶解10-50 min后，将溶液过滤后用碱性物质调节至pH=7.0-8.5，搅拌20-50 min，静置沉淀；
（2）将沉淀物抽滤脱水后，于100℃干燥脱水，干燥后的样品研磨成粉末，在马弗炉中于600~1200 ℃下焙烧1.0-3.0 h；
（3）将焙烧后的样品经过0.5mol/L的稀盐酸洗涤30 min，过滤干燥得到平均粒径为800-200 nm的铬镁尖晶石粉体。
所述的镁法脱硫渣来自于湿式氧化镁烟气脱硫工艺产生的废弃物，铬泥来自于以亚硫酸盐、焦亚硫酸盐、硫代硫酸盐、SO2、水合肼及甲醛等为还原剂的化学沉淀法所产生的绿色铬泥，其主要成分为Cr3+氢氧化物。
所述的镁法脱硫渣及铬泥加入量分别按照废弃物中所含的镁及铬元素的摩尔比Mg:Cr=1.0~1.2:2.0投加，二者总质量不超过溶液质量的20%。
所述的调pH的酸是硫酸、盐酸、硝酸中的一种或几种，溶解pH=2.0-4.5；溶液过滤后以氢氧化钠、碳酸钠或氨水中的一种或几种调节pH=7.0-8.5。
所述的沉淀物的焙烧温度为600~1200 ℃，焙烧时间1.0-3.0 h。
与现有技术相比，本发明的特点和有益效果是：
本发明既解决了化学沉淀法产生的重金属沉淀物铬泥及湿式氧化镁烟气脱硫废弃物占地及二次污染等问题，也降低了铬镁尖晶石材料的原料成本，实现了废弃物的资源化利用。
附图说明
图1为本发明实施例中所制备的铬镁尖晶石SEM图谱。
具体实施方式
下面通过实例对本发明所述的方法和技术加以说明，实际应用中，不限于此。
本发明实施例中所制备的铬镁尖晶石其主要元素成分表如表1所示：
表1 铬镁尖晶石粉体化学成分（质量分数）
Cr<sub>2</sub>O<sub>3</sub> MgO SiO<sub>2</sub> TFe CaO
78.43 19.78 2.15 0.88 0.12
实施例1
本实施例的一种利用铬泥和镁法脱硫渣制备纳米铬镁尖晶石的方法，按照以下步骤进行：
（1）取镁法脱硫渣和铬泥共20g加入到200ml自来水中，其中镁及铬元素摩尔比为Mg:Cr=1.1:1.0，以硫酸调节溶液pH=2.5并持续搅拌溶解30 min，将溶液过滤后用氨水调节至pH=8.0，缓慢搅拌30 min，静置沉淀；
（2）将沉淀物抽滤脱水后，于100℃干燥脱水，干燥后的样品研磨成粉末，在马弗炉中于900℃下焙烧1.5 h；
（3）将焙烧后的样品经过0.5mol/L的稀盐酸洗涤30 min，过滤干燥得到平均粒径为200 nm的铬镁尖晶石粉体。
实施例2
本实施例的一种利用铬泥和镁法脱硫渣制备纳米铬镁尖晶石的方法，按照以下步骤进行：
（1）取镁法脱硫渣和铬泥共15g加入到200ml自来水中，其中镁及铬元素摩尔比为Mg:Cr=1.0:1.0，以硫酸调节溶液pH=2.0并持续搅拌溶解20 min，将溶液过滤后用碳酸钠调节至pH=8.0，缓慢搅拌30 min，静置沉淀；
（2）将沉淀物抽滤脱水后，于100℃干燥脱水，干燥后的样品研磨成粉末，在马弗炉中于1000℃下焙烧1.5 h；
（3）将焙烧后的样品经过0.5mol/L的稀盐酸洗涤30 min，过滤干燥得到平均粒径为300 nm的铬镁尖晶石粉体。
以上所述，仅为本发明较佳的具体实施案例，但本发明的保护范围并不局限于此，
任何熟悉本技术领域的技术人员在本发明披露的技术范围内，根据本发明的技术方案及其
发明构思加以等同替换或改变，都应涵盖在本发明的保护范围之内。

Claims (5)

1.一种利用铬泥和镁法脱硫渣制备纳米铬镁尖晶石的方法，其特征在于按照以下步骤进行：
（1）利用镁法脱硫渣作为镁源，含铬废水处理过程中产生的含铬绿泥作为铬源，按一定比例加入到自来水中，以无机酸调节溶液pH=2.0-4.5持续搅拌溶解10-50 min后，将溶液过滤后用碱性物质调节至pH=7.0-8.5，搅拌20-50 min，静置沉淀；
（2）将沉淀物抽滤脱水后，于100℃干燥脱水，干燥后的样品研磨成粉末，在马弗炉中于600~1200 ℃下焙烧1.0-3.0 h；
（3）将焙烧后的样品经过0.5mol/L的稀盐酸洗涤30 min，过滤干燥得到平均粒径为80-500 nm的铬镁尖晶石粉体。
2.根据权利要求1所述一种利用铬泥和镁法脱硫渣制备纳米铬镁尖晶石的方法，其特征在于所述的镁法脱硫渣来自于湿式氧化镁烟气脱硫工艺产生的废弃物，铬泥来自于以亚硫酸盐、焦亚硫酸盐、硫代硫酸盐、SO2、水合肼及甲醛等为还原剂的化学沉淀法所产生的绿色铬泥，其主要成分为Cr3+氢氧化物。
3.根据权利要求1所述一种利用铬泥和镁法脱硫渣制备纳米铬镁尖晶石的方法，其特征在于所述的镁法脱硫渣及铬泥加入量分别按照废弃物中所含的镁及铬元素的摩尔比Mg:Cr=1.0~1.2:2.0投加，二者总质量不超过溶液质量的30%。
4.根据权利要求1所述一种利用铬泥和镁法脱硫渣制备纳米铬镁尖晶石的方法，其特征在于所述的调pH的酸是硫酸、盐酸、硝酸中的一种或几种，溶解pH=2.0-4.5；溶液过滤后以氢氧化钠、碳酸钠或氨水中的一种或几种调节pH=7.0-8.5。
5.根据权利要求1所述一种利用铬泥和镁法脱硫渣制备纳米铬镁尖晶石的方法，其特征在于所述的沉淀物的焙烧温度为600~1200 ℃，焙烧时间1.0-3.0 h。
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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB1481583A (en) * 1974-06-03 1977-08-03 Gen Refractories Co Methods of making magnesium oxidechrome ore refractory shapes
CN105923836A (zh) * 2016-06-20 2016-09-07 东北大学 一种镁法脱硫废弃物治理钒工业废水的方法
CN108588427A (zh) * 2018-05-17 2018-09-28 东北大学 一种提钒废水水处理沉淀的铬泥的资源化利用方法
CN112340757A (zh) * 2020-09-11 2021-02-09 华南理工大学 一种资源化处理电镀污泥制备高值尖晶石材料的方法

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB1481583A (en) * 1974-06-03 1977-08-03 Gen Refractories Co Methods of making magnesium oxidechrome ore refractory shapes
CN105923836A (zh) * 2016-06-20 2016-09-07 东北大学 一种镁法脱硫废弃物治理钒工业废水的方法
CN108588427A (zh) * 2018-05-17 2018-09-28 东北大学 一种提钒废水水处理沉淀的铬泥的资源化利用方法
CN112340757A (zh) * 2020-09-11 2021-02-09 华南理工大学 一种资源化处理电镀污泥制备高值尖晶石材料的方法

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
DEAN FANG, ET AL.: "A novel method to remove chromium, vanadium and ammoniumfrom vanadium industrial wastewater using a byproduct of magnesium-based wet flue gas desulfurization", 《JOURNAL OF HAZARDOUS MATERIALS》 *

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Application publication date: 20210518