CN112266235A - 一种钙镁质磷矿尾矿复合镁质原料制备白云石砖的方法 - Google Patents

一种钙镁质磷矿尾矿复合镁质原料制备白云石砖的方法 Download PDF

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CN112266235A
CN112266235A CN202011196086.1A CN202011196086A CN112266235A CN 112266235 A CN112266235 A CN 112266235A CN 202011196086 A CN202011196086 A CN 202011196086A CN 112266235 A CN112266235 A CN 112266235A
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magnesium
calcium
dolomite
phosphate ore
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张晋
贺爱平
秦元奎
郭茂生
李国栋
胡修权
尤大海
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Hubei Metallurgy Geology Research Institute (central South Institute Of Metallurgical Geology)
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Abstract

本发明提供一种钙镁质磷矿尾矿复合镁质原料（包括蛇纹石、镁橄榄石等）制备白云石砖的方法。（1）将处理后的钙镁质磷矿尾矿与镁质矿石按比例混合后加入酚醛树脂，经混炼、压坯煅烧得到白云石熟料；（2）白云石熟料经破碎成不同粒径配料后，再按粒径级别顺序经混合，边搅拌，边添加酚醛树脂，经混炼、压坯煅烧得到白云石砖。最终得到符合一定技术标准的白云石砖耐火材料制品，将磷尾矿这一大宗工业固废转变为特色资源加以综合利用，为磷化工产业的绿色发生和可持续发展注入新的动力。

Description

一种钙镁质磷矿尾矿复合镁质原料制备白云石砖的方法
技术领域
本发明涉及一种钙镁质磷矿尾矿复合镁质原料制备白云石砖的方法，尤其是经过浮选之后直接与镁质原料复合后经过一定的工艺处理后制得稳定性能较好的白云石砖，可作为耐火材料，为磷化工企业尾矿处理得到新的利润增长点。
背景技术：
磷矿尾矿是磷化工行业选矿提取精矿后产生的大宗矿业固体废弃物，目前我国约有2亿吨的磷尾矿堆积，其综合利用率不足10％，大部分堆存在尾矿库中。磷尾矿的堆存会带来一系列的环境问题、安全问题，也会给企业带来巨大的资金及用地压力，严重制约了企业的可持续发展。
白云石砖广泛应用于转炉炉衬耐火材料，具有良好的挂窑皮性能和使用寿命。目前国内对于白云石砖的研究很多，但是用钙镁质磷尾矿作为原料的很少。在已有的研究资料中，磷尾矿中加入了氧化锆、氧化钛等高价值、高质量的物料作为改性剂。磷尾矿与矿石原料复合制备白云石砖的研究还不曾见到。
本发明针对钙镁质磷尾矿的特点镁钙质耐火材料稳定性差的问题，对磷尾矿进行提纯以及复合，最终制得稳定性能较好的白云石砖。
发明内容
本发明的目的在于提供一种钙镁质磷矿尾矿复合镁质原料制备白云石砖的方法，可以有效降低利用磷尾矿制备耐火材料的成本，试现对磷尾矿的高附加值利用。本发明技术方案包括以下几个步骤：
(1)将镁钙质磷矿尾矿经过洗涤、分离、脱药、烘干经磷浮选得到钙镁质(主要是白云石)组分，其中18-21％，CaO品位28-32％，两者折合成白云石约为90-98％；P2O5品位小于2.0％(作为原料1)；
(2)将镁质矿石原料经过破碎、磨矿等步骤处理至粒度为50-80μm；(作为原料2)；
(3)将原料1、原料2以一定的比例混合，加入适量的酚醛树脂作为结合剂，充分混炼后用摩擦压砖机压坯。干燥后在1600-1700℃煅烧，制得稳定性白云石熟料。
(4)将步骤(3)获得的熟料再破、粉碎成颗粒料，一部分磨成细粉，按一定的级配进行配料。以酚醛树脂为结合剂，按照一定的加料顺序在湿碾机中混合均匀，用摩擦压砖机成型。砖坯经一定时间的湿养护后，干燥至水分小于0.5％，于1400-1500℃烧成后即为白云石砖。
步骤(1)中浮选磷过程中采用一粗一精一扫的闭路作业。其中，粗选药剂制度：碳酸钠7000-9000g/t，捕收剂TP 200-300g/t；磷扫选药剂制度：碳酸钠2000-3000g/t，捕收剂TP 100-150g/t；磷精选药剂制度：碳酸钠2000-3000g/t。
步骤(2)中镁质原料包括蛇纹石、镁橄榄石等含有镁质、硅质具有一定耐火性能的矿石原料。
步骤(3)原料1、原料2的质量比为1-4∶1，结合剂酚醛树脂的比例为原料总重的1％-4％，最终混合物料中P2O5不超过1.2％。
步骤(4)中白云石熟料经破碎成1mm以下、1-3mm、3-5mm三个不同粒级配料，三者最佳配比为1：0.6-1.5：0.4-1。
云石熟料不同粒级配料的加料顺序为3-5mm粒级配料→酚醛树脂→混练2-3min→1-3mm粒级配料→混练2-3min→1mm以下粒级配料→混练5-8min。
在本发明中，将钙镁质磷尾矿经过脱磷处理后，与镁质矿物原料进行复合，然后加以混练、成型、烧结得到白云石熟料，再将白云石熟料破粉碎后分成粗中细三个粒级，以一定的比例混合后再次成型、煅烧得到耐火性能和稳定性较好的白云石砖。相对于已有的研究，本发明避免使用纯度和质量很高的添加剂(如氧化锆、氧化钛等)，大大降低了磷尾矿制备耐火材料的成本，提高了技术的可行性。
附图说明
图1为本发明所用磷尾矿X射线衍射图。
图2为浮选后磷尾矿中胶磷矿(Col)与方解石(Cal)连生体矿物的共伴生关系。
图3为浮选后磷尾矿中方解石(Cal)与白云石(Dol)连生体矿物的共伴生关系。
图4为本发明的工艺路线图。
具体实施方式
下面列举几个实施实例对本发明作进行一步说明，但不是对本发明的限制。
实施例1：
将镁钙质磷矿尾矿经过洗涤、分离、脱药、脱泥等处理后烘干；然后通过一粗一精一扫的闭路试验流程脱除一定量的磷，剩下的组分中主要含有钙镁硅等。
浮选磷过程中采用一粗一精一扫的闭路作业药剂制度：粗选：碳酸钠8000g/t，捕收剂TP 200g/t；扫选：碳酸钠2400g/t，捕收剂TP 100g/t；精选：碳酸钠2000g/t。得到钙镁硅组分产率75％。
表1脱磷处理之后的钙镁硅质组分化学分析结果
Figure BDA0002754057300000031
将镁橄榄石经过破碎、磨矿等步骤处理至粒度为80μm。同时经浮选后的磷尾矿的附图见图2、图3。由图2、3可以看出，经浮选后，磷尾矿中含有胶磷矿与方解石连生体矿物，以及含有方解石与白云石的连生体矿物。浮选之后的磷尾矿中还含有少量的磷，可以起到稳定剂的作用，增加白云石砖的稳定性。
表2镁橄榄石化学分析结果
Figure BDA0002754057300000032
表3酚醛树脂性能指标
Figure BDA0002754057300000033
将处理后的磷尾矿和镁橄榄石按照质量比1∶1混合，然后加入总量2wt％的酚醛树脂做结合剂，充分混炼后用摩擦压砖机压坯，干燥后在1500℃煅烧3h，制成稳定的白云石熟料。熟料再破粉碎成颗粒料(1mm以下、1-3mm、3-5mm)，然后三者按照一定的质量比进行配料(具体配比及白云石砖性质见表4)。按照大颗粒→酚醛树脂→混练2min→中间颗粒→混练2min→细粉→混练5min顺序加料，酚醛树脂的加入量为2％，在湿碾机中混合均匀，用摩擦压砖机成型，湿养护8h后，干燥至水分小于0.5％，于1450℃烧成，达到具有一定耐火度和稳定性的白云石砖。
表4颗粒配比及白云石砖性质
Figure BDA0002754057300000034
通过控制三种颗粒的配比，可以调整优化白云石砖的耐火性质。由表4可知当三者比例在1∶2∶1.5时，白云石砖的体积密度最大，水化增重率最小，其他的耐火性质随着这两项指标优化。小颗粒粉料填充进了大、中颗粒的缝隙，减小了试块的显气孔率，体积密度随之增大；微观层面氧化镁粉体包裹在了氧化钙颗粒的周围，减小了氧化钙水化的概率进而优化了白云石砖的抗水化性。
实施例2：
将镁钙质磷矿尾矿(理化性质同例1)经过洗涤、分离、脱药、脱泥等处理后烘干；然后通过一粗一精一扫的闭路试验流程脱除一定量的磷，剩下的组分中主要含有钙镁硅等。
浮选磷过程中采用一粗一精一扫的闭路作业药剂制度：粗选：碳酸钠8000g/t，捕收剂TP 150g/t；扫选：碳酸钠2400g/t，捕收剂TP 80g/t；精选：碳酸钠2000g/t。得到钙镁硅组分产率80％，MgO品位19％，CaO品位32％。
表5脱磷处理之后的钙镁硅质组分化学分析结果
Figure BDA0002754057300000041
将蛇纹石经过破碎、磨矿等步骤处理至粒度为88μm。
表6蛇纹石X射线荧光光谱分析结果
Figure BDA0002754057300000042
将处理后的磷尾矿和蛇纹石按照2∶3混合，然后加入总量2％的酚醛树脂做结合剂，充分混炼后用摩擦压砖机压坯，干燥后在1600℃煅烧2h，制成稳定的白云石熟料。熟料再破粉碎成颗粒料(1mm以下、1-3mm、3-5mm)，然后三者按照1∶1∶0.5进行配料。按照大颗粒→酚醛树脂→混练2min→中间颗粒→混练2min→细粉→混练5min顺序加料，酚醛树脂的加入量为3％，在湿碾机中混合均匀，用摩擦压砖机成型，湿养护8h后，干燥至水分小于0.5％，于1500℃烧成，达到具有一定耐火度和稳定性的白云石砖。
经检测白云石砖性能为：白云石砂体积密度3.2g/cm3，显气孔率5.8％、常温抗压强度65MPa、高温抗折强度6.1MPa、水化试验增重率2.59％。
实施例3：
将镁钙质磷矿尾矿(理化性质同例1)经过洗涤、分离、脱药、脱泥等处理后烘干；然后通过一粗一精一扫的闭路试验流程脱除一定量的磷，剩下的组分中主要含有钙镁硅等。
将处理后的钙镁质磷矿尾矿以一定比例(配方及相关性质见表7)与镁质矿物原料(镁橄榄石)混合，其他实施步骤同实施例1。
表7物料配比比及白云石砖性质
Figure BDA0002754057300000043
Figure BDA0002754057300000051
通过控制两种原料的配比，可以调整优化白云石砖的耐火性质。钙镁质磷矿尾矿(物料1)占比较少，对其的综合利用效果不佳；占比较多时，白云石耐火砖的体积密度及抗水化性能大幅度降低。当钙镁质磷矿尾矿占比过多时，活化氧化钙的含量增高，未被包裹的概率增大，更易被水化，所以需控制物料1、物料2的比例在1-1.5∶1之间为宜。

Claims (9)

1.一种钙镁质磷矿复合镁质原料制备白云石砖的方法，其特征在于，主要包括以下几个步骤：
（1）将处理后的钙镁质磷矿与镁质矿石按比例混合后加入酚醛树脂，经混炼、压坯煅烧得到白云石熟料；
（2）白云石熟料经破碎成不同粒径配料后，再按粒径级别顺序经混合，边搅拌，边添加酚醛树脂，经混炼、压坯煅烧得到白云石砖。
2.根据权利要求1所述的钙镁质磷矿尾矿复合镁质原料制备白云石砖的方法，其特征在于，钙镁质磷矿尾矿中MgO品位为18-22%，CaO品位28-32%，P2O5品位小于2.0%。
3.根据权利要求1所述的钙镁质磷矿尾矿复合镁质原料制备白云石砖的方法，其特征在于，镁质原料包括蛇纹石、镁橄榄石；镁质矿石的粒度为50-80μm。
4.根据权利要求1所述的钙镁质磷矿尾矿复合镁质原料制备白云石砖的方法，其特征在于，步骤（1）中原料1、原料2的质量比为1-2∶1；酚醛树脂的比例为原料总重的1%-4%，最终混合物料中P2O5不超过1.2%。
5.根据权利要求1所述的钙镁质磷矿尾矿复合镁质原料制备白云石砖的方法，其特征在于，步骤（1）中压坯煅烧温度为1500-1700℃。
6.根据权利要求1所述的钙镁质磷矿尾矿复合镁质原料制备白云石砖的方法，其特征在于，步骤（2）中白云石熟料经破碎成1mm以下、1-3mm、3-5mm三个不同粒级配料，三者最佳配比为1：0.6-1.5：0.4-1。
7.根据权利要求6所述的钙镁质磷矿尾矿复合镁质原料制备白云石砖的方法，其特征在于，白云石熟料不同粒级配料的加料顺序为3-5mm粒级配料→酚醛树脂→混练2-3min→1-3mm粒级配料→混练2-3min→1mm以下粒级配料→混练5-8min。
8.根据权利要求7所述的钙镁质磷矿尾矿复合镁质原料制备白云石砖的方法，其特征在于，所述的酚醛树脂的添加量为2wt%-4wt%。
9.根据权利要求1所述的钙镁质磷矿尾矿复合镁质原料制备白云石砖的方法，其特征在于，步骤（2）中煅烧温度为1400-1500℃。
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