CN108911726B - 一种煤矸石-脱硫石膏-碳酸钙体系透水陶瓷砖及其制备方法 - Google Patents
一种煤矸石-脱硫石膏-碳酸钙体系透水陶瓷砖及其制备方法 Download PDFInfo
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Abstract
本发明公开了一种煤矸石‑脱硫石膏‑碳酸钙体系透水陶瓷砖及其制备方法，该透水砖是以煤矸石和脱硫石膏两种废渣为主要原料，外加少量碳酸钙助烧剂，经历高温烧结而获得的。其中，尾矿在高温条件下释放的气体赋予其优良的多孔结构。其主要物相是钙长石相，强度高、透水性好、抗腐蚀和不产生二次污染，显气孔率15.21～22.51％，抗压强度21.56～54.97MPa，抗弯强度8.45～18.50MPa，耐酸性99.60～99.80％，耐碱性99.63～99.80％，透水系数4.12‑9.33×10‑ 2cm/s，此材料的制备工艺简单高效且成本低廉，并具有废渣利用率高等特点，可用作海绵城市建设用路面透水砖材料。
Description
技术领域
本发明属于固体废弃物资的循环利用及新型建筑用陶瓷材料领域，具体涉及的是一种煤矸石-脱硫石膏-碳酸钙体系透水陶瓷砖及其制备方法。
背景技术
煤矸石是一种在煤形成过程中共生的坚硬岩石，在开采和洗选加工过程中容易被分离出来，属于固体废弃物。随着工业化的迅速发展，对煤炭的需求量日益增多，促使煤炭的开采量逐年递增，随之产生的煤矸石排放量和积存量将十分惊人。据统计，国内煤矸石的平均年产量约为2亿吨，积存量高达38亿吨。更值得注意的是，这种废弃物引起的环境污染和土地占用问题，不仅给企业的发展带来困难，也大大降低了周边居民的生活质量。因此，如何有效地降低煤矸石的存量并获得有效的回收再利用成为政府和企业当前亟待解决的问题。煤矸石的化学组成包含SiO2、Al2O3、Fe2O3、CaO、MgO、TiO2、K2O等，其中SiO2和Al2O3占据煤矸石中的主要组分，是制备陶瓷砖的必要成分。据报道，这种煤矸石可以应用在发电、制备建材、提炼元素、筑基修路和充填采空区等领域。然而这些应用对技术和设备的要求过高，前期以及后期的处理工艺过于复杂，成本也较高。因此，煤矸石的利用率仍然是比较低的。另一方面，脱硫石膏为火力发电厂湿式石灰石-石膏法脱硫工艺的主要副产品，其成分主要为二水硫酸钙(CaSO4·2H2O)，仅2010年我国脱硫石膏产量就已经高达2000万吨，如何有效地回收利用引起人们的广泛关注。
在相关透水陶瓷砖的开发研究中，公开号为CN105330331A的专利报道了一种节能型烧结透水砖材料，其组成配比和工艺如下：1)组成配比：污水厂污泥40～43％，稻壳6～7％，钾长石粉4～5％，粉煤灰10～12％，煤矸石14～16％，页岩18～20％，铝铬渣9～11％等。2)工艺：将各原料进行预处理、粉磨、造粒、压制成型并烧结制备而成。该专利以污泥、粉煤灰、页岩、煤矸石和铝铬渣等为原料，制备透水砖，其烧结温度在1150℃，透水系数为2.29×10-2cm/s，抗弯强度为55.2MPa，25次冻融循环抗压强度损失小于20％。但是煤矸石废渣的利用率较低(仅为14～16％)，原料成分复杂，加工难度大，成本相对高，且未涉及煤矸石-脱硫石膏-碳酸钙体系透水陶瓷砖及其制备方法。
公开号为CN106518005A的专利公开了一种利用废砖块制备的烧结透水砖材料，1)组成配比：废砖块50～60份，淀粉厂污泥粉15～20份，中药渣5～15份，粘土8～13％，蒙脱石粉5～10份，松香树脂1份等。2)工艺：将各原料进行预处理、制坯、干燥并烧结制备而成。该专利以废砖块、淀粉厂污泥、中药渣、粘土和蒙脱石粉等来制备透水砖，烧结温度在1050～1100℃，保温1～2h。该发明实现了废弃物的循环利用，透水系数达4×10-2cm/s以上，具有原料来源广泛和成本低等特点。显然，该专利原料成分较复杂，加工难度较大，成本相对较高，且未涉及煤矸石或脱硫石膏等废渣的利用，也未涉用煤矸石-脱硫石膏-碳酸钙体系透水陶瓷砖及其制备方法。
发明内容
本发明的目的是提供一种煤矸石-脱硫石膏-碳酸钙体系透水陶瓷砖材料及其制备方法。该材料表现出高的抗弯及抗压强度、高的透水性和抗腐蚀性，并不产生二次污染等特点，适用于路面铺设材料、非承重墙等建筑性应用。其制备方法具有煤矸石利用率高和烧结温度低等特点，因而可有效地降低固体废弃物对环境的危害，同时可降低透水砖的生产成本。
一种煤矸石-脱硫石膏-碳酸钙体系透水陶瓷砖，该透水陶瓷砖生坯的化学组成质量百分比为：SiO2：37.5～42.9％；Al2O3：17.5～20％；CaO：24.20～30.60％；MgO：0.93～1.04％；Na2O：2.87～3.30％；Fe2O3：4.05～4.63％，其余组成：5.50～12.95％，对应的透水陶瓷砖生坯原料的质量百分比组成：煤矸石70～80％，脱硫石膏10～25％，碳酸钙9～19％。本发明的技术优势如下：
1、煤矸石中含有大量的SiO2和Al2O3成分，而脱硫石膏和碳酸钙的主要成份分别为CaSO4和CaCO3，在高温下分解出大量的CaO。在烧结过程中，部分CaO与SiO2、Al2O3生成钙长石CaAl2Si2O8相，构成陶瓷砖的主体结构，赋予透水陶瓷优良的机械性能和化学稳定性；废渣中含有多种碱金属和碱土金属氧化物，在高温下与SiO2和Al2O3形成硅酸盐、铝酸盐熔体，可加快质点的扩散迁移，从而大大降低陶瓷的烧结温度；在陶瓷烧成后的冷却过程中，液相将陶瓷中的钙长石晶粒牢固地粘结在一起，形成透水陶瓷的致密骨架和气孔壁，赋予陶瓷砖的高强度和高化学稳定性。
2、煤矸石中含有一定量Fe2O3，在1100-1200℃高温下烧结，一部分Fe2O3颗粒被还原并释放出O2气体；一部分的Fe2O3颗粒则在高温下融于形成的玻璃相中，也释放出O2气体。同时，脱硫石膏和碳酸钙在高温下分别放出SO3和CO2气体，可促进透水陶瓷中连通气孔的形成，进而促进致密陶瓷骨架的形成，从而在确保透水陶瓷砖高强度的同时又赋予陶瓷的高透水系数。
3、废渣中含有多种碱金属和碱土金属氧化物，在烧结过程中具有助熔作用，因此，利用废渣中的Na2O、K2O等碱金属氧化物和CaO、MgO等碱土金属氧化物与SiO2、Al2O3化合物在陶瓷烧结过程中的反应，生成液相，从而降低陶瓷的烧结温度，促进烧结进程。
4、玻璃相也可与重金属离子等有毒有害组分固溶，形成化学键合，如Si-O-Pb2+、Al-O-Cd2+、Al-O-Cr3+等，从而使后者受到束缚与变性。或者通过玻璃熔体的物理包埋方式对重金属离子及放射性物质等有毒害组分进行固封，从而实现陶瓷类制品中由废渣引入的有毒害物的零排放。
5、当不同目数的原料混合时，加入少量PVA，在一定机械压力作用下成型后，颗粒间产生一定粘结力，从而赋予陶瓷坯体一定的机械强度。
本发明提供的方案中将煤矸石加工成20～30/30～40/40～60/60～80/80～200目，各目数所占比例为1:2:5:5:2，脱硫石膏经球磨机加工成细小颗粒，通过过筛获取粒度为100～200目的粉末，将所得的各种目数的颗粒按照预先设计的配比进行混合、干燥后获得配合料，然后外加少量的PVA使其易于压制成型，混合均匀后装入模具，在一定压力下压制成型，得到坯体；所得的透水陶瓷坯体先置于干燥箱中进行干燥，再进行高温烧结并保温一定时间，烧结温度为1100～1200℃，保温0.5～1h，冷却，即得透水陶瓷。
本发明所述的煤矸石-脱硫石膏-碳酸钙体系透水陶瓷砖及其制备方法还包括以下优选方案：
优选的方案中将充分干燥的陶瓷坯体置于燃气窑炉或电阻炉中，以5℃/min的升温速率。
优选的方案中总质量3～5％的PVA的加入起到润湿和粘结性能，有利于原料的压制成型，赋予陶瓷坯体初始机械强度。
优选的方案中压制成型采用单面加压方式成型，成形圧力为20～25MPa。
优选的方案中冷却方式为随炉冷却。
本发明的技术优势：根据材料的化学组成，利用煤矸石、脱硫石膏中不同组成和粒度的颗粒相互搭配对材料制备工艺及性能潜在的作用，粗颗粒构建透水陶瓷的骨架，细颗粒填充到部分空隙中，颗粒表面在烧结过程中产生化学键合，形成透水性高、强度高的陶瓷。进而最大限度地利用固体废渣，开发出优良综合性能的透水陶瓷制品，且不再产生二次污染。
综上所述本发明的技术优势，带来了非常优异的技术效果：
1、最大限度地利用了煤矸石和脱硫石膏2种废渣，废渣最高引入量达91％(质量百分数)。充分利用了废渣和添加物中不同组成和粒径间的科学搭配，实现了透水陶瓷的可控制备，成功制备出综合性能优异的透水陶瓷。
2、制备的透水陶瓷砖以钙长石为主晶相，具有高强、高透水性、抗腐蚀和不产生二次污染等特点；具体体现在透水陶瓷的显气孔率15.21～22.51％，抗压强度21.56～54.97MPa，抗弯强度8.45～18.50MPa，耐酸性99.60～99.80％，耐碱性99.63～99.80％，透水系数4.12～9.33×10-2cm/s，可用作海绵城市建设用路面透水砖材料。
附图说明
图1为本发明实施例2制备的透水陶瓷砖的XRD图；
图2为本发明实施例3制备的透水陶瓷的实物图。
具体实施方式
下面结合实例对本发明内容作进一步说明，但不应以此限制本发明的保护范围。
实施例1
将设计化学组成SiO2：38.56％，Al2O3：18.00％，CaO：27.99％，MgO：0.85，Na2O：2.95％，Fe2O3：4.17％，其余组成：7.53％，换算成废渣及添加料用量，将各种原料按煤矸石72％，脱硫石膏10％，碳酸钙18％的质量百分比称量并混合均匀后，加入少量PVA或者以原料总质量3～5％的水作为粘结剂，混合均匀后放入金属模具中在25MPa下压制成透水陶瓷坯体，放入干燥箱中进行干燥；将充分干燥后的坯体置于箱式电阻炉中以5℃/min匀速升温到1140℃，保温0.5h后随炉冷却。制得的透水陶瓷的显气孔率为17.3％，透水系数为9.33×10-2cm/s，抗压强度为20.56MPa，抗弯强度为8.45MPa，耐酸性为99.72％，耐碱性为99.76％。
实施例2
将设计化学组成SiO2：38.56％，Al2O3：18％，CaO：23.37％，MgO：0.94，Na2O：2.95％，Fe2O3：4.17％，其余组成：12.04％，将各种原料按煤矸石72％，脱硫石膏18％，碳酸钙10％的质量百分比称量并混合均匀后，加入少量PVA或者以原料总质量3～5％的水作为粘结剂，混合均匀后放入金属模具中在25MPa下压制成透水陶瓷坯体，放入干燥箱中进行干燥；将充分干燥后的坯体置于箱式电阻炉中以5℃/min匀速升温到1145℃，保温0.5h后随炉冷却。制得的透水陶瓷的显气孔率为14.06％，透水系数为4.75×10-2cm/s，抗压强度为43.58MPa，抗弯强度为13.33MPa，耐酸性为99.80％，耐碱性为99.79％。图1为制备的透水陶瓷砖的XRD图。
实施例3
将设计化学组成SiO2：38.56％，Al2O3：18％，CaO：23.37％，MgO：0.94，Na2O：2.95％，Fe2O3：4.17％，其余组成：12.04％，将各种原料按煤矸石72％，脱硫石膏18％，碳酸钙10％的质量百分比称量并混合均匀后，加入少量PVA或者以原料总质量3-5％的水作为粘结剂，混合均匀后放入金属模具中在25MPa下压制成透水陶瓷坯体，放入干燥箱中进行干燥；将充分干燥后的坯体置于箱式电阻炉中以5℃/min匀速升温到1140℃，保温1h后随炉冷却。制得的透水陶瓷的显气孔率为22.51％，透水系数为4.83×10-2cm/s，抗压强度为54.97MPa，抗弯强度为11.56MPa，耐酸性为99.60％，耐碱性为99.63％。图2为制备的透水陶瓷的实物图。
实施例4
将设计化学组成SiO2：36.59％，Al2O3：17.00％，CaO：22.64％，MgO：0.75％，Na2O：2.01％，Fe2O3：4.17％，其余组成：16.84％，将各种原料按煤矸石68％，脱硫石膏23％，碳酸钙9％的质量百分比称量并混合均匀后，加入少量PVA或者以原料总质量3～5％的水作为粘结剂，混合均匀后放入金属模具中在25MPa下压制成透水陶瓷坯体，放入干燥箱中进行干燥；将充分干燥后的坯体置于箱式电阻炉中以5℃/min匀速升温到1145℃，保温0.5h后随炉冷却。制得的透水陶瓷的显气孔率为15.21％，透水系数为4.12×10-2cm/s，抗压强度为43.58MPa，抗弯强度为18.5MPa，耐酸性为99.76％，耐碱性为99.80％。
表1实施例1～4制备的透水陶瓷的性能指标
所有实施例中样品的抗压强度是根据GB/T 1964-1996《多孔陶瓷压缩强度测试方法》测得的。
所有实施例中样品的抗弯曲强度是根据GB/T 1965-1996《多孔陶瓷弯曲强度测试方法》测得的。
Claims (4)
1.一种煤矸石-脱硫石膏-碳酸钙体系透水陶瓷砖，其特征在于，以煤矸石和脱硫石膏两种废渣为主要原料，外加少量碳酸钙助烧剂，脱硫石膏和碳酸钙同时兼作发泡剂，透水陶瓷砖生坯的化学组成质量百分比为：SiO2：37.5～42.9%；Al2O3：17.5～20%；CaO：24.20～30.60%；MgO：0.93～1.04%；Na2O：2.87～3.30%；Fe2O3：4.05～4.63%，TiO2，SO3和K2O及少量其他杂质：5.50～8.95%，对应的透水陶瓷砖生坯原料的质量百分比组成：煤矸石70-80%，脱硫石膏10~25%，碳酸钙9~19%，其中，废渣总引入量达到81~91%。
2.权利要求1所述的煤矸石-脱硫石膏-碳酸钙体系的透水陶瓷砖的制备方法，包括以下工艺步骤：
1）将煤矸石和脱硫石膏原料经球磨机加工成不同目数的颗粒,其中，煤矸石：20~30/30~40/40~60/60~80/80~200目，各目数所占比例为1:2:5:5:2，脱硫石膏：100~200目；
2）将步骤1）所得的不同粒径的原料按预先设计的配比进行混合，经干燥后获得配合料，然后添加原料总质量3~5%的PVA作为粘结剂，混合均匀后装入模具，压制成型，得到坯体；
3）将步骤2）所制得的陶瓷坯体先置于空气或干燥箱中干燥，再置于燃气窑炉或电阻炉中烧结并保温，烧结温度为1100~1200°C，保温时间为0.5~1h，随炉冷却，即得透水陶瓷砖。
3.根据权利要求2所述的煤矸石-脱硫石膏-碳酸钙系透水陶瓷砖的制备方法，其特征在于，陶瓷砖的压制成型压力为20-25MPa。
4.根据权利要求2所述的煤矸石-脱硫石膏-碳酸钙体系透水陶瓷砖的制备方法，其特征在于，经充分干燥的陶瓷坯体被送入燃气窑炉或电阻炉中进行烧结，其升温速率为5°C/min。
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| CN104496535A (zh) * | 2015-01-04 | 2015-04-08 | 中南大学 | 以硅砂尾矿和粉煤灰为主要原料的泡沫陶瓷及其制备方法 |
| CN106904938A (zh) * | 2017-01-16 | 2017-06-30 | 武汉新陶环保科技有限公司 | 一种以煤矸石为原料和燃料的高强陶粒及其制备方法 |
| CN108083767A (zh) * | 2017-12-22 | 2018-05-29 | 广东科达洁能股份有限公司 | 一种透水砖的制备方法 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102731138A (zh) * | 2012-07-17 | 2012-10-17 | 湖南亿泰环保科技股份有限公司 | 一种粉煤灰基高强度高气孔率泡沫陶瓷及制备方法 |
| CN104496535A (zh) * | 2015-01-04 | 2015-04-08 | 中南大学 | 以硅砂尾矿和粉煤灰为主要原料的泡沫陶瓷及其制备方法 |
| CN106904938A (zh) * | 2017-01-16 | 2017-06-30 | 武汉新陶环保科技有限公司 | 一种以煤矸石为原料和燃料的高强陶粒及其制备方法 |
| CN108083767A (zh) * | 2017-12-22 | 2018-05-29 | 广东科达洁能股份有限公司 | 一种透水砖的制备方法 |
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