CN109231963B - 一种轻质高强度瓷砖及其制备方法 - Google Patents
一种轻质高强度瓷砖及其制备方法 Download PDFInfo
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Abstract
本发明属于建筑材料技术领域，公开了一种轻质高强度瓷砖，按重量份计，由以下原料组成：超轻粘土50‑80份、酸洗石英砂45‑85份、金属粉末12‑20份、白刚玉粉3‑5份、高温砂5‑7份、煅烧高岭土18‑30份、白云石6‑8份、电熔莫来石7‑11份、粉煤灰陶粒1‑3份、火山岩碎屑7‑13份、黑云母3‑6份、超细硅灰石粉12‑18份、粘性胶粉3‑5份、乙酰水杨酸1‑2份，先将超细硅灰石粉进行功能改性，同时将上述其他原料破碎熔合、球磨成粉，最后再次将所有物料混合，加水搅拌为均匀浆料，倒入模具经阶梯压制程序压制成型，制得高强度瓷砖，本发明的轻质高强度瓷砖，机械强度高，不易破碎。
Description
技术领域
本发明属于建筑材料技术领域，尤其涉及轻质高强度瓷砖及其制备方法。
背景技术
瓷砖，是以耐火的金属氧化物及半金属氧化物，经由研磨、混合、压制、施釉、烧结之过程，而形成之一种耐酸碱的瓷质或石质等之建筑或装饰之材料，总称之为瓷砖。其原材料多由粘土、石英沙等等混合而成。随着建筑装饰材料行业的蓬勃发展，市场上的瓷砖、陶瓷类产品规格不断变化，新型、功能性瓷砖的需求日渐增加，其前景愈发广阔。高强度砖可降低基础的造价，节约钢筋混凝土，同时由于加气混凝土隔热，保温效果好，且具有良好的可加工性，施工方便简单，但市面上的高强度砖通常强度都不高，易碎，使用寿命短。
发明内容
本发明的发明目的在于提供一种强度高，使用过程中不易破碎的轻质高强度瓷砖。
为了实现上述发明目的，本发明采用的技术方案如下：
一种轻质高强度瓷砖的制备方法，具体包含以下步骤：
(1)按重量份计，称量如下原料：超轻粘土50-80份、酸洗石英砂45-85份、金属粉末12-20份、白刚玉粉3-5份、高温砂5-7份、煅烧高岭土18-30份、白云石6-8份、电熔莫来石7-11份、粉煤灰陶粒1-3份、火山岩碎屑7-13份、黑云母3-6份、超细硅灰石粉12-18份、粘性胶粉3-5份、乙酰水杨酸1-2份；金属粉末为纳米二氧化钛粉末和氧化锆粉的混合物，其质量比为2.4-3.6:1.0-1.8；所述的粘性胶粉，由以下方法制备得到：
1)取10-20份白色糊精，溶入30-40份蒸馏水中，加入3-5份羟乙基纤维素、4-7份碱木素、1-3份偏硼酸钠，在30-40℃条件下，滴加0.8-1.2份40％浓度醋酸乙烯溶液，滴加完毕后以喷雾形式加入20-30份EVA乳液，搅拌均匀，保温1-2h；
2)将上步所制物离心、水洗，脱水干燥后研磨成粉，至过40目筛为止；
(2)将除超细硅灰石粉以外的配料混合均匀，经初步破碎后放入熔解炉中，加温至1600-1800℃熔融2-3h，冷却，获取熔块；
(3)取出后熔块冷却至常温，放入球磨机中,湿法球磨12-24h，取出后热风干燥3-5h，过100目筛留用，颗粒过大则重复进行此步骤至合格；
(4)将粘性胶粉溶于足量丙酮，200-300r/min搅拌30min后加入超细硅灰石粉，提高搅拌速度至500-700r/min搅拌，同时在混料上方喷洒0.8-1.2份三钛酸异丙酯及1-2份硬脂酸钠，反应2-3h后，于120-140℃下烘干，得改性硅灰石粉；
(5)将破碎后的合格粉料放入搅拌机中，加入适量水和改性硅灰石粉，600-800r/min搅拌1-2h，转速升至800-100r/min搅拌2-3h，60-80℃下微波继续处理1-2h，至呈均匀浆料；
(6)将浆料倒入模具内，抽真空后，经压机压制成型，出炉后静置2-3h，脱模，去除毛边，即得；其中压制程序为：开机升温升压至500℃，30MPa维持8min，继续升至900℃，60MPa维持20min，接着升至1200℃、75MPa维持1h，开始降温降压至1100℃、70MPa维持40min，继续降至1000℃、65MPa维持30min，接着降至800℃、60MPa维持20min，最后冷却，其中，升温速率为30℃/min，降温速率为20℃/min。
进一步的，所述的步骤(3)，湿法球磨中，物料含水率控制在35％-50％。
更进一步的，所述的超细硅灰石粉粒径为1000-1200目，长径比为16-20:1-2。
由于采用了上述技术方案，本发明的有益效果是：
(1)本发明采用阶梯压制成型的方法制备瓷砖，由于配方中火山岩碎屑、酸洗石英砂和莫来石等主要成分多为矿物质，成分复杂，无固定熔点，在1800-2200℃之间均有成分熔化，且各自的粒径及熔体流动性并不一致，经多次实验发现，采用本申请的技术对超细硅灰石粉进行改性后，可有效降低配方中除了硅灰石粉以外的其余组分的熔点，且能将不同熔点的原料在同一个温度条件下熔融，并发现当处于1000℃、65MPa条件下，组分完全熔化，继续升温加压后趋于硬化，当至1300℃、80MPa，制品表面出现龟裂，说明压力及温度超过载荷，故将最高条件设为1200℃、75MPa，而由于组分较多且存在性质差异，相同温度、压力条件下，火山岩、酸洗石英砂、高温砂、电熔莫来石和白刚玉熔融所需时间相比较高岭土、白云母和黑云母的熔融所需时间更长，长达15-20min，因此在原料发生物性变化的时间点上需要进行等温等压的条件维持，若采用直升直降温度的方式，则瓷砖在固化过程中易发生受热不均，各部分固化不完全，导致内部出现孔隙、分层等现象，影响制品性能，因此，在压制成型工艺中，依据原料的熔化-固化特性，将温度、压力变化分段进行并维持相应时长，使得原料在当前压制条件下流动性趋同，组分熔合程度增加，受热、受压均匀，能够得到表面平常，内部缺陷少，强度较大的瓷砖制品。
(2)本发明对超细硅灰石粉进行改性，得到兼具粘性及较大比表面积的改性硅灰石粉，其线膨胀系数小，在高温高压下可与相对收缩率更大的超轻粘土、黑云母等相互交织，形成呈交织结构，金属粉末填充入该结构的空隙中，三者交熔固化，提高了制品密度，增强机械强度。(3)本发明采用压制成型工艺，相比于传统的烧结成型，制成时间短，可批量生产，提高生产效率，且通过此成型工艺制备的瓷砖机械强度优于传统烧结成型。
具体实施方式
为了使本发明实现的技术手段、创作特征、达成目的与功效易于明白了解，下面结合实施例，进一步阐述本发明。应当理解，此处所描述的具体实施例仅仅用以解释本发明，并不用于限定本发明。
实施例1
一种轻质高强度瓷砖的制备方法，具体包含以下步骤：
(1)按重量份计，称量如下原料：超轻粘土50份、酸洗石英砂45份、金属粉末(纳米二氧化钛粉末和氧化锆粉质量比为2.4:1.0的混合物)12份、白刚玉粉3份、高温砂5份、煅烧高岭土18份、白云石6份、电熔莫来石7份、粉煤灰陶粒1份、火山岩碎屑7份、黑云母3份、粒径为1000目，长径比为16:1的超细硅灰石粉12份、粘性胶粉3份、乙酰水杨酸1份
(2)将除超细硅灰石粉以外的配料混合均匀，经初步破碎后放入熔解炉中加温至1600℃熔融3h，冷却，获取熔块；
(3)取出后熔块冷却至常温，放入球磨机中,湿法球磨12h且球磨过程中物料含水率控制在35％，球磨完成后取出后热风干燥3h，过100目筛留用，颗粒过大则重复进行此步骤至合格；
(4)取10份白色糊精，溶入30份蒸馏水中，加入3份羟乙基纤维素、4份碱木素、1份偏硼酸钠，在30℃条件下，滴加0.8份40％浓度醋酸乙烯溶液，滴加完毕后以喷雾形式加入20份EVA乳液，搅拌均匀，保温1h；将上步所制物离心、水洗，脱水干燥后研磨成粉，至过40目筛为止，得粘性胶粉；
(5)将粘性胶粉溶于足量丙酮，200r/min搅拌30min后加入超细硅灰石粉，提高搅拌速度至500r/min搅拌，同时在混料上方喷洒0.8份三钛酸异丙酯及1份硬脂酸钠，反应3h后，于120℃下烘干，得改性硅灰石粉；
(6)将破碎后的合格粉料放入搅拌机中，加入适量水改性硅灰石粉，600r/min搅拌2h，转速升至800r/min搅拌3h，80℃下微波继续处理1h，至呈均匀浆料；
(7)将浆料倒入模具内，抽真空后，经压机压制成型，程序为：开机升温升压至500℃，30MPa维持8min，继续升至900℃，60MPa维持20min，接着升至1200℃、75MPa维持1h，开始降温降压至1100℃、70MPa维持40min，继续降至1000℃、65MPa维持30min，接着降至800℃、60MPa维持20min，最后冷却(其中，升温速率为30℃/min，降温速率为20℃/min)，出炉后静置2h，脱模，去除毛边，即得。
实施例2
一种轻质高强度瓷砖的制备方法，具体包含以下步骤：
(1)按重量份计，称量如下原料超轻粘土65份、酸洗石英砂65份、金属粉末(纳米二氧化钛粉末和氧化锆粉质量比为3.0:1.4的混合物)16份、白刚玉粉4份、高温砂6份、煅烧高岭土23份、白云石4份、电熔莫来石9份、粉煤灰陶粒2份、火山岩碎屑10份、黑云母4.5份、粒径为1100目，长径比为18:1.5超细硅灰石粉15份、粘性胶粉4份、乙酰水杨酸1.5份；
(2)将除超细硅灰石粉以外的配料混合均匀，经初步破碎后放入熔解炉中，加温至1700℃熔融2.5h，冷却，获取熔块；
(3)取出后熔块冷却至常温，放入球磨机中,湿法球磨18h，且球磨过程中物料含水率控制在42.5％，球磨完成后取出后热风干燥4h，过100目筛留用，颗粒过大则重复进行此步骤至合格；
(4)取15份白色糊精，溶入35份蒸馏水中，加入4份羟乙基纤维素、5.5份碱木素、2份偏硼酸钠，在35℃条件下，滴加1.0份40％浓度醋酸乙烯溶液，滴加完毕后以喷雾形式加入25份EVA乳液，搅拌均匀，保温1.5h；将上步所制物离心、水洗，脱水干燥后研磨成粉，至过40目筛为止，得粘性胶粉；
(5)将粘性胶粉溶于足量丙酮，250r/min搅拌30min后加入超细硅灰石粉，提高搅拌速度至600r/min搅拌，同时在混料上方喷洒1.0份三钛酸异丙酯及1.5份硬脂酸钠，反应2.5h后，于130℃下烘干，得改性硅灰石粉；
(6)将破碎后的合格粉料放入搅拌机中，加入适量水改性硅灰石粉，700r/min搅拌1.5h，转速升至900r/min搅拌2.5h，70℃下微波继续处理1.5h，至呈均匀浆料；
(7)将浆料倒入模具内，抽真空后，经压机压制成型，程序为：开机升温升压至500℃，30MPa维持8min，继续升至900℃，60MPa维持20min，接着升至1200℃、75MPa维持1h，开始降温降压至1100℃、70MPa维持40min，继续降至1000℃、65MPa维持30min，接着降至800℃、60MPa维持20min，最后冷却(其中，升温速率为30℃/min，降温速率为20℃/min)，出炉后静置2.5h，脱模，去除毛边，即得。
实施例3
一种轻质高强度瓷砖的制备方法，具体包含以下步骤：
(1)按重量份计，称量如下原料：超轻粘土80份、酸洗石英砂85份、金属粉末(纳米二氧化钛粉末和氧化锆粉质量比为3.6:1.8的混合物)20份、白刚玉粉5份、高温砂7份、煅烧高岭土30份、白云石8份、电熔莫来石11份、粉煤灰陶粒3份、火山岩碎屑13份、黑云母6份、粒径为1200目，长径比为20:2超细硅灰石粉18份、粘性胶粉5份、乙酰水杨酸2份；
(2)将除超细硅灰石粉以外的配料混合均匀，经初步破碎后放入熔解炉中，加温至1800℃熔融2h，冷却，获取熔块；
(3)取出后熔块冷却至常温，放入球磨机中,湿法球磨24h且球磨过程中物料含水率控制在50％，球磨完成后取出后热风干燥3h，过100目筛留用，颗粒过大则重复进行此步骤至合格；
(4)取20份白色糊精，溶入40份蒸馏水中，加入5份羟乙基纤维素、7份碱木素、3份偏硼酸钠，在40℃条件下，滴加1.2份40％浓度醋酸乙烯溶液，滴加完毕后以喷雾形式加入30份EVA乳液，搅拌均匀，保温2h；将上步所制物离心、水洗，脱水干燥后研磨成粉，至过40目筛为止，得粘性胶粉；
(5)将粘性胶粉溶于足量丙酮，200-300r/min搅拌30min后加入超细硅灰石粉，提高搅拌速度至500-700r/min搅拌，同时在混料上方喷洒0.8-1.2份三钛酸异丙酯及1-2份硬脂酸钠，反应2-3h后，于120-140℃下烘干，得改性硅灰石粉；
(6)将破碎后的合格粉料放入搅拌机中，加入适量水改性硅灰石粉，800r/min搅拌1h，转速升至100r/min搅拌2h，60℃下微波继续处理1h，至呈均匀浆料；
(7)将浆料倒入模具内，抽真空后，经压机压制成型，程序为：开机升温升压至500℃，30MPa维持8min，继续升至900℃，60MPa维持20min，接着升至1200℃、75MPa维持1h，开始降温降压至1100℃、70MPa维持40min，继续降至1000℃、65MPa维持30min，接着降至800℃、60MPa维持20min，最后冷却(其中，升温速率为30℃/min，降温速率为20℃/min)，出炉后静置2h，脱模，去除毛边，即得。
性能测试
设置：
对比例1：与实施例1的技术方案基本相同，不同点是步骤(7)中经压机压制成型，程序为：开机以30℃/min升温升压至1200℃、75MPa维持1h，降温降压程序与实施例1相同。
对比例2：与实施例1的技术方案基本相同，不同点是步骤(7)中经压机压制成型，程序为：升温升压程序步骤不变，降温降压程序中以20℃/min直接降至800℃、60MPa维持20min，最后冷却；
对比例3：与实施例1的技术方案基本相同，不同点是压制成型中升温过程保持75MPa压力不变，其余条件不变；
对比例4：与实施例1的技术方案基本相同，不同点是压制成型中降温保持60MPa压力不变，其余条件不变；
对比例5：与实施例1的技术方案基本相同，不同点是成型工艺为传统烧结成型；
对比例6：与实施例1的技术方案基本相同，不同点是轻质高强度瓷砖的制备步骤中直接使用超细硅灰粉；
对比例7：与实施例1的技术方案基本相同，不同点是轻质高强度瓷砖的制备步骤中未添加粘性胶粉。
结果记录于下表：
表一
由上表可知，实施例1-3中，实施例2的测试数据最好，为本发明的最佳实施方案。
(1)对比例1-4为压制成型阶段恒温/恒压制备，从测试数据来看，全面低于实施例1-3与对比例5，说明恒温/恒压制备的产品内部存在缺陷。
(2)对比例5为烧结成型工艺制备，数据较对比例1-4高，仍低于实施例3，说明传统烧结成型制备的瓷砖未能较好发挥组份性能，制品内部仍存在缺陷。
(3)对比例6中，不添加硅灰石粉的制品，机械强度较正常品低，说明硅灰石粉对制品机械强度具有较大影响。
(4)对比例7中，缺少粘性胶粉使得浆料组份的粘结性能下降，成型后的制品，机械强度较低，但下降幅度较对比例6小，说明硅灰石粉对制品性能的影响大于粘性胶粉。
本发明并不局限于前述的具体实施方式。本发明扩展到任何在本说明书中披露的新特征或任何新的组合，以及披露的任一新的方法或过程的步骤或任何新的组合。
Claims (3)
1.一种轻质高强度瓷砖的制备方法，其特征在于，具体包含以下步骤：
(1)按重量份计，称量如下原料：超轻粘土50-80份、酸洗石英砂45-85份、金属粉末12-20份、白刚玉粉3-5份、高温砂5-7份、煅烧高岭土18-30份、白云石6-8份、电熔莫来石7-11份、粉煤灰陶粒1-3份、火山岩碎屑7-13份、黑云母3-6份、超细硅灰石粉12-18份、粘性胶粉3-5份、乙酰水杨酸1-2份；金属粉末为纳米二氧化钛粉末和氧化锆粉的混合物，其质量比为2.4-3.6:1.0-1.8；所述的粘性胶粉由以下方法制备得到：
1)取10-20份白色糊精，溶入30-40份蒸馏水中，加入3-5份羟乙基纤维素、4-7份碱木素、1-3份偏硼酸钠，在30-40℃条件下，滴加0.8-1.2份40％浓度醋酸乙烯溶液，滴加完毕后以喷雾形式加入20-30份EVA乳液，搅拌均匀，保温1-2h；
2)将上步所制物离心、水洗，脱水干燥后研磨成粉，至过40目筛为止；
(2)将除超细硅灰石粉以外的配料混合均匀，经初步破碎后放入熔解炉中，加温至1600-1800℃熔融2-3h，冷却，获取熔块；
(3)取出后熔块冷却至常温，放入球磨机中,湿法球磨12-24h，取出后热风干燥3-5h，过100目筛留用，颗粒过大则重复进行此步骤至合格；
(4)将粘性胶粉溶于足量丙酮，200-300r/min搅拌30min后加入超细硅灰石粉，提高搅拌速度至500-700r/min搅拌，同时在混料上方喷洒0.8-1.2份三钛酸异丙酯及1-2份硬脂酸钠，反应2-3h后，于120-140℃下烘干，得改性硅灰石粉；
(5)将破碎后的合格粉料放入搅拌机中，加入适量水和改性硅灰石粉，600-800r/min搅拌1-2h，转速升至800-100r/min搅拌2-3h，60-80℃下微波继续处理1-2h，至呈均匀浆料；
(6)将浆料倒入模具内，抽真空后，经压机压制成型，出炉后静置2-3h，脱模，去除毛边，即得；其中压制程序为：开机升温升压至500℃，30MPa维持8min，继续升至900℃，60MPa维持20min，接着升至1200℃、75MPa维持1h，开始降温降压至1100℃、70MPa维持40min，继续降至1000℃、65MPa维持30min，接着降至800℃、60MPa维持20min，最后冷却，其中，升温速率为30℃/min，降温速率为20℃/min。
2.根据权利要求1所述的轻质高强度瓷砖的制备方法，其特征在于，所述的步骤(3)，湿法球磨中，物料含水率控制在35％-50％。
3.根据权利要求1所述的轻质高强度瓷砖的制备方法，其特征在于，所述的超细硅灰石粉粒径为1000-1200目，长径比为16-20:1-2。
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