CN114714691A - 一种新型陶瓷一体化板及其加工工艺 - Google Patents

一种新型陶瓷一体化板及其加工工艺 Download PDF

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CN114714691A
CN114714691A CN202210484391.3A CN202210484391A CN114714691A CN 114714691 A CN114714691 A CN 114714691A CN 202210484391 A CN202210484391 A CN 202210484391A CN 114714691 A CN114714691 A CN 114714691A
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ceramic
integrated plate
stirring
expanded graphite
waste
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王壮
徐成
邢杰
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Anhui Dinghuan Energy Saving Technology Co ltd
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Abstract

本发明公开了一种新型陶瓷一体化板及其加工工艺，所述陶瓷一体化板包括保温层和装饰层，保温层包括聚氨酯硬质泡沫层和泡沫陶瓷层，装饰层为防护漆层。本发明采用泡沫陶瓷和聚氨酯硬质泡沫作为一体化板的主体，泡沫陶瓷不仅实现废物利用，而且通过调节烧成温度达到气孔率最高和导热系数最小，得到隔热、高性能泡沫陶瓷材料；聚氨酯硬质泡沫中加入了阻燃剂和增强填料，增强填料经过改性处理，不仅能够提高分散，提高增强效果，而且能够与聚氨酯基体产生键合作用，提高聚氨酯的耐热性能；此外，增强填料为改性膨胀石墨，其对聚磷酸铵的阻燃具有协同促进作用；使一体化板在提升阻燃性能的基础上，不会对物理机械性能造成降低。

Description

一种新型陶瓷一体化板及其加工工艺
技术领域
本发明属于建筑材料技术领域，具体地，涉及一种新型陶瓷一体化板及其加工工艺。
背景技术
陶瓷一体化板又称为陶瓷保温装饰一体化板，由粘结层、保温装饰产品板、锚固件、密封材料等组成。应用广泛，不仅适用于新建的外墙保温装饰，也适用于旧建筑的节能装饰；适用于各种公共建筑和住宅建筑的外墙保温；适用于北方寒冷地区和南方炎热地区。陶瓷保温装饰一体化板具有诸多优点，从主要原材料、无尘车间自动化、加工工艺到节点冷桥处理，比传统节能保温施工方法具有更多、更好的保温功能，完成施工保温一体化。
现有技术中多采用聚氨酯硬质泡沫作为陶瓷一体化板的主体材质之一，而为了提升其阻燃性能，会在聚氨酯合成过程中掺入阻燃剂，但是阻燃剂的加入会一定程度对聚氨酯的力学性能有所影响，为了提升机械性能，又会考虑加入无机填料进行增强，但是无机填料难以于聚合物基体分散均匀，难以实现阻燃性能和物理机械性能的同步提高，从而限制了聚氨酯硬泡在陶瓷一体化板中的应用。
发明内容
本发明的目的在于克服现有技术的缺陷，提供了一种新型陶瓷一体化板及其加工工艺。
本发明的目的可以通过以下技术方案实现：
一种新型陶瓷一体化板，包括保温层和装饰层，保温层包括聚氨酯硬质泡沫层和泡沫陶瓷层，装饰层为防护漆层。
进一步地，泡沫陶瓷由如下步骤制备：
将破碎球磨后的膨胀蛭石在800℃煅烧2h后，过100目筛，再将废弃粉煤灰和废弃陶瓷片的混合物破碎球磨后过100目筛；
将膨胀蛭石粉、废弃粉煤灰和废弃陶瓷片混合物粉、滑石粉、碳化硅按比例混合，球磨1h，然后加入PVA溶液(质量分数8％)，继续充分研磨，之后液压成型制得陶瓷生坯，将压制好的陶瓷生坯放置在马弗炉中以10℃/min的升温速率上升至900℃，保温30min，再以5℃/min的升温速率上升至1040-1050℃，保温60min后随炉冷却，得到泡沫陶瓷；
其中，膨胀蛭石粉、废弃粉煤灰和废弃陶瓷片混合物粉、滑石粉、碳化硅、PVA溶液的用量比为30g:20g:5g:5g:20mL；
利用膨胀蛭石、废弃粉煤灰和废弃陶瓷片为主要原料，添加碳化硅为造孔剂，滑石为助熔剂制备泡沫陶瓷，通过调节烧成温度达到气孔率最高和导热系数最小；泡沫陶瓷中无机固体废弃物(废弃粉煤灰、废弃陶瓷片)所占比例可达1/3，在消化大量无机固体废弃物的同时，产品本身作为外墙外保温或其他隔热部位的保温材料，可以实现节能环保目的；
聚氨酯硬质泡沫通过如下步骤制备：
向多元醇中加入聚磷酸铵和增强填料，搅拌均匀后倒入一定质量的发泡剂正戊烷和PAPI(多苯基多亚甲基异氰酸酯)，以800r/s高速搅拌15s，倒入模具中，室温条件下自然发泡成型，成型后脱模；然后放入105℃的烘箱中熟化，制得聚氨酯硬质泡沫；
多元醇为聚醚多元醇，多元醇的用量与PAPI的质量之比为3:2；聚磷酸铵和增强填料的加入质量分别为多元醇质量的30％和10％；
进一步地，增强填料通过如下步骤制备：
S1、将膨胀石墨置于三口烧瓶内，缓缓加入体积比为3:1的浓硫酸和浓硝酸混合液，搅拌的同时超声波分散70-90min，再升温至60℃搅拌反应3h，反应液自然冷却至室温，抽滤，去离子水洗涤至滤液为中性；滤饼放入80℃干燥箱干燥至恒重，研磨，过筛，得到酸化膨胀石墨；膨胀石墨与浓酸的用量比为1g：50-60mL；
膨胀石墨在浓酸的作用下，在表面发生氧化反应，在膨胀石墨的表面引入-COOH基团；
S2、将酸化膨胀石墨置于三口烧瓶中，加入无水甲苯，N2保护下，搅拌同时超声分散40-50min，加热至60℃，加入TDI并滴入二月桂酸二丁基锡，搅拌反应10h；抽滤，用无水甲苯洗涤至滤液中无TDI，将滤饼置于45℃真空干燥箱干燥12h，研磨，过筛，得到产物；
酸化膨胀石墨、无水甲苯、TDI、二月桂酸二丁基锡的用量比为5g：300mL：50-54g：0.2mL；
膨胀石墨表面引入的-COOH与TDI(甲苯二异氰酸酯)的一个-NCO基团发生反应，在膨胀石墨表面引入苯环和-NCO(TDI上含有两个-NCO，在位阻作用的影响以及反应条件的控制下，另一个-NCO不会继续与膨胀石墨表面的-COOH反应，剩余一个裸露的-NCO)，膨胀石墨表面引入TDI分子，能够避免填料骨架的直接接触，从而能够提高填料的分散效果，发挥增强效果；引入的-NCO能够直接参与聚氨酯聚合过程，使得增强填料与聚合物基体之间产生键合作用，生成具有微交联网状结构的复合材料，使高分子链段运动受到限制，构象改变需要更高的能量，进而提高聚氨酯泡沫的抗热变形能力；另外，膨胀石墨对聚磷酸铵的阻燃效果具有促进作用，能够协同促进聚氨酯泡沫的阻燃效果。
陶瓷一体化板的加工工艺，包括如下步骤：
在聚氨酯硬质泡沫层与泡沫陶瓷层的接触面上涂覆胶黏剂，在15-35℃下，将粘结的一体板在压力机上压制4-6小时；再于泡沫陶瓷的另一侧表面涂布防护漆，得到陶瓷一体化板。
本发明的有益效果：
本发明采用泡沫陶瓷和聚氨酯硬质泡沫作为一体化板的主体，泡沫陶瓷不仅实现废物利用，而且通过调节烧成温度达到气孔率最高和导热系数最小，得到隔热、高性能泡沫陶瓷材料；聚氨酯硬质泡沫中加入了阻燃剂(聚磷酸铵)和增强填料，增强填料经过改性处理，不仅能够提高分散，提高增强效果，而且能够与聚氨酯基体产生键合作用，提高聚氨酯的耐热性能；此外，增强填料为改性膨胀石墨，其对聚磷酸铵的阻燃具有协同促进作用，更进一步提高聚氨酯硬泡的阻燃效果；使制得的一体化板在提升阻燃性能的基础上，不会对物理机械性能造成降低。
具体实施方式
下面将结合本发明实施例，对本发明实施例中的技术方案进行清楚、完整地描述，显然，所描述的实施例仅仅是本发明一部分实施例，而不是全部的实施例。基于本发明中的实施例，本领域普通技术人员在没有作出创造性劳动前提下所获得的所有其它实施例，都属于本发明保护的范围。
实施例1
制备泡沫陶瓷：
将破碎球磨后的膨胀蛭石在800℃煅烧2h后，过100目筛，再将废弃粉煤灰和废弃陶瓷片的混合物破碎球磨后过100目筛；
将膨胀蛭石粉、废弃粉煤灰和废弃陶瓷片混合物粉、滑石粉、碳化硅按比例混合，球磨1h，然后加入PVA溶液(质量分数8％)，继续充分研磨，之后液压成型制得陶瓷生坯，将压制好的陶瓷生坯放置在马弗炉中以10℃/min的升温速率上升至900℃，保温30min，再以5℃/min的升温速率上升至1040℃，保温60min后随炉冷却，得到泡沫陶瓷；
其中，膨胀蛭石粉、废弃粉煤灰和废弃陶瓷片混合物粉、滑石粉、碳化硅、PVA溶液的用量比为30g:20g:5g:5g:20mL。
实施例2
制备泡沫陶瓷：
将破碎球磨后的膨胀蛭石在800℃煅烧2h后，过100目筛，再将废弃粉煤灰和废弃陶瓷片的混合物破碎球磨后过100目筛；
将膨胀蛭石粉、废弃粉煤灰和废弃陶瓷片混合物粉、滑石粉、碳化硅按比例混合，球磨1h，然后加入PVA溶液(质量分数8％)，继续充分研磨，之后液压成型制得陶瓷生坯，将压制好的陶瓷生坯放置在马弗炉中以10℃/min的升温速率上升至900℃，保温30min，再以5℃/min的升温速率上升至1050℃，保温60min后随炉冷却，得到泡沫陶瓷；
其中，膨胀蛭石粉、废弃粉煤灰和废弃陶瓷片混合物粉、滑石粉、碳化硅、PVA溶液的用量比为30g:20g:5g:5g:20mL。
实施例3
制备增强填料：
S1、将膨胀石墨置于三口烧瓶内，缓缓加入体积比为3:1的浓硫酸和浓硝酸混合液，搅拌的同时超声波分散70min，再升温至60℃搅拌反应3h，反应液自然冷却至室温，抽滤，去离子水洗涤至滤液为中性；滤饼放入80℃干燥箱干燥至恒重，研磨，过筛，得到酸化膨胀石墨；膨胀石墨与浓酸的用量比为1g：50mL；
S2、将酸化膨胀石墨置于三口烧瓶中，加入无水甲苯，N2保护下，搅拌同时超声分散40min，加热至60℃，加入TDI并滴入二月桂酸二丁基锡，搅拌反应10h；抽滤，用无水甲苯洗涤至滤液中无TDI，将滤饼置于45℃真空干燥箱干燥12h，研磨，过筛，得到产物；酸化膨胀石墨、无水甲苯、TDI、二月桂酸二丁基锡的用量比为5g：300mL：50g：0.2mL。
实施例4
制备增强填料：
S1、将膨胀石墨置于三口烧瓶内，缓缓加入体积比为3:1的浓硫酸和浓硝酸混合液，搅拌的同时超声波分散80min，再升温至60℃搅拌反应3h，反应液自然冷却至室温，抽滤，去离子水洗涤至滤液为中性；滤饼放入80℃干燥箱干燥至恒重，研磨，过筛，得到酸化膨胀石墨；膨胀石墨与浓酸的用量比为1g：55mL；
S2、将酸化膨胀石墨置于三口烧瓶中，加入无水甲苯，N2保护下，搅拌同时超声分散45min，加热至60℃，加入TDI并滴入二月桂酸二丁基锡，搅拌反应10h；抽滤，用无水甲苯洗涤至滤液中无TDI，将滤饼置于45℃真空干燥箱干燥12h，研磨，过筛，得到产物；酸化膨胀石墨、无水甲苯、TDI、二月桂酸二丁基锡的用量比为5g：300mL：52g：0.2mL。
实施例5
制备增强填料：
S1、将膨胀石墨置于三口烧瓶内，缓缓加入体积比为3:1的浓硫酸和浓硝酸混合液，搅拌的同时超声波分散90min，再升温至60℃搅拌反应3h，反应液自然冷却至室温，抽滤，去离子水洗涤至滤液为中性；滤饼放入80℃干燥箱干燥至恒重，研磨，过筛，得到酸化膨胀石墨；膨胀石墨与浓酸的用量比为1g：60mL；
S2、将酸化膨胀石墨置于三口烧瓶中，加入无水甲苯，N2保护下，搅拌同时超声分散50min，加热至60℃，加入TDI并滴入二月桂酸二丁基锡，搅拌反应10h；抽滤，用无水甲苯洗涤至滤液中无TDI，将滤饼置于45℃真空干燥箱干燥12h，研磨，过筛，得到产物；酸化膨胀石墨、无水甲苯、TDI、二月桂酸二丁基锡的用量比为5g：300mL：54g：0.2mL。
实施例6
聚氨酯硬质泡沫通过如下步骤制备：
向多元醇中加入聚磷酸铵和实施例3制备的增强填料，搅拌均匀后倒入一定质量的发泡剂正戊烷和PAPI(多苯基多亚甲基异氰酸酯)，以800r/s高速搅拌15s，倒入模具中，室温条件下自然发泡成型，成型后脱模；然后放入105℃的烘箱中熟化，制得聚氨酯硬质泡沫；
多元醇为聚醚多元醇，多元醇的用量与PAPI的质量之比为3:2；聚磷酸铵和增强填料的加入质量分别为多元醇质量的30％和10％。
实施例7
聚氨酯硬质泡沫通过如下步骤制备：
向多元醇中加入聚磷酸铵和实施例4制备的增强填料，搅拌均匀后倒入一定质量的发泡剂正戊烷和PAPI(多苯基多亚甲基异氰酸酯)，以800r/s高速搅拌15s，倒入模具中，室温条件下自然发泡成型，成型后脱模；然后放入105℃的烘箱中熟化，制得聚氨酯硬质泡沫；
多元醇为聚醚多元醇，多元醇的用量与PAPI的质量之比为3:2；聚磷酸铵和增强填料的加入质量分别为多元醇质量的30％和10％。
实施例8
聚氨酯硬质泡沫通过如下步骤制备：
向多元醇中加入聚磷酸铵和实施例5制备的增强填料，搅拌均匀后倒入一定质量的发泡剂正戊烷和PAPI(多苯基多亚甲基异氰酸酯)，以800r/s高速搅拌15s，倒入模具中，室温条件下自然发泡成型，成型后脱模；然后放入105℃的烘箱中熟化，制得聚氨酯硬质泡沫；
多元醇为聚醚多元醇，多元醇的用量与PAPI的质量之比为3:2；聚磷酸铵和增强填料的加入质量分别为多元醇质量的30％和10％。
对比例1
将实施例6中的增强填料换为未经任何处理的膨胀石墨，其余原料及制备过程不变。
对比例2
将实施例6中的增强填料原料去掉，其余原料及制备过程不变。
对实施例6-8和对比例1-2制得的聚氨酯硬质泡沫做如下性能测试：
其中密度的测定按GB/T6343-2009《泡沫塑料及橡胶表观密度的测定》进行。压缩强度的测定按GB/T8813-2008《硬质泡沫塑料压缩性能的测定》进行。导热系数的测定按GB/T10294-2008《绝热材料稳态热阻及有关特性的测定防护热板法》进行。阻燃性的测定按GB/T2406.2-2009《塑料用氧指数法测定燃烧行为第2部分室温试验》进行。测试结果如下表所示：
Figure BDA0003628661090000081
由上表可知，实施例6-8制得的聚氨酯硬质泡沫具有较高的力学性能和阻燃性能；由对比例1的数据可知，膨胀石墨经过改性处理后，能够提高与聚合物基体的相互作用，进而提高力学性能和协同提高聚磷酸铵的阻燃效果；由对比例2的数据可知，膨胀石墨能够对聚磷酸铵的阻燃性能起到协同提高的作用。
实施例9
制备陶瓷一体化板：
在聚氨酯硬质泡沫层与泡沫陶瓷层的接触面上涂覆胶黏剂，在15℃下，将粘结的一体板在压力机上压制4小时；再于泡沫陶瓷的另一侧表面涂布防护漆，得到陶瓷一体化板。
实施例10
制备陶瓷一体化板：
在聚氨酯硬质泡沫层与泡沫陶瓷层的接触面上涂覆胶黏剂，在20℃下，将粘结的一体板在压力机上压制5小时；再于泡沫陶瓷的另一侧表面涂布防护漆，得到陶瓷一体化板。
实施例11
制备陶瓷一体化板：
在聚氨酯硬质泡沫层与泡沫陶瓷层的接触面上涂覆胶黏剂，在35℃下，将粘结的一体板在压力机上压制6小时；再于泡沫陶瓷的另一侧表面涂布防护漆，得到陶瓷一体化板。
在说明书的描述中，参考术语“一个实施例”、“示例”、“具体示例”等的描述意指结合该实施例或示例描述的具体特征、结构、材料或者特点包含于本发明的至少一个实施例或示例中。在本说明书中，对上述术语的示意性表述不一定指的是相同的实施例或示例。而且，描述的具体特征、结构、材料或者特点可以在任何的一个或多个实施例或示例中以合适的方式结合。
以上内容仅仅是对本发明所作的举例和说明，所属本技术领域的技术人员对所描述的具体实施例做各种各样的修改或补充或采用类似的方式替代，只要不偏离发明或者超越本权利要求书所定义的范围，均应属于本发明的保护范围。

Claims (8)

1.一种新型陶瓷一体化板，包括保温层和装饰层，保温层包括聚氨酯硬质泡沫层和泡沫陶瓷层，装饰层为防护漆层，其特征在于，聚氨酯硬质泡沫通过如下步骤制备：
向多元醇中加入聚磷酸铵和增强填料，搅拌均匀后倒入一定质量的发泡剂正戊烷和PAPI，以800r/s高速搅拌15s，倒入模具中，室温条件下自然发泡成型，成型后脱模；然后放入105℃的烘箱中熟化，制得聚氨酯硬质泡沫。
2.根据权利要求1所述的一种新型陶瓷一体化板，其特征在于，增强填料通过如下步骤制备：
S1、将膨胀石墨置于三口烧瓶内，缓缓加入体积比为3:1的浓硫酸和浓硝酸混合液，搅拌的同时超声波分散70-90min，再升温至60℃搅拌反应3h，反应液自然冷却至室温，抽滤，去离子水洗涤至滤液为中性；滤饼放入80℃干燥箱干燥至恒重，研磨，过筛，得到酸化膨胀石墨；
S2、将酸化膨胀石墨置于三口烧瓶中，加入无水甲苯，N2保护下，搅拌同时超声分散40-50min，加热至60℃，加入TDI并滴入二月桂酸二丁基锡，搅拌反应10h；抽滤，用无水甲苯洗涤至滤液中无TDI，将滤饼置于45℃真空干燥箱干燥12h，研磨，过筛，得到产物。
3.根据权利要求2所述的一种新型陶瓷一体化板，其特征在于，步骤S1中膨胀石墨与浓酸的用量比为1g：50-60mL。
4.根据权利要求2所述的一种新型陶瓷一体化板，其特征在于，步骤S2中酸化膨胀石墨、无水甲苯、TDI、二月桂酸二丁基锡的用量比为5g：300mL：50-54g：0.2mL。
5.根据权利要求1所述的一种新型陶瓷一体化板，其特征在于，泡沫陶瓷由如下步骤制备：
将破碎球磨后的膨胀蛭石在800℃煅烧2h后，过100目筛，再将废弃粉煤灰和废弃陶瓷片的混合物破碎球磨后过100目筛；
将膨胀蛭石粉、废弃粉煤灰和废弃陶瓷片混合物粉、滑石粉、碳化硅按比例混合，球磨1h，然后加入PVA溶液，继续充分研磨，之后液压成型制得陶瓷生坯，将压制好的陶瓷生坯放置在马弗炉中以10℃/min的升温速率上升至900℃，保温30min，再以5℃/min的升温速率上升至1040-1050℃，保温60min后随炉冷却，得到泡沫陶瓷。
6.根据权利要求5所述的一种新型陶瓷一体化板，其特征在于，膨胀蛭石粉、废弃粉煤灰和废弃陶瓷片混合物粉、滑石粉、碳化硅、PVA溶液的用量比为30g:20g:5g:5g:20mL。
7.根据权利要求5所述的一种新型陶瓷一体化板，其特征在于，PVA溶液的质量分数8％。
8.根据权利要求1所述的一种新型陶瓷一体化板的加工工艺，其特征在于，包括如下步骤：
在聚氨酯硬质泡沫层与泡沫陶瓷层的接触面上涂覆胶黏剂，在15-35℃下，将粘结的一体板在压力机上压制4-6小时；再于泡沫陶瓷的另一侧表面涂布防护漆，得到陶瓷一体化板。
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