CN113354436B - 一种用于石墨基体的复合耐高温陶瓷组合物及其制备方法和应用 - Google Patents

一种用于石墨基体的复合耐高温陶瓷组合物及其制备方法和应用 Download PDF

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CN113354436B
CN113354436B CN202110841961.5A CN202110841961A CN113354436B CN 113354436 B CN113354436 B CN 113354436B CN 202110841961 A CN202110841961 A CN 202110841961A CN 113354436 B CN113354436 B CN 113354436B
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孟晓东
汪琴
丁毅
周有恒
沈华军
黄晓锋
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Jiangsu Longye Energy Saving Technology Co ltd
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Abstract

本发明公开了一种用于石墨基体的复合耐高温陶瓷组合物及其制备方法和应用，所述组合物的原料组分及配比为：碳化硅30‑40份、石墨20‑30份、二氧化硅30‑40份、高岭土5‑10份、稻壳粉35‑80份、氧化镍1‑5份、纤维4‑8份、偶联剂1‑2份、酚醛树脂70‑90份、有机溶剂100‑120份、分散剂0.5‑1份、pH调节剂1‑2份。

Description

一种用于石墨基体的复合耐高温陶瓷组合物及其制备方法和 应用
技术领域
本发明涉及无机非金属材料技术领域，具体涉及一种用于石墨基体的复合耐高温陶瓷组合物及其制备方法和应用。
背景技术
耐高温涂料可分为有机耐高温涂料和无机耐高温涂料两大类。无机耐高温涂料是一种以无机材料为主要成膜物质的涂料，是由无机聚合物和经过分散活化的金属、金属氧化物纳米材料、稀土超微粉体组成的无机聚合物涂料，能与钢结构表面铁原子快速反应，生成具有物理、化学双重保护作用，通过化学键与基体牢固结合的无机聚合物防腐涂层。无机耐高温涂料相对于有机耐高温涂料往往直接取材于自然界，绝大多数为无毒无机原料。无机材料的生产及使用过程中对环境的污染小，产品多数是以水为分散介质，无环境和健康方面的不良影响，并能阻燃，耐高温达600℃以上。
而现有技术CN203653484U，一种焦炉荒煤气余热利用清扫装置，记载了焦炉上升管是用于导出焦炉荒煤气的设备，焦炉荒煤气的温度在结焦初期为200～400℃，结焦中期400～700℃，结焦末期700～900℃，推焦前或焦炉热修时敞开炉盖和上升管盖后因烟囱效应引入了大量空气，在上升管内燃烧残余碳，上升管内温度可达1600℃，焦炉荒煤气的主要成分即含H2、CO，可知文献提供的耐高温隔热保温涂料若简单的直接应用于所述的焦炉上升管内壁涂覆，因CO侵蚀，涂层表面会慢慢崩裂，最终不能覆盖上升管内壁耐热钢，导致耐热钢在温度过高时产生蠕变，因高温气流的作用而过快腐蚀成片剥落；对文献提供的耐高温隔热保温涂料因结构疏松，在微珠和微珠之间的存在间隙，也不能防止在推焦前或焦炉热修时因引入空气后产生的高温氧化，使耐热钢产生氧化皮的现象。
因此，无机耐高温涂料在一定程度上具有较高的施工难度，且涂膜厚度大、附着力不足，最高耐受温度较低。
发明内容
为了克服现有技术中的不足，本申请提供一种用于石墨基体的复合耐高温陶瓷组合物及其制备方法和应用，具体方案如下：
一种用于石墨基体的复合耐高温陶瓷组合物，所述组合物的原料组分及配比为：碳化硅30-40份、石墨20-30份、二氧化硅30-40份、高岭土5-10份、稻壳粉35-80份、氧化镍1-5份、纤维4-8份、偶联剂1-2份、酚醛树脂70-90份、有机溶剂100-120份、分散剂0.5-1份、pH调节剂1-2份
优选，所述稻壳粉的粒径为10μm至20μm。
优选，所述偶联剂为聚丙烯衍生物；
在本发明的一个特别优选的实施方式中，所述偶联剂为下式(1)所示：
Figure GDA0003645023660000031
其中，a≥1的整数，n≥a的整数。
所述式(1)偶联剂与Ni离子反应，从而将重金属离子固定下来。
当使用所述式(1)偶联剂时，能够与Ni2+形成如下产物：
Figure GDA0003645023660000032
优选，所述分散剂为阴离子型或者非离子型分散剂；所述有机溶剂为无水乙醇或者乙醚。
优选，所述纤维为陶瓷纤维、玻璃纤维或者碳纤维。
一种制备所述组合物的方法，所述方法步骤如下：
步骤一、原料的混合；
步骤二、原料的混练；
步骤三、原料的干燥；
步骤四、原料的造粒成型。
优选，
所述步骤一中，先将有机溶剂与酚醛树脂按照原料配比进行混合，得到溶剂A，再将碳化硅、石墨、二氧化硅、高岭土、稻壳粉、氧化镍、纤维按顺序加入到溶剂A，边搅拌边加入，使加入的固体原料全部浸润；然后再加入偶联剂、分散剂和pH调节剂；
所述步骤二中，保持室温，混练搅拌机转速大于3500r/min，搅拌时间为60min至100min；
所述步骤三中，干燥的温度为80-100℃，干燥的时间为60-72小时；
所述步骤四中采用常规的造粒机进行造粒。
一种所述组合物的应用，所述应用步骤如下：
步骤A：将石墨基体置于密闭的耐火材料匣钵中，并用造粒成型的所述组合物的颗粒包埋；
步骤B：经过1600-1700℃，1小时还原气氛下的烧成，得到具有复合耐高温陶瓷涂层的石墨基体产品。
优选，所述还原气氛为氮气或者氩气等惰性气体条件；所述包埋的厚度为4-7mm。
本发明的涂层在高温下缩合成耐热性强、键能高、具有氧化稳定性的硅氧键、硅碳键，有机高分子均匀分散在“-Si-O-Si-”无机涂层的间隙中，以有机物特有的较好弹性弥补硅氧键的韧性不足，提高涂料的抗干裂性能，其耐高温性可高达1500～1800℃，当涂层中成膜物质充分交联固化，涂层变成致密的网状结构，连续的涂层使氧气和CO难以透入，阻止或减缓高温状态涂层下的基体受氧气氧化或被游离C沉积，涂料中的纤维及氧化镍对氧气和CO的直接扩散和网络内的氧离子迁移有抑制或阻挡作用，氧化镍分散于涂层基胶中，与涂层的偶联剂发生化学反应，形成如下稳定的产物。
Figure GDA0003645023660000051
本发明的耐高温隔热保温涂料中存在Si4+、Ni2+，其半径分别为0.041nm、0.051nm，在涂层涂覆于石墨基体上后，由于耐火高炉内气体温度高达1000～1600℃，Si4+、Ni2+渗进基体界面与之形成界面过渡层，产生“钉合”效应；涂层与基体的结合还包括吸附结合、扩散结合、金属基体的化学键结合。
“搅拌温度为有机热固性树脂熔点以上5℃至30℃”，“搅拌时间为60min至100min”，“继续搅拌60min以上”。用于使无机成膜剂与有机成膜剂中的水分、低分子物质在受热情况下挥发，利用离心力使挥发出的气泡排出，涂料结构更为致密，减少涂料内形成的气泡，带来了使涂料更为致密的技术效果，使耐高温隔热保温涂料更耐腐蚀和耐磨。
有益效果
1、本申请中的偶联剂能够有效结合重金属离子，能够起阻止或延缓涂层裂缝扩展的作用，可适度提高其抗拉、抗弯强度并显著提高其韧性。此外，与一般的偶联剂相比，本发明的聚合物偶联剂不存在重金属浸出的风险，从而极大提高了使用安全性。
2、本申请中的组合物，能够有效的形成复合耐高温陶瓷组合物涂层，对石墨基体形成耐高温的保护，在1000-1500℃的应用环境下，连续工作100小时，失重率变化不超过2％。
具体实施方式
实施例1
一种用于石墨基体的复合耐高温陶瓷组合物，所述组合物的原料组分及配比为：碳化硅30份、石墨20份、二氧化硅30份、高岭土5份、稻壳粉35份、氧化镍1份、纤维4份、偶联剂1份、酚醛树脂70份、有机溶剂100份、分散剂0.5份、pH调节剂1份。
所述稻壳粉的粒径为10μm。
实施例2
一种用于石墨基体的复合耐高温陶瓷组合物，所述组合物的原料组分及配比为：碳化硅40份、石墨30份、二氧化硅40份、高岭土10份、稻壳粉80份、氧化镍5份、纤维8份、偶联剂2份、酚醛树脂90份、有机溶剂120份、分散剂1份、pH调节剂2份
优选，所述稻壳粉的粒径为20μm。
优选，所述偶联剂为聚丙烯衍生物。
实施例3
一种用于石墨基体的复合耐高温陶瓷组合物，所述组合物的原料组分及配比为：碳化硅35份、石墨25份、二氧化硅38份、高岭土9份、稻壳粉70份、氧化镍4份、纤维6份、偶联剂2份、酚醛树脂80份、有机溶剂110份、分散剂1份、pH调节剂2份。
优选，所述稻壳粉的粒径为15μm。
优选，所述偶联剂为
Figure GDA0003645023660000071
其中a为大于1的整数，n为不小于a的整数。
最后应说明的是：显然，上述实施例仅仅是为清楚地说明本申请所作的举例，而并非对实施方式的限定。对于所属领域的普通技术人员来说，在上述说明的基础上还可以做出其它不同形式的变化或变动。这里无需也无法对所有的实施方式予以穷举。而由此所引申出的显而易见的变化或变动仍处于本申请型的保护范围之中。

Claims (8)

1.一种用于石墨基体的复合耐高温陶瓷组合物，其特征在于，所述组合物的原料组分及重量配比为：碳化硅30-40份、石墨20-30份、二氧化硅30-40份、高岭土5-10份、稻壳粉35-80份、氧化镍1-5份、纤维4-8份、偶联剂1-2份、酚醛树脂70-90份、有机溶剂100-120份、分散剂0.5-1份、pH调节剂1-2份；所述偶联剂为下式(1)所示：
Figure FDA0003645023650000011
其中，a≥1的整数，n≥a的整数。
2.根据权利要求1所述的组合物，其特征在于：所述稻壳粉的粒径为10μm至20μm。
3.根据权利要求1所述的组合物，其特征在于：所述分散剂为阴离子型或者非离子型分散剂；所述有机溶剂为无水乙醇或者乙醚。
4.根据权利要求1所述的组合物，其特征在于：所述纤维为陶瓷纤维、玻璃纤维或者碳纤维。
5.一种制备权利要求1所述组合物的方法，其特征在于，所述方法步骤如下：
步骤一、原料的混合；
步骤二、原料的混练；
步骤三、原料的干燥；
步骤四、原料的造粒成型。
6.根据权利要求5所述的方法，其特征在于，
所述步骤一中，先将有机溶剂与酚醛树脂按照原料配比进行混合，得到溶剂A，再将碳化硅、石墨、二氧化硅、高岭土、稻壳粉、氧化镍、纤维按顺序加入到溶剂A，边搅拌边加入，使加入的固体原料全部浸润；然后再加入偶联剂、分散剂和pH调节剂；
所述步骤二中，保持室温，混练搅拌机转速大于3500r/min，搅拌时间为60min至100min；
所述步骤三中，干燥的温度为80-100℃，干燥的时间为60-72小时；
所述步骤四中采用常规的造粒机进行造粒。
7.一种权利要求1所述组合物的应用，其特征在于，所述应用步骤如下：
步骤A：将石墨基体置于密闭的耐火材料匣钵中，并用造粒成型的所述组合物的颗粒包埋；
步骤B：经过1600-1700℃，1小时还原气氛下的烧成，得到具有复合耐高温陶瓷涂层的石墨基体产品。
8.根据权利要求7所述的应用，其特征在于：所述还原气氛为氮气或者氩气惰性气体条件；所述包埋的厚度为4-7mm。
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