CN110330319A - 一种低碳超低碳的铝碳烧成耐火材料及其制备方法 - Google Patents

一种低碳超低碳的铝碳烧成耐火材料及其制备方法 Download PDF

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CN110330319A
CN110330319A CN201910632420.4A CN201910632420A CN110330319A CN 110330319 A CN110330319 A CN 110330319A CN 201910632420 A CN201910632420 A CN 201910632420A CN 110330319 A CN110330319 A CN 110330319A
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carbon
low
ultra
refractory material
aluminium
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黄军同
熊庆明
陈智
李秋燕
刘明强
李喜宝
胡智辉
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Nanchang Hangkong University
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Nanchang Hangkong University
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Abstract

本发明公开了一种低碳超低碳的铝碳烧成耐火材料及其制备方法，该耐火材料是以Al2O3基耐火集料和鳞片状碳素物为主要原料，添加抗氧化剂和炭黑，以酚醛树脂为结合剂、硝酸盐为催化剂。其技术方案是：配置硝酸盐的酒精溶液，加入到酚醛树脂中搅拌，然后将0.5～5wt％鳞片状碳素物加入其中搅拌形成混合液；将混合液加入到三辊研磨机循环剥离1～20次，得到微纳米石墨薄片的树脂基混合物；将集料颗粒放入混炼机中干混，然后加入水浴加热后的树脂基混合物继续混炼，最后加入集料细粉、抗氧化剂和炭黑形成的混合细粉混炼制成泥料，将泥料压制成砖坯；将砖坯在150～300℃烘烤固化后在1100～1550℃烧成，即得到低碳超低碳的铝碳烧成耐火材料。

Description

一种低碳超低碳的铝碳烧成耐火材料及其制备方法
技术领域
本发明涉及耐火材料技术领域，具体涉及一种低碳超低碳的铝碳烧成耐火材料及其制备方法。
背景技术
铝碳质耐火材料主要以氧化铝和碳素为原料，用沥青或树脂等有机结合剂黏结而成的碳复合特种耐火材料，按照工艺不同可分为不烧铝炭质耐火材料和烧成铝炭质耐火材料。后者在连铸上应用广泛，大量用于滑动水口系统的滑板砖和连铸三大件(长水口、浸入式水口和整体塞棒)。滑板砖是作为控制钢水流量和流速的开关，安装在钢包和中间包底部，需长时间承受1600℃左右的高温钢液的化学侵蚀以及承重压力，因此，要求滑板砖具有较高的耐高温强度、优良的耐侵蚀性、抗冲刷性和抗热震稳定性。长水口、浸入式水口主要起到保护浇筑的作用，塞棒起到控流的作用。长水口的作用是在浇筑过程中隔断空气避免精炼后的钢水被空气氧化、吸入氮气，由于钢水在长水口内迅速通过，长水口必须要具有良好的耐热震性、抗钢水冲击性和抗渣侵蚀性能。浸入式水口可调节钢水的流动状态，防止保护渣等非金属夹杂物卷入钢水，防止钢水二次氧化和使结晶器内铸坯断面热流分布均匀等功能，浸入式水口渣线要求抗保护渣侵蚀性能优异，而本体则要求耐热震、抗冲刷且能防止Al2O3附着阻塞水口，整体塞棒控制中间包和结晶器间的钢水流量，用塞棒还可向钢水中喷吹氩气等惰性气体，还可以防止水口絮瘤，减少铸坯中及杂物含量和总氧含量，因其要控制开浇和停浇，所以塞棒头部必须抗冲刷、与浸入式水口能很好配合，同时渣线还必须具有较好的抗侵蚀性能来抵抗中间包钢渣的侵蚀。
滑板砖和连铸三大件质量的好坏对于连铸生产的连续性和稳定性具有重要意义。铝碳质耐火材料的氧化是影响该材料寿命的主要因素，而且铝碳质耐火材料中与钢水直接接触的碳(石墨)在钢水中会发生溶解，铝碳质耐火材料的脱碳会造成钢水中碳含量的增加改变钢的组成，影响钢水的洁净度。洁净钢生产用耐火材料正向着低碳化甚至无碳化发展。但如果大幅度直接减少铝碳耐火材料中的碳含量，必然会使材料的抗热震性和抗侵蚀性降低，影响铝碳耐火材料的使用寿命。为了解决上诉问题，围绕着优化Al2O3-C耐火材料中的碳的结构与组织，开发新技术制备低碳超低铝碳耐火材料迫在眉睫。
发明内容
本发明所要解决的问题是：提供一种低碳超低碳的铝碳烧成耐火材料及其制备方法，该材料不仅碳含量低，而且综合性能优异。
本发明为解决上述问题所提供的技术方案为：一种低碳超低碳的铝碳烧成耐火材料，所述的低碳超低碳的铝碳烧成耐火材料是以耐火集料和碳素物为主要原料成分，加入抗氧化剂、结合剂和催化剂；原料组分按重量百分数计为：集料颗粒55～75wt％、集料细粉15～25wt％、2～6wt％的酚醛树脂结合剂、0.5～5wt％的碳素物原料、另外加入0.1～1wt％的炭黑、0～0.5wt％的硝酸盐化合物、0.1～3.5wt％的抗氧化剂；所述的碳素物原料为鳞片石墨、膨胀石墨中的一种或两种混合物；所述的硝酸盐化合物为无水硝酸镍、无水硝酸铁、无水硝酸钴中的一种或者两种以上。
优选的，所述集料颗粒为电熔刚玉、烧结刚玉或烧结板状刚玉、特级或I级优质矾土熟料，其Al2O3含量为≥98wt％；集料颗粒占总配料55～75wt％，其中粒度5～3mm的占总配料的12～25wt％，粒度3～1mm的占总配料的25～35wt％，粒度1～0mm的占总配料的10～20wt％；所述集料细粉为刚玉细粉、电熔莫来石细粉、烧成莫来石细粉或锆莫来石细粉，其粒度≤0.074mm，占总配料的15～25wt％。
优选的，所述抗氧化剂为金属Si粉、Al粉、SiC粉、硼化物中的任意一种或者几种，粒径≤0.074mm。
优选的，所述硼化物为B4C或BN或ZrB2或CaB6。
一种低碳超低碳的铝碳烧成耐火材料的制备方法，所述制备方法包括以下步骤，
(1)先将0～1wt％的硝酸盐化合物配制成质量百分数浓度为1～30wt％的无水酒精溶液；
(2)将(1)中配制好的硝酸盐酒精溶液倒入2～6wt％的酚醛树脂结合剂中搅拌混合1～15min，再将0.5～5wt％的碳素物倒入其中进行搅拌混合2～20min，形成均匀分散的混合物；
(3)然后将(2)中的混合物从进料辊加入到三辊研磨机进行三辊差速剥离，循环剥离1～20次后，从出料辊收集得到石墨剥离形成的微纳米石墨薄片均匀分散在含硝酸盐的酚醛树脂基混合物；
(4)为降低(3)中收集得到的酚醛树脂基混合物的粘度以增加流动性，将其在35℃～90℃水浴中进行5～30min的加热；
(5)将占总配料15～25wt％的集料细粉、0.1～3.5wt％的抗氧化剂、0.1～1wt％的炭黑混合均匀，得到混合细粉；
(6)将占总配料55～75wt％的集料颗粒放入混炼机(湿碾机)中干混1～15min,然后加入(4)中加热后的酚醛树脂基混合物继续混炼3～15min，最后加入(5)中的集料细粉、抗氧化剂和炭黑形成的混合细粉继续混炼4～12min制成泥料，然后困料1～24h；
(7)将困好的泥料加入模具中采用复合式摩擦压砖机或等静压机进行压制成型制成砖坯；
(8)将成型的砖坯烘烤固化后，然后在1100～1550℃的温度下保温5～24h，即得到所述的一种低碳超低碳的铝碳烧成耐火材料。
优选的，所述步骤(3)中三辊研磨机中的三辊速率的转速比为N3(进料辊):N2(中心辊):N1(出料辊)在1:1.5:3～1:3:9以内，每个辊轴之间的间隙为0.01～0.2mm。
优选的，所述步骤(8)中烘烤温度150～300℃，烘烤时间为5～24h。
与现有技术相比，本发明的优点是：1)以鳞片石墨、膨胀石墨用作起始原料，通过三辊研磨差速剥离技术获得结晶效果好且比表面积大、均匀分散在酚醛树脂中的微纳米石墨薄片，能够有效降低外加纳米碳引起的成本和关联的均匀分散问题；2)剥离后的微纳米石墨薄片均匀分散在酚醛树脂中进而在整个Al2O3-C耐火材料基质中更有效、均匀的分布，整体碳含量可大幅度减少；3)与碳含量高的材料相比，低碳的Al2O3-C材料中集料颗粒之间的间距小，在材料的工作表面容易形成富Al2O3的保护层，阻碍氧的传输，从而抑制材料中碳的氧化，提高材料抗氧化性能；4)石墨薄片的纵横比将被保留甚至有所增加，所以原来的增强/增韧机理也不会丢失甚至可能得到强化，从而耐热冲击性和抗侵蚀能力可保留甚至得到改善；5)制备得到的低碳、超低碳Al2O3-C耐火材料在1100～1550℃的烧成温度下部分酚醛树脂会被硝酸盐原位催化反应形成碳纳米管、碳纳米纤维以及在外加抗氧化剂时产生的SiC晶须，这都可显著提升产品的高温抗折、抗热震稳定性、抗氧化性能、耐剥落性能。
具体实施方式
以下将通过实施例来详细说明本发明的实施方式，藉此对本发明如何应用技术手段来解决技术问题并达成技术功效的实现过程能充分理解并据以实施。
实施例1
一种低碳超低碳的铝碳烧成耐火材料及其制备方法，本实施例在不添加催化剂的情况下先以1wt％的鳞片石墨一起倒入3wt％的热固型液体酚醛树脂中搅拌混合15min；然后将混合物从进料辊加入到三辊研磨机进行三辊差速剥离，三辊研磨机中的三辊速率的转速比N3(进料辊):N2(中心辊):N1(出料辊)为1:3:6，进料辊与中心辊之间的间隙为0.05mm，中心辊与出料辊之间的间隙为0.01mm，循环剥离5次后，从出料辊收集得到剥离形成微纳米石墨薄片均匀分散在酚醛树脂基混合物；将收集得到的酚醛树脂基混合物在40℃水浴中进行28min的加热；将20.5wt％的烧成莫来石细粉、0.5wt％的Si粉、0.5wt％的Al粉、0.3wt％的炭黑混合均匀，得到混合细粉；将占总配料74.2wt％的电熔刚玉放入混炼机(湿碾机)中干混15min，粒度5～3mm的占总配料的24.2wt％，粒度3～1mm的占总配料的33wt％，粒度1～0mm的占总配料的17wt％，然后加入加热后的树脂基混合物继续混炼15min，最后加入烧成莫来石细粉、Si粉、Al粉和炭黑形成的混合细粉继续混炼10min制成泥料，然后困料24h；将困好的泥料加入模具中采用复合式摩擦压砖机进行压制成型制成砖坯；将成型的砖坯置于隧道式干燥窑中烘烤固化后，烘烤温度200℃，烘烤时间为10h；然后在1200℃的温度下保温16h，即得到所述的一种超低碳的铝碳烧成耐火材料。
所制备得到的一种含原位剥离的二维纳米石墨片酚醛树脂结合的低碳镁碳耐火材料制品的性能如下：体积密度：3.08g/cm3，显气孔率：12.2％，常温耐压强度：130.8MPa，常温抗折强度：28.2MPa，高温抗折强度(1400℃*3h)：14.7MPa。
实施例2
一种低碳超低碳的铝碳烧成耐火材料及其制备方法，本实施先将0.01wt％的无水硝酸镍配制成质量百分数浓度为10wt％的无水酒精溶液，将配制好的硝酸镍酒精溶液倒入4wt％的酚醛树脂结合剂中搅拌混合5min，再将1wt％的膨胀石墨倒入其中进行搅拌混合12min，形成均匀分散的混合物；然后将混合物从进料辊加入到三辊研磨机进行三辊差速剥离，循环剥离10次后，从出料辊收集得到石墨剥离形成的微纳米石墨薄片均匀分散在含无水硝酸镍的酚醛树脂基混合物；三辊研磨机中的三辊速率的转速比N3(进料辊):N2(中心辊):N1(出料辊)为1:3:9，进料辊与中心辊之间的间隙为0.04mm，中心辊与出料辊之间的间隙为0.02mm；为降低收集得到的酚醛树脂基混合物的粘度以增加流动性，将其在50℃水浴中进行22min的加热；将21wt％的刚玉细粉、0.79wt％的SiC粉、0.7wt％的Al粉和0.5wt％的炭黑混合均匀，得到混合细粉；将占总配料72wt％的烧结板状刚玉，粒度5～3mm的占总配料的22wt％，粒度3～1mm的占总配料的32wt％，粒度1～0mm的占总配料的18wt％，放入混炼机(湿碾机)中干混15min，然后加入加热后的树脂基混合物继续混炼15min，最后加入刚玉细粉、SiC粉、Al粉和炭黑形成的混合细粉继续混炼10min制成泥料，然后困料24h；将困好的泥料加入模具中采用复合式摩擦压砖机进行压制成型制成砖坯；将成型的砖坯置于隧道式干燥窑中烘烤固化后，烘烤温度200℃，烘烤时间为10h，然后在1200℃的温度下保温16h，即得到所述的一种超低碳的铝碳烧成耐火材料。
所制备得到的一种含原位剥离的二维纳米石墨片酚醛树脂结合的低碳镁碳耐火材料制品的性能如下：体积密度：3.16g/cm3，显气孔率：6.2％，常温耐压强度：164.3MPa，常温抗折强度：36.8MPa，高温抗折强度(1400℃*3h)：16.8MPa。
实施例3
一种低碳超低碳的铝碳烧成耐火材料及其制备方法，本实施先将0.1wt％的无水硝酸镍配制成浓度为15wt％的无水酒精溶液，将配制好的硝酸镍酒精溶液倒入5wt％的酚醛树脂结合剂中搅拌混合8min，再将4wt％的膨胀石墨倒入其中进行搅拌混合10min，形成均匀分散的混合物；然后将混合物从进料辊加入到三辊研磨机进行三辊差速剥离，循环剥离10次后，从出料辊收集得到石墨剥离形成的微纳米石墨薄片均匀分散在含无水硝酸镍的酚醛树脂基混合物；三辊研磨机中的三辊速率的转速比N3(进料辊):N2(中心辊):N1(出料辊)为1:3:8，进料辊与中心辊之间的间隙为0.1mm，中心辊与出料辊之间的间隙为0.02mm；为降低收集得到的酚醛树脂基混合物的粘度以增加流动性，将其在60℃水浴中进行18min的加热；将18.6wt％的刚玉细粉、0.5wt％的Si粉、0.8wt％炭黑混合均匀，得到混合细粉；将占总配料71wt％的烧结刚玉颗粒，粒度5～3mm的占总配料的24wt％，粒度3～1mm的占总配料的32wt％，粒度1～0mm的占总配料的15wt％，放入混炼机(湿碾机)中干混15min，然后加入加热后的树脂基混合物继续混炼15min，最后加入刚玉细粉、Si粉和炭黑形成的混合细粉继续混炼10min制成泥料，然后困料24h；将困好的泥料加入模具中采用复合式摩擦压砖机进行压制成型制成砖坯；将成型的砖坯置于隧道式干燥窑中烘烤固化后，烘烤温度200℃，烘烤时间为10h，然后在1250℃的温度下保温16h，即得到所述的所述的一种超低碳的铝碳烧成耐火材料。
所制备得到的一种含原位剥离的二维纳米石墨片酚醛树脂结合的低碳镁碳耐火材料制品的性能如下：体积密度：3.12g/cm3，显气孔率：6.9％，常温耐压强度：158.3MPa，常温抗折强度：32.6MPa，高温抗折强度(1400℃*3h)：15.2MPa。
实施例4
一种低碳超低碳的铝碳烧成耐火材料及其制备方法，本实施先将0.2wt％的无水硝酸钴配制成质量百分数浓度为25wt％的无水酒精溶液，将配制好的硝酸钴酒精溶液倒入5wt％的酚醛树脂结合剂中搅拌混合8min，再将3wt％的膨胀石墨倒入其中进行搅拌混合15min，形成均匀分散的混合物；然后将混合物从进料辊加入到三辊研磨机进行三辊差速剥离，循环剥离10次后，从出料辊收集得到石墨剥离形成的微纳米石墨薄片均匀分散在含无水硝酸钴的酚醛树脂基混合物；三辊研磨机中的三辊速率的转速比N3(进料辊):N2(中心辊):N1(出料辊)为1:3:7，进料辊与中心辊之间的间隙为0.04mm，中心辊与出料辊之间的间隙为0.01mm；为降低收集得到的酚醛树脂基混合物的粘度以增加流动性，将其在65℃水浴中进行16min的加热；将25wt％的电熔莫来石细粉、0.45wt％的Si粉、0.3wt％的ZrB2粉、0.25wt％炭黑混合均匀，得到混合细粉；将占总配料65.8wt％的烧结板状刚玉，其中粒度5～3mm的占总配料的18wt％，粒度3～1mm的占总配料的30wt％，粒度1～0mm的占总配料的17.8wt％，放入混炼机(湿碾机)中干混15min，然后加入中加热后的树脂基混合物继续混炼15min，最后加入电熔莫来石细粉、Si粉、ZrB2粉和炭黑形成的混合细粉继续混炼10min制成泥料，然后困料24h；将困好的泥料加入模具中采用复合式摩擦压砖机进行压制成型制成砖坯；将成型的砖坯置于隧道式干燥窑中烘烤固化后，烘烤温度200℃，烘烤时间为10h，然后在1300℃的温度下保温16h，即得到所述的所述的一种超低碳的铝碳烧成耐火材料。
所制备得到的一种含原位剥离的二维纳米石墨片酚醛树脂结合的低碳镁碳耐火材料制品的性能如下：体积密度：3.09g/cm3，显气孔率：7.5％，常温耐压强度：152.7MPa，常温抗折强度：30.3MPa，高温抗折强度(1400℃*3h)：14.8MPa。
实施例5
一种低碳超低碳的铝碳烧成耐火材料及其制备方法，本实施先将0.5wt％的无水硝酸钴配制成质量百分数浓度为30wt％的无水酒精溶液，将配制好的硝酸钴酒精溶液倒入5wt％的酚醛树脂结合剂中搅拌混合10min，再将5wt％的膨胀石墨倒入其中进行搅拌混合15min，形成均匀分散的混合物；然后将混合物从进料辊加入到三辊研磨机进行三辊差速剥离，循环剥离10次后，从出料辊收集得到石墨剥离形成的微纳米石墨薄片均匀分散在含无水硝酸钴的酚醛树脂基混合物；三辊研磨机中的三辊速率的转速比N3(进料辊):N2(中心辊):N1(出料辊)为1:3:9，进料辊与中心辊之间的间隙为0.06mm，中心辊与出料辊之间的间隙为0.02mm；为降低收集得到的酚醛树脂基混合物的粘度以增加流动性，将其在80℃水浴中进行10min的加热；将18wt％的烧成莫来石细粉、1wt％的B4C粉、0.5wt％炭黑混合均匀，得到混合细粉；将占总配料70wt％的烧结板状刚玉，其中粒度5～3mm的占总配料的21wt％，粒度3～1mm的占总配料的31wt％，粒度1～0mm的占总配料的18wt％，放入混炼机(湿碾机)中干混15min，然后加入中加热后的树脂基混合物继续混炼15min，最后加入中的烧成莫来石细粉、B4C粉、炭黑形成的混合细粉继续混炼10min制成泥料，然后困料24h；将困好的泥料加入模具中采用等静压成型制成砖坯；将成型的砖坯置于隧道式干燥窑中烘烤固化后，烘烤温度200℃，烘烤时间为10h，然后在1350℃的温度下保温24h，即得到所述的所述的一种超低碳的铝碳烧成耐火材料。
所制备得到的所述的一种超低碳的铝碳烧成耐火材料制品的性能如下：体积密度：2.89g/cm3，显气孔率：12.8％，常温耐压强度：132.7MPa，常温抗折强度：25.8MPa，高温抗折强度(1400℃*3h)：12.8MPa。
以上仅就本发明的最佳实施例作了说明，但不能理解为是对权利要求的限制。本发明不仅局限于以上实施例，其具体结构允许有变化。凡在本发明独立权利要求的保护范围内所作的各种变化均在本发明保护范围内。

Claims (7)

1.一种低碳超低碳的碳铝碳烧成耐火材料，所述的低碳超低碳的铝碳烧成耐火材料是以耐火集料和碳素物为主要原料成分，加入抗氧化剂、结合剂和催化剂；其特征在于：原料组分按重量百分数计为：集料颗粒55～75wt％、集料细粉15～25wt％、2～6wt％的酚醛树脂结合剂、0.5～5wt％的碳素物原料、另外加入0.1～1wt％的炭黑、0～0.5wt％的硝酸盐化合物、0.1～3.5wt％的抗氧化剂；所述的碳素物原料为鳞片石墨、膨胀石墨中的一种或两种混合物；所述的硝酸盐化合物为无水硝酸镍、无水硝酸铁、无水硝酸钴中的一种或者两种以上。
2.根据权利要求1所述的一种低碳超低碳的铝碳烧成耐火材料，其特征在于：所述集料颗粒为电熔刚玉、烧结刚玉或烧结板状刚玉、特级或I级优质矾土熟料，其Al2O3含量为≥98wt％；集料颗粒占总配料55～75wt％，其中粒度5～3mm的占总配料的12～25wt％，粒度3～1mm的占总配料的25～35wt％，粒度1～0mm的占总配料的10～20wt％；所述集料细粉为刚玉细粉、电熔莫来石细粉、烧成莫来石细粉或锆莫来石细粉，其粒度≤0.074mm，占总配料的15～25wt％。
3.根据权利要求1所述的一种低碳超低碳的铝碳烧成的耐火材料，其特征在于：所述抗氧化剂为金属Si粉、Al粉、SiC粉、硼化物中的任意一种或者几种，粒径≤0.074mm。
4.根据权利要求3所述的一种低碳超低碳的铝碳烧成耐火材料，其特征在于：所述硼化物为B4C或BN或ZrB2或CaB6。
5.如权利要求1或4任一所述的一种低碳超低碳的铝碳烧成耐火材料的制备方法，其特征在于：所述制备方法包括以下步骤，
(1)先将0～1wt％的硝酸盐化合物配制成质量百分数浓度为1～30wt％的无水酒精溶液；
(2)将(1)中配制好的硝酸盐酒精溶液倒入2～6wt％的酚醛树脂结合剂中搅拌混合1～15min，再将0.5～5wt％的碳素物倒入其中进行搅拌混合2～20min，形成均匀分散的混合物；
(3)然后将(2)中的混合物从进料辊加入到三辊研磨机进行三辊差速剥离，循环剥离1～20次后，从出料辊收集得到石墨剥离形成的微纳米石墨薄片均匀分散在含硝酸盐的酚醛树脂基混合物；
(4)为降低(3)中收集得到的酚醛树脂基混合物的粘度以增加流动性，将其在35℃～90℃水浴中进行5～30min的加热；
(5)将占总配料15～25wt％的集料细粉、0.1～3.5wt％的抗氧化剂、0.1～1wt％的炭黑混合均匀，得到混合细粉；
(6)将占总配料55～75wt％的集料颗粒放入混炼机(湿碾机)中干混1～15min,然后加入(4)中加热后的酚醛树脂基混合物继续混炼3～15min，最后加入(5)中的集料细粉、抗氧化剂和炭黑形成的混合细粉继续混炼4～12min制成泥料，然后困料1～24h；
(7)将困好的泥料加入模具中采用复合式摩擦压砖机或等静压机进行压制成型制成砖坯；
(8)将成型的砖坯烘烤固化后，然后在1100～1550℃的温度下保温5～24h，即得到所述的一种低碳超低碳的铝碳烧成耐火材料。
6.根据权利要求5所述的一种低碳超低碳的铝碳烧成耐火材料的制备方法，其特征在于：所述步骤(3)中三辊研磨机中的三辊速率的转速比为N3(进料辊):N2(中心辊):N1(出料辊)在1:1.5:3～1:3:9以内，每个辊轴之间的间隙为0.01～0.2mm。
7.根据权利要求5所述的一种低碳超低碳的铝碳烧成耐火材料的制备方法，其特征在于：所述步骤(8)中烘烤温度150～300℃，烘烤时间为5～24h。
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