CN115196983A - 一种原位催化合成SiCw增强低碳铝碳耐火材料及其制备方法 - Google Patents
一种原位催化合成SiCw增强低碳铝碳耐火材料及其制备方法 Download PDFInfo
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- 238000011065 in-situ storage Methods 0.000 title claims abstract description 49
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- 229910052593 corundum Inorganic materials 0.000 claims abstract description 65
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 44
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- 229910007948 ZrB2 Inorganic materials 0.000 claims abstract description 20
- VWZIXVXBCBBRGP-UHFFFAOYSA-N boron;zirconium Chemical compound B#[Zr]#B VWZIXVXBCBBRGP-UHFFFAOYSA-N 0.000 claims abstract description 20
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- 150000001875 compounds Chemical class 0.000 claims abstract description 7
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- PUZPDOWCWNUUKD-UHFFFAOYSA-M sodium fluoride Chemical compound [F-].[Na+] PUZPDOWCWNUUKD-UHFFFAOYSA-M 0.000 claims description 16
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- KLZUFWVZNOTSEM-UHFFFAOYSA-K Aluminum fluoride Inorganic materials F[Al](F)F KLZUFWVZNOTSEM-UHFFFAOYSA-K 0.000 claims description 11
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- PUAQLLVFLMYYJJ-UHFFFAOYSA-N 2-aminopropiophenone Chemical compound CC(N)C(=O)C1=CC=CC=C1 PUAQLLVFLMYYJJ-UHFFFAOYSA-N 0.000 description 3
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- 238000002441 X-ray diffraction Methods 0.000 description 2
- 239000010941 cobalt Substances 0.000 description 2
- 229910017052 cobalt Inorganic materials 0.000 description 2
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 2
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Abstract
本发明属于低碳铝碳耐火材料技术领域，具体涉及一种原位催化合成SiCw增强低碳铝碳耐火材料及其制备方法，该材料包括以下质量份的原料：60～75份的刚玉颗粒料、5～25份的刚玉微粉、2～5份的碳源、1～4份的硅粉、0.06～0.24份含氟化合物、0～3份铝粉、0～3份二硼化锆粉体，及占上述原料总质量3～8％的酚醛树脂或沥青；制备方法具有工艺易于控制、制备过程污染小和可原位催化制备复合耐火材料的特点。本发明制备的原位催化合成SiCw增强的低碳铝碳耐火材料生成了大量的SiCw，且分布均匀，其拥有更好的常温力学性能、高温力学性能、抗渣性、抗热震性及抗氧化性。
Description
技术领域
本发明属于低碳铝碳耐火材料技术领域，具体涉及一种原位催化合成SiCw增强低碳铝碳耐火材料及其制备方法。
背景技术
铝碳耐火材料以其优异的抗热震性和抗渣性，被广泛地应用于滑板、高炉风口、钢包、转炉等冶金设备。但是传统的铝碳耐火材料因碳含量高，致使其强度低、抗氧化性差、热损耗高，且浪费石墨资源，同时也会在炼钢过程中使钢水增碳。随着洁净钢质量要求的提高，使 Al2O3-C耐火材料向着低碳化发展。但碳含量的降低会导致Al2O3-C耐火材料的抗热震性、抗渣侵蚀性能等明显下降，严重影响其高温性能。
碳化硅晶须(SiCw)具有熔点高、抗拉强度高、弹性模量高等优异性能。将其引入陶瓷材料、耐火材料基体中，可以显著提高基体的高温力学性能。但SiCw由外部直接引入到基体材料中存在着晶须分散困难、成本高，且对人体健康有害等系列缺点。因此，晶须原位反应生成技术受到研究人员的广泛重视。原位反应法具有制备工艺简单、晶须分布均匀等优点，但该方法存在反应温度高、晶须不易形成，需在制备过程中加入铁、钴和镍等催化剂，该方法虽然可以原位制备出形貌可控的碳化硅晶须，但是铁、钴和镍熔点低，加入后会降低铝碳耐火材料的高温力学性能，且钴和镍价格相对昂贵，很难规模化生产。
现有原位生成碳化硅晶须增强低碳铝碳耐火材料制备技术存在反应温度高，能耗大，反应速率慢，不易生成碳化硅晶须等缺点，极大限制了原位生成碳化硅晶须增强低碳铝碳耐火材料的应用和规模化生产。
发明内容
本发明的目的在于克服传统技术中存在的上述问题，提供一种原位催化合成SiCw增强低碳铝碳耐火材料及其制备方法。
为实现上述技术目的，达到上述技术效果，本发明是通过以下技术方案实现：
一种原位催化合成SiCw增强低碳铝碳耐火材料，包括以下质量份的原料：60～75份的刚玉颗粒料、5～25份的刚玉微粉、2～5份的碳源、 1～4份的硅粉、0.06～0.24份含氟化合物、0～3份铝粉、0～3份二硼化锆粉体，及占上述原料总质量3～8％的酚醛树脂或沥青。
进一步地，上述原位催化合成SiCw增强低碳铝碳耐火材料中，所述刚玉颗粒料由粒径为5-3mm、3-1mm和1-0mm的板状刚玉或电熔刚玉混合而成。
进一步地，上述原位催化合成SiCw增强低碳铝碳耐火材料中，所述刚玉微粉的粒径为0.1～50μm。
进一步地，上述原位催化合成SiCw增强低碳铝碳耐火材料中，所述氟化物粉末为氟化钠、氟化铝、氟化镁、氟化锆中的至少一种，氟化钠、氟化铝、氟化镁、氟化锆为工业纯或为分析纯。
进一步地，上述原位催化合成SiCw增强低碳铝碳耐火材料中，所述碳源为鳞片石墨、纳米炭黑、葡萄糖、壳聚糖、膨胀石墨中的至少一种。
进一步地，上述原位催化合成SiCw增强低碳铝碳耐火材料中，所述硅粉的粒径≤100μm。
如上所述的原位催化合成SiCw增强低碳铝碳耐火材料的制备方法，包括如下步骤：
1)按配比将含氟化合物、铝粉、刚玉微粉、二硼化锆粉体、硅粉和碳源混合均匀，制得预混合粉体；
2)将不同粒度的刚玉颗粒料进行轮碾，然后添加1/2总量的酚醛树脂或液态沥青，轮碾3～5分钟，制得预混合刚玉骨料；
3)将步骤1)制得的预混合粉体加入至步骤2)制得的预混合刚玉骨料，然后加入剩余1/2总量的酚醛树脂或液态沥青，轮碾5～10分钟，制得混合料；
4)将步骤3)制得的混合料置于密闭环境中静置困料一段时间，然后压制成型，制得坯体；
5)将步骤4)制得的坯体置于烘箱中固化一段时间，再将其埋碳置于高温下热处理一段时间，即可制得原位催化生成SiCw增强低碳铝碳耐火材料。
进一步地，步骤4)中，将混合料置于密闭环境中静置困料 12～36h。
进一步地，步骤4)中，静置困料后，将混合料在100～200MPa下压制成型。
进一步地，步骤5)中，将坯体置于150～220℃的烘箱中固化 18-36h，再将其埋碳置于1200～1600℃下热处理1～8h。
本发明的有益效果是：
1、本发明制备方法所采用的催化剂均安全无毒；粘结剂对操作人员和环境危害小；使用的有机物含量低，所用原料可以加入到复合耐火材料中直接原位生成晶须，以此提高复合耐火材料的高温性能，适于规模化生产；工艺简单，可直接使用自动液压机压制成型。
2、本发明制备的原位催化合成SiCw增强的低碳铝碳耐火材料生成了大量的SiCw，且分布均匀；相对于现有的低碳铝碳耐火材料，其拥有更好的常温力学性能、高温力学性能、抗渣性、抗热震性及抗氧化性。
当然，实施本发明的任一产品并不一定需要同时达到以上的所有优点。
附图说明
为了更清楚地说明本发明实施例的技术方案，下面将对实施例描述所需要使用的附图作简单地介绍，显而易见地，下面描述中的附图仅仅是本发明的一些实施例，对于本领域普通技术人员来讲，在不付出创造性劳动的前提下，还可以根据这些附图获得其他的附图。
图1为本发明实施例1制备低碳铝碳耐火材料的SEM图；
图2为本发明实施例1制备低碳铝碳耐火材料的XRD图。
具体实施方式
下面将结合本发明实施例中的附图，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。
本发明提供一种原位催化合成SiCw增强低碳铝碳耐火材料，包括以下质量份的原料：60～75份的刚玉颗粒料、5～25份的刚玉微粉、2～5 份的碳源、1～4份的硅粉、0.06～0.24份含氟化合物、0～3份铝粉、0～3 份二硼化锆粉体，及占上述原料总质量3～8％的酚醛树脂或沥青。
本发明中，刚玉颗粒料由粒径为5-3mm、3-1mm和1-0mm的板状刚玉或电熔刚玉混合而成。
本发明中，刚玉微粉的粒径为0.1～50μm。
本发明中，氟化物粉末为氟化钠、氟化铝、氟化镁、氟化锆中的至少一种，氟化钠、氟化铝、氟化镁、氟化锆为工业纯或为分析纯。
本发明中，碳源为鳞片石墨、纳米炭黑、葡萄糖、壳聚糖、膨胀石墨中的至少一种。
本发明中，硅粉的粒径≤100μm。
本发明提供一种原位催化合成SiCw增强低碳铝碳耐火材料的制备方法，包括如下步骤：
1)按配比将含氟化合物、铝粉、刚玉微粉、二硼化锆粉体、硅粉和碳源混合均匀，制得预混合粉体；
2)将不同粒度的刚玉颗粒料进行轮碾，然后添加1/2总量的酚醛树脂或液态沥青，轮碾3～5分钟，制得预混合刚玉骨料；
3)将步骤1)制得的预混合粉体加入至步骤2)制得的预混合刚玉骨料，然后加入剩余1/2总量的酚醛树脂或液态沥青，轮碾5～10分钟，制得混合料；
4)将步骤3)制得的混合料置于密闭环境中静置困料12～36h，然后在100～200MPa下压制成型，制得坯体；
5)将步骤4)制得的坯体置于150～220℃的烘箱中固化18-36h，再将其埋碳置于1200～1600℃下热处理1～8h，即可制得原位催化生成 SiCw增强低碳铝碳耐火材料。
本发明的具体实施例如下：
实施例1
本实施例的原位催化生成SiCw增强低碳铝碳耐火材料，按质量百分比，其原料组成为75％的刚玉颗粒料、12％的刚玉微粉、5％的鳞片石墨、4％的硅粉、0.24％氟化铝、1％铝粉、2.76％二硼化锆粉体，及占上述原料总质量5％的沥青。
本实施例原位催化生成SiCw增强低碳铝碳耐火材料的制备方法为：
(1)按氟化铝:铝粉:刚玉微粉:二硼化锆粉体:硅粉:碳源摩尔比为0.004:0.08:0.16:0.06:0.36:1，将含氟化铝、铝粉、刚玉微粉、二硼化锆粉体、硅粉和碳源混合均匀，制得预混合粉体。
(2)将不同粒度的刚玉颗粒料进行轮碾，然后添加总质量1/2的液态沥青轮碾3-5分钟，制得预混合刚玉骨料。
(3)将(1)中的预混合粉体加入至(2)预混合刚玉骨料，然后加入剩余1/2的液态沥青轮碾8分钟，制得混合料。
(4)将(3)混合料置于密闭环境中静置困料24h，然后在110MPa 下压制成型，制得坯体。
(5)将(4)中坯体置于200℃的烘箱中固化24h后，将其埋碳置于1600℃下热处理2h，制得原位催化生成SiCw增强低碳铝碳耐火材料。
本实施例所得SiCw增强低碳铝碳耐火材料的显气孔率为15.5％、常温耐压强度达94.3MPa，常温抗折强度达17.2MPa。
实施例2
本实施例的原位催化生成SiCw增强低碳铝碳耐火材料，按质量百分比，其原料组成为70％的刚玉颗粒料、17％的刚玉微粉、4％的膨胀石墨、5％的硅粉、0.06％氟化钠、1％铝粉、2.94％二硼化锆粉体，及占上述原料总质量5％的酚醛树脂。
本实施例原位催化生成SiCw增强低碳铝碳耐火材料的制备方法为：
(1)按氟化钠:铝粉:刚玉微粉:二硼化锆粉体:硅粉:碳源摩尔比为 0.0045:0.1:0.3:0.1:0.5:1，将含氟化钠、铝粉、刚玉微粉、二硼化锆粉体、硅粉和碳源混合均匀，制得预混合粉体。
(2)将不同粒度的刚玉颗粒料进行轮碾，然后添加总质量1/2的酚醛树脂轮碾3-5分钟，制得预混合刚玉骨料。
(3)将(1)中的预混合粉体加入至(2)预混合刚玉骨料，然后加入剩余1/2的酚醛树脂轮碾8分钟，制得混合料。
(4)将(3)混合料置于密闭环境中静置困料18h，然后在120MPa 下压制成型，制得坯体。
(5)将(4)中坯体置于200℃的烘箱中固化30h后，将其埋碳置于1200℃下热处理2h，制得原位催化生成SiCw增强低碳铝碳耐火材料。
本实施例所得SiCw增强低碳铝碳耐火材料的显气孔率为17.5％、常温耐压强度达78.8MPa，常温抗折强度达14.6MPa。
实施例3
本实施例的原位催化生成SiCw增强低碳铝碳耐火材料，按质量百分比，其原料组成为70％的刚玉颗粒料、20％的刚玉微粉、2％的纳米炭黑、3％的硅粉、0.18％氟化锆、3％铝粉、1.82％二硼化锆粉体，及占上述原料总质量5％的酚醛树脂。
本实施例原位催化生成SiCw增强低碳铝碳耐火材料的制备方法为：
(1)按氟化锆:铝粉:刚玉微粉:二硼化锆粉体:硅粉:碳源摩尔比为 0.006:0.7:0.3:0.1:0.6:1将含氟化锆、铝粉、刚玉微粉、二硼化锆粉体、硅粉和碳源混合均匀，制得预混合粉体。
(2)将不同粒度的刚玉颗粒料进行轮碾，然后添加总质量1/2的酚醛树脂轮碾3-5分钟，制得预混合刚玉骨料。
(3)将(1)中的预混合粉体加入至(2)预混合刚玉骨料，然后加入剩余1/2的酚醛树脂轮碾8分钟，制得混合料。
(4)将(3)混合料置于密闭环境中静置困料28h，然后在130MPa 下压制成型，制得坯体。
(5)将(4)中坯体置于180℃的烘箱中固化20h后，将其埋碳置于1500℃下热处理2h，制得原位催化生成SiCw增强低碳铝碳耐火材料。
本实施例所得SiCw增强低碳铝碳耐火材料的显气孔率为15.9％、常温耐压强度达87.8MPa，常温抗折强度达15.8MPa。
实施例4
本实施例的原位催化生成SiCw增强低碳铝碳耐火材料，按质量百分比，其原料组成为73％的刚玉颗粒料、18％的刚玉微粉、1％的壳聚糖、4％的硅粉、0.24％氟化镁、2％铝粉、1.76％二硼化锆粉体，及占上述原料总质量5％的沥青。
本实施例原位催化生成SiCw增强低碳铝碳耐火材料的制备方法为：
(1)按氟化镁:铝粉:刚玉微粉:二硼化锆粉体:硅粉:碳源摩尔比为 0.04:0.8:1:0.18:1.8:1，将含氟化镁、铝粉、刚玉微粉、二硼化锆粉体、硅粉和碳源混合均匀，制得预混合粉体。
(2)将不同粒度的刚玉颗粒料进行轮碾，然后添加总质量1/2的液态沥青轮碾3-5分钟，制得预混合刚玉骨料。
(3)将(1)中的预混合粉体加入至(2)预混合刚玉骨料，然后加入剩余1/2的液态沥青轮碾8分钟，制得混合料。
(4)将(3)混合料置于密闭环境中静置困料20h，然后在140MPa 下压制成型，制得坯体。
(5)将(4)中坯体置于200℃的烘箱中固化20h后，将其埋碳置于1300℃下热处理2h，制得原位催化生成SiCw增强低碳铝碳耐火材料。
本实施例所得SiCw增强低碳铝碳耐火材料的显气孔率为16.3％、常温耐压强度达83.4MPa，常温抗折强度达14.3MPa。
实施例5
本实施例的原位催化生成SiCw增强低碳铝碳耐火材料，按质量百分比，其原料组成为70％的刚玉颗粒料、20％的刚玉微粉、1％的纳米炭黑、1％的鳞片石墨、4％的硅粉、0.12％氟化铝、2％铝粉、1.88％二硼化锆粉体，及占上述原料总质量5％的酚醛树脂。
本实施例原位催化生成SiCw增强低碳铝碳耐火材料的制备方法为：
(1)按氟化铝:铝粉:刚玉微粉:二硼化锆粉体:硅粉:碳源摩尔比为 0.008:0.4:0.3:0.1:0.9:1，将含氟化铝、铝粉、刚玉微粉、二硼化锆粉体、硅粉和碳源混合均匀，制得预混合粉体。
(2)将不同粒度的刚玉颗粒料进行轮碾，然后添加总质量1/2的酚醛树脂轮碾3-5分钟，制得预混合刚玉骨料。
(3)将(1)中的预混合粉体加入至(2)预混合刚玉骨料，然后加入剩余1/2的酚醛树脂轮碾8分钟，制得混合料。
(4)将(3)混合料置于密闭环境中静置困料24h，然后在150MPa 下压制成型，制得坯体。
(5)将(4)中坯体置于200℃的烘箱中固化24h后，将其埋碳置于1400℃下热处理2h，制得原位催化生成SiCw增强低碳铝碳耐火材料。
本实施例所得SiCw增强低碳铝碳耐火材料的显气孔率为14.8％、常温耐压强度达108.2MPa，常温抗折强度达20.7MPa。
图1和图2分别为本实施例所制备的原位催化合成SiCw增强低碳铝碳耐火材料的SEM图和XRD图。从图1中可以看出所制备的试样中形成了大量的SiCw，且分布均匀。从图2可以看出，所制备的试样中生成了碳化硅。
以上公开的本发明优选实施例只是用于帮助阐述本发明。优选实施例并没有详尽叙述所有的细节，也不限制该发明仅为具体实施方式。显然，根据本说明书的内容，可作很多的修改和变化。本说明书选取并具体描述这些实施例，是为了更好地解释本发明的原理和实际应用，从而使所属技术领域技术人员能很好地理解和利用本发明。本发明仅受权利要求书及其全部范围和等效物的限制。
Claims (10)
1.一种原位催化合成SiCw增强低碳铝碳耐火材料，其特征在于，包括以下质量份的原料：60～75份的刚玉颗粒料、5～25份的刚玉微粉、2～5份的碳源、1～4份的硅粉、0.06～0.24份含氟化合物、0～3份铝粉、0～3份二硼化锆粉体，及占上述原料总质量3～8％的酚醛树脂或沥青。
2.根据权利要求1所述的原位催化合成SiCw增强低碳铝碳耐火材料，其特征在于：所述刚玉颗粒料由粒径为5-3mm、3-1mm和1-0mm的板状刚玉或电熔刚玉混合而成。
3.根据权利要求1所述的原位催化合成SiCw增强低碳铝碳耐火材料，其特征在于：所述刚玉微粉的粒径为0.1～50μm。
4.根据权利要求1所述的原位催化合成SiCw增强低碳铝碳耐火材料，其特征在于：所述氟化物粉末为氟化钠、氟化铝、氟化镁、氟化锆中的至少一种，氟化钠、氟化铝、氟化镁、氟化锆为工业纯或为分析纯。
5.根据权利要求1所述的原位催化合成SiCw增强低碳铝碳耐火材料，其特征在于：所述碳源为鳞片石墨、纳米炭黑、葡萄糖、壳聚糖、膨胀石墨中的至少一种。
6.根据权利要求1所述的原位催化合成SiCw增强低碳铝碳耐火材料，其特征在于：所述硅粉的粒径≤100μm。
7.如权利要求1所述的原位催化合成SiCw增强低碳铝碳耐火材料的制备方法，其特征在于，包括如下步骤：
1)按配比将含氟化合物、铝粉、刚玉微粉、二硼化锆粉体、硅粉和碳源混合均匀，制得预混合粉体；
2)将不同粒度的刚玉颗粒料进行轮碾，然后添加1/2总量的酚醛树脂或液态沥青，轮碾3～5分钟，制得预混合刚玉骨料；
3)将步骤1)制得的预混合粉体加入至步骤2)制得的预混合刚玉骨料，然后加入剩余1/2总量的酚醛树脂或液态沥青，轮碾5～10分钟，制得混合料；
4)将步骤3)制得的混合料置于密闭环境中静置困料一段时间，然后压制成型，制得坯体；
5)将步骤4)制得的坯体置于烘箱中固化一段时间，再将其埋碳置于高温下热处理一段时间，即可制得原位催化生成SiCw增强低碳铝碳耐火材料。
8.根据权利要求7所述的制备方法，其特征在于：步骤4)中，将混合料置于密闭环境中静置困料12～36h。
9.根据权利要求7所述的制备方法，其特征在于：步骤4)中，静置困料后，将混合料在100～200MPa下压制成型。
10.根据权利要求7所述的制备方法，其特征在于：步骤5)中，将坯体置于150～220℃的烘箱中固化18-36h，再将其埋碳置于1200～1600℃下热处理1～8h。
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