CN110386812A - 一种耐高温高强度耐热瓷的制备方法 - Google Patents
一种耐高温高强度耐热瓷的制备方法 Download PDFInfo
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Abstract
本发明涉及一种耐高温高强度耐热瓷的制备方法,属于无机非金属材料技术领域。本发明首先将甘蔗渣与水稻秸秆混合烘干,烘干后粉碎与盐酸混合,混合后过滤洗涤得到有机混合物,随后将有机混合物与氢氧化钠溶液混合,搅拌后加入铝粉混合反应制得改性浆液,然后加入柠檬酸溶液反应,加入高锰酸钾反应,反应后浓缩制得浓缩反应产物,随后进行高温处理制得热炭化纤维,最后将热炭化纤维与长石、滑石以及其它物料混合研磨,压制成型、高温焙烧制得耐高温高强度耐热瓷,本发明从甘蔗渣和水稻秸秆中提取植物纤维成分,利用纤维成分与其它成分之间的粘结作用提高耐热瓷的结构强度,纤维中再引入铝离子增强纤维的结构强度,具有广阔的应用前景。
Description
技术领域
本发明涉及一种耐高温高强度耐热瓷的制备方法,属于无机非金属材料技术领域。
背景技术
陶瓷是以天然粘土以及各种天然矿物为主要原料经过粉碎混炼、成型和煅烧制得的材料的各种制品;以前人们把用陶土制作成的在专门的窑炉中高温烧制的物品称作陶瓷,陶瓷是陶器和瓷器的总称,陶瓷的传统概念是指所有以粘土等无机非金属矿物为原料的人工工业产品,它包括由粘土或含有粘土的混合物经混炼,成形,煅烧而制成的各种制品,由最粗糙的土器到最精细的精陶和瓷器都属于它的范围,陶瓷产品对水有一定的吸附渗透能力,水如果被吸进陶瓷,会产生一定的膨胀,容易使陶瓷表面的釉面因膨胀而龟裂,吸水率不合格的产品,在使用中吸收水分后容易引起坯体吸湿膨胀,可能产生裂纹。
随着社会的发展,人们生活水平的提高,对陶瓷用品的要求也越发提高,现有的热传导及抗热震性能差,无法适应各种热源,因而无法满足各种形式烹饪的需要,在急冷即热环境下,容易破裂损坏。
高耐热瓷器的研究一直是日用陶瓷领域的一个难题,现有的耐热陶瓷制品具有如下缺点:一是耐热温度通常只能达到400-500℃,消费者在使用该类陶瓷制品时,常常食材快熟了,陶瓷制品也就裂了,不但浪费食材,也具有极大的安全隐患;二是热膨胀系数较高,为2-4×10-6/℃,抗热冲击性能较差,热交换容易破裂,不能在较苛刻的环境下使用。申请人对德化地区现有的耐热陶瓷制品进行了成分分析,发现通常的耐热陶瓷制品原料中铝、硅、镁和锂的成分比例约为24-26∶60-62∶2-4∶1-2。
因此亟需发明一种抗冲击、抗压性能良好同时耐高温性能优异的耐热瓷。
发明内容
本发明所要解决的技术问题:针对目前耐热瓷在高温条件下易开裂,力学性能下降使耐热瓷的脆性变高、抗冲击性能下降的缺陷,提供了一种耐高温高强度耐热瓷的制备方法。
为解决上述技术问题,本发明采用的技术方案是:
一种耐高温高强度耐热瓷的制备方法,其特征在于具体制备步骤为:
将热炭化纤维、滑石、黏土、长石、氯化钙粉末投入行星球磨机中,在转速为100~120r/min和球料比为10:1的条件下研磨60~80min得到预制混料,将预制混料进行压制成型,投入窑炉中,在温度为1100~1200℃的条件下焙烧80~100min,冷却后即得耐高温高强度耐热瓷。
所述的热炭化纤维的具体制备步骤为:
(1)将改性浆液倒入三口烧瓶中,将三口烧瓶置于水浴温度为30~40℃的水浴锅中,用搅拌器以500~600r/min的转速搅拌60~80min制得反应混合液,向烧杯中加入质量分数为10~15%的柠檬酸溶液,用搅拌器以300~360r/min的转速搅拌30~40min制得酸性反应液;
(2)向三口烧瓶中加入高锰酸钾粉末,将三口烧瓶置于电阻加热套中,将加热套内温度升高至70~80℃,恒温调节下用搅拌器以600~700r/min的转速搅拌30~40min,搅拌后将三口烧瓶内物料投入旋转蒸发仪中,在温度为60~80℃的条件下浓缩蒸发至产物质量恒重制得浓缩反应产物;
(3)将浓缩反应产物投入高温炉中,将高温炉内温度身高至120~130℃,恒温预热50~60min制得,预热后向高温炉内充满氩气,将高温炉内温度升高至400~450℃,恒温静置60~80min,再次高温炉内温度升高,高温下反应3~4h制得热炭化纤维;
所述的改性浆液的具体制备步骤为:
(1)将甘蔗渣与水稻秸秆投入烘箱中,在温度为80~100℃的条件下干燥60~80min,干燥后投入粉碎机中粉碎得到混合物,将混合物与质量分数为8~10%的盐酸投入烧杯中,用搅拌器以300~350r/min的转速混合搅拌2~3h,搅拌后过滤得到滤渣,用蒸馏水清洗滤渣3~5次制得有机混合物;
(2)将有机混合物与质量分数为3~5%的氢氧化钠溶液投入反应釜中,密闭反应釜,将反应釜内温度升高至90~100℃,恒温下用搅拌器以200~240r/min的转速搅拌40~60min制得反应浆液,向反应釜中加入铝粉,继续搅拌30~40min制得改性浆液。
优选的按重量份数计,所述的热炭化纤维为8~10份、滑石为35~38份、黏土为16~20份、长石为9~12份、氯化钙粉末为2~4份。
热炭化纤维的具体制备步骤(1)中所述的向烧杯中加入的质量分数为10~15%的柠檬酸溶液的质量为反应混合液质量的20~25%。
热炭化纤维的具体制备步骤(2)中所述的向三口烧瓶中加入的高锰酸钾粉末的质量为酸性反应液质量的1.0~1.5%。
热炭化纤维的具体制备步骤(3)中所述的高温炉内高温下反应的温度为600~650℃。
改性浆液的具体制备步骤(1)中所述的甘蔗渣与水稻秸秆按质量比为5:1。
改性浆液的具体制备步骤(1)中所述的混合物与质量分数为8~10%的盐酸的质量比为1:10。
改性浆液的具体制备步骤(2)中所述的有机混合物与质量分数为3~5%的氢氧化钠溶液的质量比为1:10。
改性浆液的具体制备步骤(2)中所述的向反应釜中加入的铝粉的质量为反应浆液质量的2~4%。
本发明的有益技术效果是:
(1)本发明首先将甘蔗渣与水稻秸秆混合烘干,烘干后粉碎与盐酸混合,混合后过滤洗涤得到有机混合物,随后将有机混合物与氢氧化钠溶液混合,高温搅拌,搅拌后加入铝粉混合反应制得改性浆液,然后向改性浆液中加入柠檬酸溶液反应,反应后加入高锰酸钾反应,反应后浓缩蒸发制得浓缩反应产物,随后将浓缩反应产物进行高温处理制得热炭化纤维,最后将热炭化纤维与长石、滑石以及其它物料混合研磨,压制成型、高温焙烧制得耐高温高强度耐热瓷,本发明将甘蔗渣与稻草混合,经过热碱液浸泡使甘蔗渣与稻草中的纤维成分分离,提取出甘蔗渣中的蔗糖、有机纤维、纤维素等成分,再经过氧化反应以及柠檬酸溶液浸泡,使有机纤维分子上生成、黏附较多的羧基基团,利用离子键、氢键等键能加强纤维成分对耐热瓷中各成分之间的粘结吸附能力,纤维成分以及蔗糖成分在高温条件下形成炭化反应,在炭化过程中会与周围成分之间形成共价键黏附作用,从而提高耐热瓷中各成分之间的粘结作用,使耐热瓷中的微观结构成分增强,提高耐热瓷整体的力学强度,炭化分子对耐热瓷中各成分进行保护作用,增强耐热瓷在高温条件下耐冲击性能,减小脆性;
(2)本发明利用将铝粉投入碱液中反应,随后在酸性液体中形成铝离子经过羧基络合反应使铝离子吸附于纤维之上,经过高温反应在炭化纤维中生成氧化铝纳米颗粒,氧化铝分子分散于炭化纤维中,经过碳纤维与耐热瓷中各成分之间的吸附粘结作用分散于耐热瓷中,包覆耐热瓷中部分成分,同时提高碳纤维的力学强度和机械性能,使耐热瓷的结构强度进一步加强,同时氧化铝颗粒具有良好的热稳定性,使耐热瓷的热稳定性能增强,加强耐热瓷在高温下结构强度难以下降,具有广阔的应用前景。
具体实施方式
将甘蔗渣与水稻秸秆按质量比为5:1投入烘箱中,在温度为80~100℃的条件下干燥60~80min,干燥后投入粉碎机中粉碎得到混合物,将混合物与质量分数为8~10%的盐酸按质量比为1:10投入烧杯中,用搅拌器以300~350r/min的转速混合搅拌2~3h,搅拌后过滤得到滤渣,用蒸馏水清洗滤渣3~5次制得有机混合物;将上述有机混合物与质量分数为3~5%的氢氧化钠溶液按质量比为1:10投入反应釜中,密闭反应釜,将反应釜内温度升高至90~100℃,恒温下用搅拌器以200~240r/min的转速搅拌40~60min制得反应浆液,向反应釜中加入反应浆液质量2~4%的铝粉,继续搅拌30~40min制得改性浆液;将上述改性浆液倒入三口烧瓶中,将三口烧瓶置于水浴温度为30~40℃的水浴锅中,用搅拌器以500~600r/min的转速搅拌60~80min制得反应混合液,向烧杯中加入反应混合液质量20~25%的质量分数为10~15%的柠檬酸溶液,用搅拌器以300~360r/min的转速搅拌30~40min制得酸性反应液;向上述三口烧瓶中加入酸性反应液质量1.0~1.5%的高锰酸钾粉末,将三口烧瓶置于电阻加热套中,将加热套内温度升高至70~80℃,恒温调节下用搅拌器以600~700r/min的转速搅拌30~40min,搅拌后将三口烧瓶内物料投入旋转蒸发仪中,在温度为60~80℃的条件下浓缩蒸发至产物质量恒重制得浓缩反应产物;将上述浓缩反应产物投入高温炉中,将高温炉内温度身高至120~130℃,恒温预热50~60min制得,预热后向高温炉内充满氩气,将高温炉内温度升高至400~450℃,恒温静置60~80min,再次高温炉内温度升高至600~650℃,高温下反应3~4h制得热炭化纤维;按重量份数计,将8~10份上述热炭化纤维、35~38份滑石、16~20份黏土、9~12份长石、2~4份氯化钙粉末投入行星球磨机中,在转速为100~120r/min和球料比为10:1的条件下研磨60~80min得到预制混料,将预制混料进行压制成型,投入窑炉中,在温度为1100~1200℃的条件下焙烧80~100min,冷却后即得耐高温高强度耐热瓷。
实施例1
热炭化纤维的制备:
将上述改性浆液倒入三口烧瓶中,将三口烧瓶置于水浴温度为30℃的水浴锅中,用搅拌器以500r/min的转速搅拌60min制得反应混合液,向烧杯中加入反应混合液质量20%的质量分数为10%的柠檬酸溶液,用搅拌器以300r/min的转速搅拌30min制得酸性反应液;
向上述三口烧瓶中加入酸性反应液质量1.0%的高锰酸钾粉末,将三口烧瓶置于电阻加热套中,将加热套内温度升高至70℃,恒温调节下用搅拌器以600r/min的转速搅拌30min,搅拌后将三口烧瓶内物料投入旋转蒸发仪中,在温度为60℃的条件下浓缩蒸发至产物质量恒重制得浓缩反应产物;
将上述浓缩反应产物投入高温炉中,将高温炉内温度身高至120℃,恒温预热50min制得,预热后向高温炉内充满氩气,将高温炉内温度升高至400℃,恒温静置60min,再次高温炉内温度升高至600℃,高温下反应3h制得热炭化纤维;改性浆液的制备:
将甘蔗渣与水稻秸秆按质量比为5:1投入烘箱中,在温度为80~100℃的条件下干燥60min,干燥后投入粉碎机中粉碎得到混合物,将混合物与质量分数为8%的盐酸按质量比为1:10投入烧杯中,用搅拌器以300r/min的转速混合搅拌2h,搅拌后过滤得到滤渣,用蒸馏水清洗滤渣3次制得有机混合物;
将上述有机混合物与质量分数为3%的氢氧化钠溶液按质量比为1:10投入反应釜中,密闭反应釜,将反应釜内温度升高至90℃,恒温下用搅拌器以200r/min的转速搅拌40min制得反应浆液,向反应釜中加入反应浆液质量2%的铝粉,继续搅拌30min制得改性浆液;
耐高温高强度耐热瓷的制备:
按重量份数计,将8份上述热炭化纤维、35份滑石、16份黏土、9份长石、2份氯化钙粉末投入行星球磨机中,在转速为100r/min和球料比为10:1的条件下研磨60min得到预制混料,将预制混料进行压制成型,投入窑炉中,在温度为1100℃的条件下焙烧80min,冷却后即得耐高温高强度耐热瓷。
实施例2
热炭化纤维的制备:
将上述改性浆液倒入三口烧瓶中,将三口烧瓶置于水浴温度为35℃的水浴锅中,用搅拌器以550r/min的转速搅拌70min制得反应混合液,向烧杯中加入反应混合液质量22%的质量分数为12%的柠檬酸溶液,用搅拌器以330r/min的转速搅拌35min制得酸性反应液;
向上述三口烧瓶中加入酸性反应液质量1.2%的高锰酸钾粉末,将三口烧瓶置于电阻加热套中,将加热套内温度升高至75℃,恒温调节下用搅拌器以650r/min的转速搅拌35min,搅拌后将三口烧瓶内物料投入旋转蒸发仪中,在温度为70℃的条件下浓缩蒸发至产物质量恒重制得浓缩反应产物;
将上述浓缩反应产物投入高温炉中,将高温炉内温度身高至125℃,恒温预热55min制得,预热后向高温炉内充满氩气,将高温炉内温度升高至420℃,恒温静置70min,再次高温炉内温度升高至620℃,高温下反应3h制得热炭化纤维;改性浆液的制备:
将甘蔗渣与水稻秸秆按质量比为5:1投入烘箱中,在温度为90℃的条件下干燥70min,干燥后投入粉碎机中粉碎得到混合物,将混合物与质量分数为9%的盐酸按质量比为1:10投入烧杯中,用搅拌器以320r/min的转速混合搅拌2h,搅拌后过滤得到滤渣,用蒸馏水清洗滤渣4次制得有机混合物;
将上述有机混合物与质量分数为4%的氢氧化钠溶液按质量比为1:10投入反应釜中,密闭反应釜,将反应釜内温度升高至95℃,恒温下用搅拌器以220r/min的转速搅拌50min制得反应浆液,向反应釜中加入反应浆液质量3%的铝粉,继续搅拌35min制得改性浆液;
耐高温高强度耐热瓷的制备:
按重量份数计,将9份上述热炭化纤维、36份滑石、18份黏土、10份长石、3份氯化钙粉末投入行星球磨机中,在转速为110r/min和球料比为10:1的条件下研磨70min得到预制混料,将预制混料进行压制成型,投入窑炉中,在温度为1150℃的条件下焙烧90min,冷却后即得耐高温高强度耐热瓷。
实施例3
热炭化纤维的制备:
将上述改性浆液倒入三口烧瓶中,将三口烧瓶置于水浴温度为40℃的水浴锅中,用搅拌器以600r/min的转速搅拌80min制得反应混合液,向烧杯中加入反应混合液质量25%的质量分数为15%的柠檬酸溶液,用搅拌器以360r/min的转速搅拌40min制得酸性反应液;
向上述三口烧瓶中加入酸性反应液质量1.5%的高锰酸钾粉末,将三口烧瓶置于电阻加热套中,将加热套内温度升高至80℃,恒温调节下用搅拌器以700r/min的转速搅拌40min,搅拌后将三口烧瓶内物料投入旋转蒸发仪中,在温度为80℃的条件下浓缩蒸发至产物质量恒重制得浓缩反应产物;
将上述浓缩反应产物投入高温炉中,将高温炉内温度身高至130℃,恒温预热60min制得,预热后向高温炉内充满氩气,将高温炉内温度升高至450℃,恒温静置80min,再次高温炉内温度升高至650℃,高温下反应4h制得热炭化纤维;改性浆液的制备:
将甘蔗渣与水稻秸秆按质量比为5:1投入烘箱中,在温度为100℃的条件下干燥80min,干燥后投入粉碎机中粉碎得到混合物,将混合物与质量分数为10%的盐酸按质量比为1:10投入烧杯中,用搅拌器以350r/min的转速混合搅拌3h,搅拌后过滤得到滤渣,用蒸馏水清洗滤渣5次制得有机混合物;
将上述有机混合物与质量分数为5%的氢氧化钠溶液按质量比为1:10投入反应釜中,密闭反应釜,将反应釜内温度升高至100℃,恒温下用搅拌器以240r/min的转速搅拌60min制得反应浆液,向反应釜中加入反应浆液质量4%的铝粉,继续搅拌40min制得改性浆液;
耐高温高强度耐热瓷的制备:
按重量份数计,将10份上述热炭化纤维、38份滑石、20份黏土、12份长石、4份氯化钙粉末投入行星球磨机中,在转速为120r/min和球料比为10:1的条件下研磨80得到预制混料,将预制混料进行压制成型,投入窑炉中,在温度为1200℃的条件下焙烧100min,冷却后即得耐高温高强度耐热瓷。
对比例1:与实施例2的制备方法基本相同,唯有不同的是缺少热炭化纤维。
对比例2:与实施例2的制备方法基本相同,唯有不同的是缺少改性浆液。
对比例3:浙江某公司生产的耐热瓷。
水平剪切强度测试采用陶瓷剪切强度试验机进行检测。
静曲强度测试采用静曲强度试验机进行检测。
破坏强度测试按GB/T 23453-2009进行检测。
耐高温测试:将各实例与对比例置于温度为800℃的高温炉内静置2~3h,静置后称取质量与放入高温炉之前的质量进行相除得到比例,比例越高说明耐热性能越好。
表1:建筑材料性能测定结果
综合上述,从表1可以看出本发明的耐热瓷的水平剪切强度、静曲强度良好具有良好的力学性能和机械强度,具有广阔应用前景。
以上所述仅为本发明的较佳方式,并不用以限制本发明,凡在本发明的精神和原则之内,所作的任何修改、等同替换、改进等,均应包含在本发明的保护范围之内。
Claims (9)
1.一种耐高温高强度耐热瓷的制备方法,其特征在于具体制备步骤为:
将热炭化纤维、滑石、黏土、长石、氯化钙粉末投入行星球磨机中,在转速为100~120r/min和球料比为10:1的条件下研磨60~80min得到预制混料,将预制混料进行压制成型,投入窑炉中,在温度为1100~1200℃的条件下焙烧80~100min,冷却后即得耐高温高强度耐热瓷。
所述的热炭化纤维的具体制备步骤为:
(1)将改性浆液倒入三口烧瓶中,将三口烧瓶置于水浴温度为30~40℃的水浴锅中,用搅拌器以500~600r/min的转速搅拌60~80min制得反应混合液,向烧杯中加入质量分数为10~15%的柠檬酸溶液,用搅拌器以300~360r/min的转速搅拌30~40min制得酸性反应液;
(2)向三口烧瓶中加入高锰酸钾粉末,将三口烧瓶置于电阻加热套中,将加热套内温度升高至70~80℃,恒温调节下用搅拌器以600~700r/min的转速搅拌30~40min,搅拌后将三口烧瓶内物料投入旋转蒸发仪中,在温度为60~80℃的条件下浓缩蒸发至产物质量恒重制得浓缩反应产物;
(3)将浓缩反应产物投入高温炉中,将高温炉内温度身高至120~130℃,恒温预热50~60min制得,预热后向高温炉内充满氩气,将高温炉内温度升高至400~450℃,恒温静置60~80min,再次高温炉内温度升高,高温下反应3~4h制得热炭化纤维;
所述的改性浆液的具体制备步骤为:
(1)将甘蔗渣与水稻秸秆投入烘箱中,在温度为80~100℃的条件下干燥60~80min,干燥后投入粉碎机中粉碎得到混合物,将混合物与质量分数为8~10%的盐酸投入烧杯中,用搅拌器以300~350r/min的转速混合搅拌2~3h,搅拌后过滤得到滤渣,用蒸馏水清洗滤渣3~5次制得有机混合物;
(2)将有机混合物与质量分数为3~5%的氢氧化钠溶液投入反应釜中,密闭反应釜,将反应釜内温度升高至90~100℃,恒温下用搅拌器以200~240r/min的转速搅拌40~60min制得反应浆液,向反应釜中加入铝粉,继续搅拌30~40min制得改性浆液。
2.根据权利要求1所述的一种耐高温高强度耐热瓷的制备方法,其特征在于:优选的按重量份数计,所述的热炭化纤维为8~10份、滑石为35~38份、黏土为16~20份、长石为9~12份、氯化钙粉末为2~4份。
3.根据权利要求1所述的一种耐高温高强度耐热瓷的制备方法,其特征在于:热炭化纤维的具体制备步骤(1)中所述的向烧杯中加入的质量分数为10~15%的柠檬酸溶液的质量为反应混合液质量的20~25%。
4.根据权利要求1所述的一种耐高温高强度耐热瓷的制备方法,其特征在于:热炭化纤维的具体制备步骤(2)中所述的向三口烧瓶中加入的高锰酸钾粉末的质量为酸性反应液质量的1.0~1.5%。
5.根据权利要求1所述的一种耐高温高强度耐热瓷的制备方法,其特征在于:热炭化纤维的具体制备步骤(3)中所述的高温炉内高温下反应的温度为600~650℃。
6.根据权利要求1所述的一种耐高温高强度耐热瓷的制备方法,其特征在于:改性浆液的具体制备步骤(1)中所述的甘蔗渣与水稻秸秆按质量比为5:1。
7.根据权利要求1所述的一种耐高温高强度耐热瓷的制备方法,其特征在于:改性浆液的具体制备步骤(1)中所述的混合物与质量分数为8~10%的盐酸的质量比为1:10。
8.根据权利要求1所述的一种耐高温高强度耐热瓷的制备方法,其特征在于:改性浆液的具体制备步骤(2)中所述的有机混合物与质量分数为3~5%的氢氧化钠溶液的质量比为1:10。
9.根据权利要求1所述的一种耐高温高强度耐热瓷的制备方法,其特征在于:改性浆液的具体制备步骤(2)中所述的向反应釜中加入的铝粉的质量为反应浆液质量的2~4%。
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CN110684341A (zh) * | 2019-10-10 | 2020-01-14 | 马贵其 | 一种抗冲击型保温板的制备方法 |
CN113683899A (zh) * | 2021-09-02 | 2021-11-23 | 程小冬 | 一种高强度高粘性沥青及其制备方法 |
CN115893985A (zh) * | 2022-12-19 | 2023-04-04 | 齐鲁工业大学 | 一种基于黄河泥的轻质耐高温、适用于陶瓷绘画的陶瓷材料及制备方法 |
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CN110684341A (zh) * | 2019-10-10 | 2020-01-14 | 马贵其 | 一种抗冲击型保温板的制备方法 |
CN113683899A (zh) * | 2021-09-02 | 2021-11-23 | 程小冬 | 一种高强度高粘性沥青及其制备方法 |
CN115893985A (zh) * | 2022-12-19 | 2023-04-04 | 齐鲁工业大学 | 一种基于黄河泥的轻质耐高温、适用于陶瓷绘画的陶瓷材料及制备方法 |
CN115893985B (zh) * | 2022-12-19 | 2024-01-23 | 齐鲁工业大学 | 一种基于黄河泥的轻质耐高温、适用于陶瓷绘画的陶瓷材料及制备方法 |
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