CN110218082B - 一种低温烧结mh型刚玉瓷球及其制备方法 - Google Patents

一种低温烧结mh型刚玉瓷球及其制备方法 Download PDF

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CN110218082B
CN110218082B CN201910523400.3A CN201910523400A CN110218082B CN 110218082 B CN110218082 B CN 110218082B CN 201910523400 A CN201910523400 A CN 201910523400A CN 110218082 B CN110218082 B CN 110218082B
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陈彦霖
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Abstract

本发明公开了一种低温烧结MH型刚玉瓷球，它由氧化铝、二氧化硅与碱金属氧化物组成，其中氧化铝质量含量为≥95%，二氧化硅质量含量1~4%，其余组分为碱性金属氧化物，碱性金属氧化物为Na2O、K2O、MgO、CaO与BaO，所述MH型刚玉瓷球按下述制备方法步骤制造而成：将煅烧氧化铝粉、高岭土与碱性金属碳酸盐按比例倒入球磨机；将混合原料在球磨机内，球磨8~36 h，然后进行喷雾干燥，得到混合原料；将步骤2得到的混合原料，投入成球机中，加入粘结剂与核桃粉，机械滚动成球，得到球形颗粒；将所得球体自然晾干，然后再放入烧结炉中进行烧结，冷却后得到MH型刚玉瓷球。本发明不仅表面更粗糙，而且烧结温度低、过滤能力强、表面粗糙、比表面积大。

Description

一种低温烧结MH型刚玉瓷球及其制备方法
技术领域
本发明涉及石油化工及特种陶瓷行业，具体涉及一种低温烧结MH型刚玉瓷球及其制备方法。
背景技术
惰性瓷球广泛应用于石油、化工、化肥、天然气及环保等行业，作为反应器内催化剂的覆盖支撑材料和塔填料，用以增加气体或液体分布点，支撑和保护强度不高的活性催化剂；开孔瓷球是在惰性氧化铝瓷球的基础上进一步改进的瓷球产品，它以球体直径为轴心进行开孔，既具有一定的机械强度、化学稳定性和热稳定性，又增加了比表面积和空隙率，从而增加了物料的分散性和通量，降低了系统的阻力。
MH型惰性瓷球(过滤瓷球)综合了惰性瓷球和开孔瓷球的特点，在惰性瓷球的表面上增加了20-30%具有吸附和拦截作用的结构孔。因而MH型惰性瓷球除具有和惰性瓷球相同的支撑覆盖催化剂和分散汽液的作用外，还同时能过滤油品中的杂质。油品中杂质的形态有颗粒状、胶质状、沥清质及重金属等，这些杂质在经过原料过滤器后虽然可滤掉一部分，但仍有相当部分还是无法滤掉。如在反应器的顶部装填MH型惰性瓷球则可将原料中未过滤掉的杂质通过表面结构孔进行拦截和过滤，从而可保护催化剂，并延长装置的运行周期。
刚玉瓷球为氧化铝含量大于90%的瓷球，由于瓷球内部氧化铝含量高，所以刚玉瓷球具有强度高、耐酸和耐碱性好、耐磨性好等优点；同时也有成本高、成型困难、烧成温度高等特点，特别是氧化铝含量在95%以上的瓷球，其烧结温度可达1600℃。
发明内容
针对上述现有技术存在的问题,本发明提供一种烧结温度低、过滤能力强、表面粗糙、比表面积大且有工艺简单，成本低廉的低温烧结MH型刚玉瓷球及其制备方法。
本发明解决技术问题采取的技术方案是：一种低温烧结MH型刚玉瓷球及其制备方法，所述MH型刚玉瓷球由该MH型由氧化铝、二氧化硅与碱金属氧化物组成，其中氧化铝质量含量为≥95%，二氧化硅质量含量1~4%，其余组分为碱性金属氧化物，所述的碱性金属氧化物为Na2O、K2O、MgO、CaO与BaO，所述的MH型刚玉瓷球按下述制备方法步骤制造而成：
1）将煅烧氧化铝粉、高岭土与碱性金属碳酸盐按比例倒入球磨机；
2）将混合原料在球磨机内，球磨8~36 h，然后进行喷雾干燥，得到混合原料；
3）将步骤2得到的混合原料，投入成球机中，加入粘结剂与核桃粉，机械滚动成球，得到球形颗粒；
4）将所得球体自然晾干，然后再放入烧结炉中进行烧结，冷却后得到MH型刚玉瓷球。
进一步地，所述的MH型刚玉瓷球的堆比3.0~4.0 g/mL，抗压强度≥1500 N/颗，吸水率≤0.5 wt%。
进一步地，所述的碱性金属碳酸盐为碳酸镁、碳酸钙与碳酸钡；所述的粘结剂为田箐胶粉。
进一步地，MH型刚玉瓷球制备步骤中混合原料组成质量比例为：煅烧氧化铝粉85%～95%、高岭土3%～8%，碱性金属碳酸盐2~7%。所述的粘结剂的加入质量占混合原料的，2~8%；所述的核桃粉的加入质量占混合原料的5~25%。
进一步地，烧结温度为1000~1400 ℃，先在600~800 ℃焙烧4~12 h，再升温至1000~1400 ℃焙烧4~12 h。
本发明的原理：一般工业用氧化铝陶瓷，大多采用成本较低，生产量大的拜耳法工业氧化铝粉。这种通过高温煅烧转相而得的ɑ-Al2O3 粉的烧结活性低，因此为了达到致密化和降低烧结温度常引入可形成玻璃液相的助烧剂（如CaO、MgO、SiO2等）。这类陶瓷的氧化铝含量普遍偏高，特别是常用的95氧化铝陶瓷。氧化铝陶瓷液相烧结的常见组成体系为CaO-SiO2-Al2O3体系、MgO-SiO2-Al2O3体系和CaO-MgO-SiO2-Al2O3体系。其中CaO-SiO2-Al2O3体系烧结温度低，但晶粒发育比较大，抗酸腐蚀能力差，且在粗大的晶粒中容易包裹未排出的闭气孔，显微结构不够理想；MgO-SiO2-Al2O3体系可以更好的使得Al2O3晶粒形成等轴结构，二面角接近120°，这样所以的晶界能力相等，均匀化微观结构，减小了各向异性作用，但烧结温度偏高；CaO-MgO-SiO2-Al2O3体系综合了上述两种体系的优点，具有烧结温度较低、晶粒较小、显微结构较致密、抗酸碱腐蚀能力较强等优点，是一种比较理想的配方体系。本次烧结的MH型刚玉瓷球就是采用了CaO-MgO-SiO2-Al2O3体系配方。
本发明与现有技术相比具有的优点主要是：以这种方法所制得的MH型刚玉瓷球相比于现有产品具有烧结温度低、表面粗糙度大、比表面积大和过滤能力强的特点，不仅MH型刚玉瓷球的表面更粗糙，而且烧结温度低、过滤能力强、表面粗糙、比表面积大。且有工艺简单，成本低廉的优点。
具体实施方式
下面对原料中的物质组分进行详细说明 ： 高岭土
组分 SiO<sub>2</sub>，wt% Al<sub>2</sub>O<sub>3</sub>，wt% 碱性金属氧化物 烧失
含量 56.1 41.8 2.1 2.0
下面结合实施例对本发明做进一步详细的说明，但是不会构成对本发明的限制。
实施例 1 ：
1）将2820kg煅烧氧化铝粉、90kg高岭土与90kg碳酸镁、碳酸钙与碳酸钡倒入球磨机；
2）在球磨机内，将混合原料球磨20h，然后在500℃进行喷雾干燥，得到混合原料；
3）将步骤2得到的混合原料，投入成球机中，加入3kg粘结剂与600kg核桃粉，机械滚动成球，得到球形颗粒；
4）将所得球体自然晾干，然后再放入烧结炉中进行烧结，先在600℃焙烧10 h，再升温至1350 ℃焙烧6h，冷却后得到MH型刚玉瓷球。
经测试，MH型刚玉瓷球吸水率为4.84%，体积密度为3.09g/cm3，抗压强度为4575N/颗。
实施例 2 ：
1）将2850kg煅烧氧化铝粉、78kg高岭土与72kg碳酸镁、碳酸钙与碳酸钡倒入球磨机；
2）在球磨机内，将混合原料球磨24h，然后在500℃进行喷雾干燥，得到混合原料；
3）将步骤2得到的混合原料，投入成球机中，加入3kg粘结剂与600kg核桃粉，机械滚动成球，得到球形颗粒；
4）将所得球体自然晾干，然后再放入烧结炉中进行烧结，先在600℃焙烧10h，再升温至1400℃焙烧6h，冷却后得到MH型刚玉瓷球。
经测试，MH型刚玉瓷球吸水率为0.2%，体积密度为3.23g/cm3，抗压强度为5385N/颗。
实施例 3 ：
1）将2850kg煅烧氧化铝粉、60kg高岭土与90kg碳酸镁、碳酸钙与碳酸钡倒入球磨机；
2）在球磨机内，将混合原料球磨36h，然后在500℃进行喷雾干燥，得到混合原料；
3）将步骤2得到的混合原料，投入成球机中，加入3kg粘结剂与600kg核桃粉，机械滚动成球，得到球形颗粒；
4）将所得球体自然晾干，然后再放入烧结炉中进行烧结，先在600 ℃焙烧10 h，再升温至1400 ℃焙烧6 h，冷却后得到MH型刚玉瓷球。
经测试，MH型瓷球吸水率为0.11%，体积密度为3.15g/cm3，抗压强度为5765N/颗。

Claims (2)

1.一种低温烧结MH型刚玉瓷球，其特征在于：所述MH型刚玉瓷球由氧化铝、二氧化硅与碱金属氧化物组成，其中氧化铝质量含量为≥95%，二氧化硅质量含量1~4%，其余组分为碱性金属氧化物，所述的碱性金属氧化物为Na2O、K2O、MgO、CaO与BaO，所述的MH型刚玉瓷球的堆比3.0～4.0 g/mL，强度≥1500 N/颗，吸水率≤0.5 %，所述的低温烧结MH型刚玉瓷球按下述制备步骤制造而成：
1）将煅烧氧化铝粉、高岭土与碱性金属碳酸盐按比例倒入球磨机；
2）将混合原料在球磨机内，球磨8～36 h，然后进行喷雾干燥，得到混合原料；
3）将步骤2）得到的混合原料，投入成球机中，加入粘结剂与核桃粉，机械滚动成球，得到球形颗粒；
4）将所得到的球形颗粒自然晾干，然后再放入烧结炉中进行烧结，冷却后得到低温烧结MH型刚玉瓷球；
所述的碱性金属碳酸盐为碳酸镁、碳酸钙与碳酸钡；所述的粘结剂为田箐胶粉；MH型刚玉瓷球制备步骤中混合原料组成质量比例为：煅烧氧化铝粉85%～95%、高岭土3%～8%，碱性金属碳酸盐2～7%，所述的粘结剂的加入质量占混合原料的2～8%；所述的核桃粉的加入质量占混合原料的5～25%。
2.根据权利要求1所述的一种低温烧结MH型刚玉瓷球，其特征在于：烧结温度为1000～1400℃，先在600～800℃焙烧4～12 h，再升温至1000～1400 ℃焙烧4～12 h。
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