CN114804868B - 一种三氧化钨陶瓷骨架坩埚的制备方法 - Google Patents

一种三氧化钨陶瓷骨架坩埚的制备方法 Download PDF

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CN114804868B
CN114804868B CN202210464558.XA CN202210464558A CN114804868B CN 114804868 B CN114804868 B CN 114804868B CN 202210464558 A CN202210464558 A CN 202210464558A CN 114804868 B CN114804868 B CN 114804868B
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闫晗
陈喜庆
李宏岩
周彤
杨红
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Changchun Thermal Power Branch Of Jilin Electric Power Co ltd
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Abstract

本发明涉及陶瓷坩埚技术领域，具体地涉及一种三氧化钨陶瓷骨架坩埚的制备方法及其该坩埚的应用。包括以下步骤：1)将三氧化钨粉末加入糊精溶液，搅拌，得到三氧化钨粘土；2)将三氧化钨粘土包裹在陶瓷支架上，制成三氧化钨坩埚坯料；3)将三氧化钨坩埚坯料压制，压制后坯料放置在烧制炉内烧制，冷却，打磨后得到三氧化钨陶瓷骨架坩埚。本发明三氧化钨作为催化剂加快了煤样硫的生成，而本身质量和化学性质没有发生变化可反复使用。使用三氧化钨制作的坩埚免去了三氧化钨粉末添加，实现了催化剂的重复使用。减少了化验工序，同时避免了催化剂对人体的损害。

Description

一种三氧化钨陶瓷骨架坩埚的制备方法
技术领域
本发明涉及陶瓷坩埚技术领域，具体地涉及一种三氧化钨陶瓷骨架坩埚的制备方法及其该坩埚的应用。
背景技术
随着国家对环保排放管控的增强，燃料结算中对化石燃料中含硫量更加重视。库仑测硫仪因具有准确度高、设备稳定度高、造价低、维护成本低、实验快速等优点，在测硫市场上得到广泛应用。
陶瓷具有良好的导热性、机械强度、耐高温性、耐腐蚀性，应用越来越广泛，可用于制作高温坩埚、耐火炉管及耐腐蚀、耐磨部件，按照国标方法GB/T212-2008中4.4.3.4，全硫测定实验前需将煤样放入陶瓷坩埚中进行称量，在煤样上撒入三氧化钨(HG 10-1129)粉末作为催化剂，实验结束后需用毛刷对煤样燃烧产生的煤灰及三氧化钨粉末进行清理，而长期大量使用的三氧化钨粉末在试验结束后清理过程中会以漂浮物形态漂浮在空中并被人员吸入体内。但是，三氧化钨为低毒物质，对眼睛、皮肤有刺激性，吸入可能出现全身无力、发热、麻疹样皮疹、蛋白尿等现象。因此，亟待一种可以降低吸入三氧化钨的坩埚。
发明内容
本发明的目的在于克服上述问题，提供一种三氧化钨陶瓷骨架坩埚的制备方法及其应用。由该方法制备出的应用于煤样库仑测硫法(GB/T212-2008)的免催化剂、防静电坩埚舟。具体而言，涉及一种通过陶瓷骨架加固的三氧化钨容器的烧制方法以及由该方法获得的免催化剂、防静电坩埚舟；即，一种舟状三氧化钨制容器/库仑硫免催化剂防静电瓷舟的制备方法。
为达到上述目的，本发明提供一种三氧化钨陶瓷骨架坩埚的制备方法，包括以下步骤：
1)将三氧化钨粉末加入糊精溶液，搅拌，得到三氧化钨粘土；
2)将三氧化钨粘土包裹在陶瓷支架上，制成三氧化钨坩埚坯料；
3)将三氧化钨坩埚坯料压制，压制后坯料放置在烧制炉内烧制，烧制后需暴露在空气中快速冷却，打磨后得到三氧化钨陶瓷骨架坩埚。
作为优选，所述步骤1)中三氧化钨粉和糊精溶液的加入比例为1-7％，其中，糊精溶液的浓度为90-110g/L。
作为优选，所述步骤2)中的陶瓷支架为陶瓷鱼骨状支架。
作为优选，所述步骤3)中在弱氧化性气氛中升温烧制，900℃内温升16-19℃/min，900℃后温升3-7℃/min，极限温度1200℃，烧制温度为1100-1200，烧制时间为5-20min。
作为优选，所述弱氧化性气氛的氧含量为10％-30％，所述弱氧化性气氛可以为通入空气。
作为优选，所述三氧化钨陶瓷骨架坩埚的底部增加条纹状突起。
作为优选，所述制备方法制得的三氧化钨陶瓷骨架坩埚在煤样库仑测硫法中作为免催化剂防静电瓷舟的应用。
与现有技术相比，本发明的优势在于：
1)静电对煤化验带来非常大的影响，而目前陶瓷材料坩埚为电不良导体。本发明三氧化钨作为电的良导体-金属氧化物通过金属基座接地，可将静电导出防止静电干扰。
2)本发明三氧化钨包裹在鱼骨状陶瓷架上，解决三氧化钨容器强度不足的问题。
3)本发明三氧化钨作为催化剂加快了煤样硫的生成，而本身质量和化学性质没有发生变化可反复使用。使用三氧化钨制作的坩埚免去了三氧化钨粉末添加，实现了催化剂的重复使用。减少了化验工序，同时避免了催化剂对人体的损害。
4)本发明在坩埚底部增加条状突起增加了催化剂与煤样的接触面积。
具体实施方式
下面结合具体实施例对本发明作进一步说明。
实施例1
一种三氧化钨陶瓷骨架坩埚的制备方法，包括以下步骤：
1)取三氧化钨粉末置于玛瑙研磨钵内研磨；
2)将研磨后的三氧化钨粉末加入适量100g/L的糊精溶液，并搅拌。使三氧化钨变成粘土状；三氧化钨粉和糊精溶液的加入比例为5％；
3)将三氧化钨粘土包裹在陶瓷鱼骨状支架上，制成坩埚坯料。
4)将三氧化钨配料放置在模具内，挤压模具使三氧化钨粘土紧实，并排除气泡。
5)将压制后坯料放置在烧制炉内烧制：弱氧化性气氛，氧含量为15％，900℃内温升17.5℃/min，900℃后5℃/min。极限温度烧制温度1200℃，烧制时间为10min。烧制后需暴露在空气中快速冷却；冷却后坩埚简单打磨即可使用。
实施例2
一种三氧化钨陶瓷骨架坩埚的制备方法，包括以下步骤：
1)取三氧化钨粉末置于玛瑙研磨钵内研磨；
2)将研磨后的三氧化钨粉末加入适量95g/L的糊精溶液，并搅拌。使三氧化钨变成粘土状；三氧化钨粉和糊精溶液的加入比例为7％；
3)将三氧化钨粘土包裹在陶瓷鱼骨状支架上，制成坩埚坯料。
4)将三氧化钨配料放置在模具内，挤压模具使三氧化钨粘土紧实，并排除气泡。
5)将压制后坯料放置在烧制炉内烧制：弱氧化性气氛，氧含量为20％，900℃内温升16.5℃/min，900℃后7℃/min。极限温度烧制温度1200℃，烧制时间为15min。烧制后需暴露在空气中快速冷却；冷却后坩埚简单打磨即可使用。
实施例3
一种三氧化钨陶瓷骨架坩埚的制备方法，包括以下步骤：
1)取三氧化钨粉末置于玛瑙研磨钵内研磨；
2)将研磨后的三氧化钨粉末加入适量105g/L的糊精溶液，并搅拌。使三氧化钨变成粘土状；三氧化钨粉和糊精溶液的加入比例为4％；
3)将三氧化钨粘土包裹在陶瓷鱼骨状支架上，制成坩埚坯料。
4)将三氧化钨配料放置在模具内，挤压模具使三氧化钨粘土紧实，并排除气泡。
5)将压制后坯料放置在烧制炉内烧制：弱氧化性气氛，即通入空气，900℃内温升18.5℃/min，900℃后4℃/min。极限温度烧制温度1200℃，烧制时间为8min。烧制后需暴露在空气中快速冷却；冷却后坩埚简单打磨即可使用。
实施例4
一种三氧化钨陶瓷骨架坩埚的制备方法，包括以下步骤：
1)取三氧化钨粉末置于玛瑙研磨钵内研磨；
2)将研磨后的三氧化钨粉末加入适量110g/L的糊精溶液，并搅拌。使三氧化钨变成粘土状；三氧化钨粉和糊精溶液的加入比例为6％；
3)将三氧化钨粘土包裹在陶瓷鱼骨状支架上，制成坩埚坯料。
4)将三氧化钨配料放置在模具内，挤压模具使三氧化钨粘土紧实，并排除气泡。
5)将压制后坯料放置在烧制炉内烧制：弱氧化性气氛，氧含量为28％，900℃内温升19℃/min，900℃后7℃/min。极限温度烧制温度1200℃，烧制时间为18min。烧制后需暴露在空气中快速冷却；冷却后坩埚简单打磨即可使用。
催化剂理想状态下在反应前后不会发生质量和化学变化，但实际长期使用过程中会逐渐发生性质改变，长期使用导致反应效率降低。配套玛瑙刮板，定期(每季度)或定量(每使用100次)对表面变性三氧化钨进行刮除可延长坩埚使用周期避免浪费。本发明的陶瓷鱼骨骨架加强坩埚强度，并在底部条纹状突起增加煤样接触面积，可以用玛瑙刮板清理坩埚延长坩埚使用周期。另外，在没有静电干扰问题下，可采用相同方法制作三氧化钨条放置于陶瓷坩埚内部重复使用。
本发明未详细说明的内容均可采用本领域的常规技术知识。
最后所应说明的是，以上实施例仅用以说明本发明的技术方案而非限制。尽管参照实施例对本发明进行了详细说明，本领域的普通技术人员应当理解，对本发明的技术方案进行修改或者等同替换，都不脱离本发明技术方案的精神和范围，其均应涵盖在本发明的权利要求范围当中。

Claims (5)

1.一种三氧化钨陶瓷骨架坩埚在煤样库仑测硫法中作为免催化剂防静电瓷舟的应用，其特征在于，所述三氧化钨陶瓷骨架坩埚的制备方法，包括以下步骤：
1）将三氧化钨粉末加入糊精溶液，搅拌，得到三氧化钨粘土；
2）将三氧化钨粘土包裹在陶瓷支架上，制成三氧化钨坩埚坯料；其中，所述陶瓷支架为陶瓷鱼骨状支架；
3）将三氧化钨坩埚坯料压制，压制后坯料放置在烧制炉内烧制，冷却，打磨后得到三氧化钨陶瓷骨架坩埚。
2.根据权利要求1所述应用，其特征在于，所述步骤1）中三氧化钨粉和糊精溶液的加入比例为1-7%，其中，糊精溶液的浓度为90-110g/L。
3.根据权利要求1所述应用，其特征在于，所述步骤3）中在弱氧化性气氛中升温烧制，900℃内温升16-19℃/min，900℃后温升3-7℃/min，极限温度1200℃，烧制温度为1100-1200，烧制时间为5-20min。
4.根据权利要求3所述应用，其特征在于，所述弱氧化性气氛的氧含量为10%-30%。
5.根据权利要求1所述应用，其特征在于，所述三氧化钨陶瓷骨架坩埚的底部增加条纹状突起。
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