CN106040166B - 高效脱吸附的空分分子筛的制备方法 - Google Patents

高效脱吸附的空分分子筛的制备方法 Download PDF

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CN106040166B
CN106040166B CN201610457430.5A CN201610457430A CN106040166B CN 106040166 B CN106040166 B CN 106040166B CN 201610457430 A CN201610457430 A CN 201610457430A CN 106040166 B CN106040166 B CN 106040166B
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易中发
黄德金
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JIANGXI CHEMPACK ENVIRONMENTAL PROTECTION CHEMICAL Co Ltd
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Abstract

本发明公开了一种高效脱吸附的空分分子筛的制备方法，包括以下具体步骤：1）分子筛原粉浸出2）将步骤1）制备的分子筛原粉于160‑180℃下进行除湿处理后，与改性原料粉、助剂混匀，再研磨造粒得到分子筛坯体；3）将分子筛坯体在氮气保护下焙烧制得高效脱吸附的空分分子筛；本发明脱吸附性能佳，能够满足现代化空分领域的要求。

Description

高效脱吸附的空分分子筛的制备方法
技术领域
本发明涉及分子筛技术领域，具体讲是一种高效脱吸附的空分分子筛的制备方法。
背景技术
在高效吸附分离、净化环保的现代化空分领域，越来越重视分子筛的应用效果。空分专用分子筛的吸附孔道以X型人工合成沸石粉体作主要原料，所合成的分子筛是根据硅铝的比例不同来确立分子筛的脱吸附能量。
现行用于空分领域的分子筛，都是采用国内生产的13X原粉为原料，一般分子筛的原粉指标为：静态水吸附32.5%，CO2吸附量23%，PH值9-11，堆积密度0.65g/ml。针对现行13X原粉生产出来的分子筛，静态水吸附最高只有27%左右，CO2吸附量18%左右（25℃），堆积密度0.64g/ml左右，这种脱吸附的技术指标很难满足现代化空分领域的技术要求。
发明内容
本发明所要解决的技术问题是，克服以上现有技术的缺点：提供一种脱吸附性能佳的高效脱吸附的空分分子筛的制备方法。
本发明的技术解决方案如下：一种高效脱吸附的空分分子筛的制备方法，包括以下具体步骤：
1）分子筛原粉浸出：将沸石粉加入碱性溶液中，经150-160℃，160-200min的水热晶化，浸出得到分子筛原粉；
2）将步骤1）制备的分子筛原粉于160-180℃下进行除湿处理后，与改性原料粉、助剂混合均匀，再研磨至325目以上后进行造粒或挤条成型得到分子筛坯体；
3）将步骤2）制备的分子筛坯体干燥后置于回转炉中在氮气保护下焙烧80-90min制得高效脱吸附的空分分子筛，其中，回转炉进口温度为500-580℃，中间温度为700-720℃，出口温度为500-565℃。
作为优选，所述步骤2）中各原料组分的重量百分比为：分子筛原粉30-40%；改性原料粉30-40%；助剂20-30%。
作为优选，所述改性原料粉为高岭土、凹凸棒土、洋坩土中的一种或多种。
作为优选，所述助剂为杨梅栲胶、SG植物胶、羧甲基纤维素钠、无水焦磷酸钠中的一种或多种。
作为优选，所述沸石粉为人工合成的沸石粉。
作为优选，所述碱性溶液是质量百分比浓度为35-45%的碳酸钠溶液或硅酸钠溶液或碳酸氢钠溶液。
作为优选，所述除湿处理为按重量百分比计烘干至含水量20%以下。
本发明的有益效果是：本发明制备的分子筛原粉的静态水吸附量达35.5%，CO2吸附量达25.2%，PH值8-10，堆积密度0.67g/ml，采用该原粉制备的高效脱吸附的空分分子筛指标为：静态水吸附29.3%，CO2吸附量（25℃）19.5%，堆积密度0.66g/ml，该指标完全能够满足现代化空分领域的要求。
具体实施方式
下面用具体实施例对本发明做进一步详细说明，但本发明不仅局限于以下具体实施例。
实施例一
按照以下具体步骤制备高效脱吸附的空分分子筛：
1）分子筛原粉浸出：将人工合成的沸石粉加入质量百分比浓度为35-45%的碳酸钠溶液中，经150℃， 200min的水热晶化，浸出得到分子筛原粉；
2）将步骤1）制备的分子筛原粉于180℃下烘干至含水量按重量百分比计20%以下后，与高岭土、凹凸棒土、洋坩、杨梅栲胶混合均匀，再研磨至325目以上后进行造粒或挤条成型得到分子筛坯体；其中各原料组分的重量百分比为：分子筛原粉40kg；高岭土10kg；凹凸棒土10kg；洋坩10kg；杨梅栲胶30kg。
3）将步骤2）制备的分子筛坯体干燥后置于回转炉中在氮气保护下焙烧80-90min制得高效脱吸附的空分分子筛，其中，回转炉进口温度为500-580℃，中间温度为700-720℃，出口温度为500-565℃。
实施例二
按照以下具体步骤制备高效脱吸附的空分分子筛：
1）分子筛原粉浸出：将沸石粉加入质量百分比浓度为35%的硅酸钠溶液中，经150℃， 200min的水热晶化，浸出得到分子筛原粉；
2）将步骤1）制备的分子筛原粉于160℃下烘干至含水量按重量百分比计18%后，与高岭土、凹凸棒土、杨梅栲胶、羧甲基纤维素钠混合均匀，再研磨至325目以上后进行造粒或挤条成型得到分子筛坯体；其中各原料组分的重量百分比为：分子筛原粉40kg；高岭土10kg；凹凸棒土20kg；杨梅栲胶20kg；羧甲基纤维素钠10kg。
3）将步骤2）制备的分子筛坯体干燥后置于回转炉中在氮气保护下焙烧90min制得高效脱吸附的空分分子筛，其中，回转炉进口温度为580℃，中间温度为720℃，出口温度为565℃。
实施例三
按照以下具体步骤制备高效脱吸附的空分分子筛：
1）分子筛原粉浸出：将沸石粉加入质量百分比浓度为45%的碳酸氢钠溶液中，经160℃，160min的水热晶化，浸出得到分子筛原粉；
2）将步骤1）制备的分子筛原粉于160℃下烘干至含水量按重量百分比计20%以下后，与凹凸棒土、杨梅栲胶混合均匀，再研磨至325目以上后进行造粒或挤条成型得到分子筛坯体；其中各原料组分的重量百分比为：分子筛原粉40kg；凹凸棒土30kg；杨梅栲胶30kg。
3）将步骤2）制备的分子筛坯体干燥后置于回转炉中在氮气保护下焙烧90min制得高效脱吸附的空分分子筛，其中，回转炉进口温度为500℃，中间温度为700℃，出口温度为500℃。
本实施例制备的分子筛与传统的对比
以上仅是本发明的特征实施范例，对本发明保护范围不构成任何限制。凡采用同等交换或者等效替换而形成的技术方案，均落在本发明权利保护范围之内。

Claims (5)

1.一种高效脱吸附的空分分子筛的制备方法，其特征在于：包括以下具体步骤：
1)分子筛原粉浸出：将沸石粉加入碱性溶液中，经150-160℃，160-200min的水热晶化，浸出得到分子筛原粉；
2)将步骤1)制备的分子筛原粉于160-180℃下进行除湿处理后，与改性原料粉、助剂混合均匀，再研磨至325目以上后进行造粒或挤条成型得到分子筛坯体；
3)将步骤2)制备的分子筛坯体干燥后置于回转炉中在氮气保护下焙烧80-90min制得高效脱吸附的空分分子筛，其中，回转炉进口温度为500-580℃，中间温度为700-720℃，出口温度为500-565℃；
所述步骤2)中各原料组分的重量百分比为：分子筛原粉30-40％；改性原料粉30-40％；助剂20-30％；
所述改性原料粉为高岭土、凹凸棒土、洋坩土中的一种或多种。
2.根据权利要求1所述的高效脱吸附的空分分子筛的制备方法，其特征在于：所述助剂为杨梅栲胶、SG植物胶、羧甲基纤维素钠、无水焦磷酸钠中的一种或多种。
3.根据权利要求1所述的高效脱吸附的空分分子筛的制备方法，其特征在于：所述沸石粉为人工合成的沸石粉。
4.根据权利要求1所述的高效脱吸附的空分分子筛的制备方法，其特征在于：所述碱性溶液是质量百分比浓度为35-45％的碳酸钠溶液或硅酸钠溶液或碳酸氢钠溶液。
5.根据权利要求1所述的高效脱吸附的空分分子筛的制备方法，其特征在于：所述除湿处理为按重量百分比计烘干至含水量20％以下。
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