CN106082256A - 乙烯专用分子筛的制备方法 - Google Patents
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Abstract
本发明公开了一种乙烯专用分子筛的制备方法,包括以下具体步骤:1)多维晶体分子筛原粉的制备2)将步骤1)制备的多维晶体分子筛原粉与粘土混合研磨至325目以上得到混合粉,然后将混合粉与粘结剂混合均匀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于焙烧制得乙烯专用分子筛;本发明脱吸附性能佳,吸附稳定、安全高效、操作便捷、使用寿命更长。
Description
技术领域
本发明涉及分子筛技术领域,具体讲是一种乙烯专用分子筛的制备方法。
背景技术
乙烯装置干燥工艺一般由四至六组干燥器联合操作,主要分为:裂解气干燥器、液相干燥器、裂解气二级干燥器、氢气干燥器、炼厂干气干燥器、炼厂干气混合碳三干燥器等组成。
针对化工行业乙烯装置较高的工艺要求,传统乙烯专用分子筛已不能满足,其主要原因是选料不正确,配方不精准而造成分子筛吸附率偏低,加之抗压强度低,落粉度大,磨耗率差,使用寿命短等不良现象。
保障乙烯分子筛的质量,是延长分子筛的寿命的关键所在,因此研发出一种吸附稳定、安全高效、使用寿命更长的乙烯专用分子筛具有重要的意义。
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:一种乙烯专用分子筛的制备方法,包括以下具体步骤:
1)多维晶体分子筛原粉的制备:将Na-A型人造沸石粉通过K+离子交换成初级K-A型分子筛原粉;再将斜发沸石粉与所述初级K-A型分子筛原粉混合后进行水热晶化为中级K-A型分子筛原粉;最后将菱沸石粉与所述中级K-A型分子筛原粉混合后进行水热晶化为多维晶体分子筛原粉;其中按重量份计:人造沸石粉55-65份;斜发沸石粉25-35份;菱沸石粉5-15份;
2)将步骤1)制备的多维晶体分子筛原粉与粘土混合研磨至325目以上得到混合粉,然后将混合粉与粘结剂混合均匀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于550-580℃焙烧制得乙烯专用分子筛。
所述步骤2)中混合粉的组分重量百分比为:多维晶体分子筛原粉70-90%;粘土10-30%。
所述步骤2)中分子筛坯体的组分重量百分比为:混合粉70-96%;粘结剂4-30%。
所述粘土为热液蚀变亚型高岭土、坡缕缟石中的一种或两种。
所述粘结剂为杨梅栲胶、SG植物胶、羧甲基纤维素钠中的一种或多种。
本发明的有益效果是: 由于Na-A型人造沸石粉为一维体系单晶体,斜发沸石粉为含K、Si较高的三维体系多晶体;菱沸石粉为含Al、Si较高的三维体系多晶体,本发明通过结合三者的空间结构合成多维晶体分子筛原粉,彻底改变分子筛主体的结构,从而达到乙烯专用分子筛吸附稳定、安全高效、操作便捷、使用寿命更长的效果。本发明的乙烯专用分子筛在试用3年后,不破碎,无落粉。再生后经检测(φ2-3mm小球)抗压强度>45N,静态水吸附>18.62%。
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乙烯专用分子筛:
1)多维晶体分子筛原粉的制备:将Na-A型人造沸石粉通过K+离子交换成初级K-A型分子筛原粉;再将斜发沸石粉与所述初级K-A型分子筛原粉混合后进行水热晶化为中级K-A型分子筛原粉;最后将菱沸石粉与所述中级K-A型分子筛原粉混合后进行水热晶化为多维晶体分子筛原粉;其中按重量份计:人造沸石粉55份;斜发沸石粉25份;菱沸石粉15份;
2)将步骤1)制备的多维晶体分子筛原粉与粘土混合研磨至325目以上得到混合粉,然后将混合粉与粘结剂混合均匀后进行造粒得到分子筛坯体;所述混合粉的组分重量百分比为:多维晶体分子筛原粉90%;粘土10%;所述分子筛坯体的组分重量百分比为:混合粉70%;粘结剂30%;所述粘土为热液蚀变亚型高岭土;所述粘结剂为杨梅栲胶。
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于550-580℃焙烧制得乙烯专用分子筛。
所获得的分子筛具有下列技术性质:动态条件下吸水量≥21%,乙烯吸附量≤2.0%,抗压强度70-130N/颗,露点-70℃,静态水吸附>22.5%,分子筛再生3000次以上,磨耗损失小于26%,再生后的分子筛保持吸附性能不变。
实施例二
按照以下具体步骤制备乙烯专用分子筛:
1)多维晶体分子筛原粉的制备:将Na-A型人造沸石粉通过K+离子交换成初级K-A型分子筛原粉;再将斜发沸石粉与所述初级K-A型分子筛原粉混合后进行水热晶化为中级K-A型分子筛原粉;最后将菱沸石粉与所述中级K-A型分子筛原粉混合后进行水热晶化为多维晶体分子筛原粉;其中按重量份计:人造沸石粉60份;斜发沸石粉30份;菱沸石粉10份;
2)将步骤1)制备的多维晶体分子筛原粉与粘土混合研磨至325目以上得到混合粉,然后将混合粉与粘结剂混合均匀后进行造粒或挤条成型得到分子筛坯体;所述混合粉的组分重量百分比为:多维晶体分子筛原粉90%;粘土10%。所述分子筛坯体的组分重量百分比为:混合粉96%;粘结剂4%;所述粘土为坡缕缟石。所述粘结剂为羧甲基纤维素钠。
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于550-580℃焙烧制得乙烯专用分子筛。
乙烯专用分子筛性能如下:动态水吸附22.6%,静态水吸附23.8%,堆比重0.68g/cm3,抗压强度分别为60N,满足露点要求-75℃,分子筛在使用期内不变形,不破碎,再生后依然保持原有性能。
实施例三
按照以下具体步骤制备乙烯专用分子筛:
1)多维晶体分子筛原粉的制备:将Na-A型人造沸石粉通过K+离子交换成初级K-A型分子筛原粉;再将斜发沸石粉与所述初级K-A型分子筛原粉混合后进行水热晶化为中级K-A型分子筛原粉;最后将菱沸石粉与所述中级K-A型分子筛原粉混合后进行水热晶化为多维晶体分子筛原粉;其中按重量份计:人造沸石粉65份;斜发沸石粉25份;菱沸石粉10份;
2)将步骤1)制备的多维晶体分子筛原粉与粘土混合研磨至325目以上得到混合粉,然后将混合粉与粘结剂混合均匀后进行造粒成型得到分子筛坯体;所述混合粉的组分重量百分比为:多维晶体分子筛原粉80%;粘土20%;所述步骤2)中分子筛坯体的组分重量百分比为:混合粉85%;粘结剂15%;所述粘土为热液蚀变亚型高岭土;所述粘结剂为SG植物胶。
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于550-580℃焙烧制得乙烯专用分子筛。
乙烯专用分子筛性能如下:动态水吸附23%,静态水吸附24.1%,堆比重0.76g/cm3,抗压强度分别为80N,满足露点要求-75℃,分子筛在使用期内不变形,不破碎,再生后依然保持原有性能。
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)
1.一种乙烯专用分子筛的制备方法,其特征在于:包括以下具体步骤:
1)多维晶体分子筛原粉的制备:将Na-A型人造沸石粉通过K+离子交换成初级K-A型分子筛原粉;再将斜发沸石粉与所述初级K-A型分子筛原粉混合后进行水热晶化为中级K-A型分子筛原粉;最后将菱沸石粉与所述中级K-A型分子筛原粉混合后进行水热晶化为多维晶体分子筛原粉;其中按重量份计:人造沸石粉55-65份;斜发沸石粉25-35份;菱沸石粉5-15份;
2)将步骤1)制备的多维晶体分子筛原粉与粘土混合研磨至325目以上得到混合粉,然后将混合粉与粘结剂混合均匀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于550-580℃焙烧制得乙烯专用分子筛。
2.根据权利要求1所述的乙烯专用分子筛的制备方法,其特征在于:所述步骤2)中混合粉的组分重量百分比为:多维晶体分子筛原粉70-90%;粘土10-30%。
3.根据权利要求1所述的乙烯专用分子筛的制备方法,其特征在于:所述步骤2)中分子筛坯体的组分重量百分比为:混合粉70-96%;粘结剂4-30%。
4.根据权利要求1所述的乙烯专用分子筛的制备方法,其特征在于:所述粘土为热液蚀变亚型高岭土、坡缕缟石中的一种或两种。
5.根据权利要求1所述的乙烯专用分子筛的制备方法,其特征在于:所述粘结剂为杨梅栲胶、SG植物胶、羧甲基纤维素钠中的一种或多种。
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CN107694544A (zh) * | 2017-10-12 | 2018-02-16 | 江西萍乡市成宇陶瓷有限责任公司 | 乙烯用高效分子筛的制备方法 |
CN109046237A (zh) * | 2018-09-19 | 2018-12-21 | 江西萍乡市成宇陶瓷有限责任公司 | 一种多选择性吸附分子筛的制备方法 |
CN109529787A (zh) * | 2018-12-11 | 2019-03-29 | 彭钰晗 | 一种甲醛吸附分子筛的制备方法 |
CN111167404A (zh) * | 2020-01-10 | 2020-05-19 | 上海航中实业有限公司 | 一种商用车刹车系统的分子筛及其制备方法 |
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CN107694544A (zh) * | 2017-10-12 | 2018-02-16 | 江西萍乡市成宇陶瓷有限责任公司 | 乙烯用高效分子筛的制备方法 |
CN109046237A (zh) * | 2018-09-19 | 2018-12-21 | 江西萍乡市成宇陶瓷有限责任公司 | 一种多选择性吸附分子筛的制备方法 |
CN109529787A (zh) * | 2018-12-11 | 2019-03-29 | 彭钰晗 | 一种甲醛吸附分子筛的制备方法 |
CN111167404A (zh) * | 2020-01-10 | 2020-05-19 | 上海航中实业有限公司 | 一种商用车刹车系统的分子筛及其制备方法 |
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