CN108906119A - 一种sapo-34复合分子筛的制备方法 - Google Patents
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Abstract
本发明通过对天然斜发沸石进行酸处理,与SAPO‑34合成了一种纳米复合分子筛,并对催化剂在MTO反应中的性能进行了研究。SAPO‑34虽是一种具有高选择性,高热稳定性的催化剂,但也由于微孔中积碳形成快速失活。将天然斜发沸石通过硝酸处理,制得H型分子筛,结晶度降低,表面积增加。本发明将H型分子筛作为粘合剂与SAPO‑34复合合成纳米SAPO‑34复合分子筛,该纳米复合分子筛具有较高选择性,与SAPO‑34相比有较长催化寿命,成本低并能加快催化反应速度。
Description
技术领域
本发明属于分子筛催化剂合成领域,具体涉及一种SAPO-34复合分子筛的制备方法。
背景技术
随着全球原油价格的上涨,乙烯和丙烯作为聚乙烯产生必不少的原材料,其需求量也逐渐增加,因此引起了研究人员注意到将甲醇催化转化为低碳烯烃(MTO)过程。由于分子筛是基于均匀三维纳米孔道具有不同的酸性强度和部位,它们成为分离和催化过程不可或缺的成员。天然斜发沸石纳米复合催化剂由于它们的结构和功能相似,如大的比表面积,离子交换能力,以及与其他大量使用的催化剂相比它们对环境无伤害,被用于更多的研究。因此,独特的特性如微孔,以及适当的酸性强度使SAPO- 34成为MTO工艺最常见的催化剂。SAPO- 34具有较高的选择性和水热稳定性,然而,它被微孔中积炭的形成迅速的破坏了。
发明内容
本发明的目的是提供一种具有较高选择性和较长催化寿命的SAPO-34复合分子筛的制备方法。
为实现上述目的,本发明采用的技术方案是,一种SAPO-34复合分子筛分子筛的制备方法,包括以下步骤:
1)天然斜发沸石处理:将天然斜发沸石加入硝酸溶液中,70℃下加热8h,离心,洗涤至pH=6,120℃干燥12h,500℃焙烧4h,即得H型分子筛;
2)SAPO-34凝胶制备:分别将异丙醇铝Al(OPri)3,二乙胺(DEA)加入去离子水中,混合搅拌2h;加入原硅酸四乙酯(TEOS),混合搅拌2.5h;加入H3PO4溶液,搅拌3h得到凝胶乳液;
3)将步骤1)所得的H型分子筛加入步骤2)所制备的凝胶乳液中,混合搅拌1h,超声1h,190℃水热晶化24h;洗涤,120℃干燥12h,500℃焙烧4h,即得SAPO-34复合分子筛。
优选的,所述步骤1)中硝酸溶液与天然斜发沸石的液固比为20:1。
优选的,步骤1)中硝酸溶液浓度为1mol/L。
优选的,步骤2)中所得凝胶乳液摩尔组成为n(Al2O3): n(P2O5): n(SiO2):n(DEA):n(H2O)=1: 1 : 0.8: 8.0 : 20。
优选的,步骤3)中制备的SAPO-34复合分子筛中SAPO-34的含量为H型分子筛的50~90wt%。
本发明产生的有益效果是:本发明通过对天然斜发沸石进行酸处理,与SAPO-34合成了一种纳米复合分子筛,并对催化剂在MTO反应中的性能进行了研究。SAPO-34虽是一种具有高选择性,高热稳定性的催化剂,但也由于微孔中积碳形成快速失活。将天然斜发沸石通过硝酸处理,制得H型分子筛,结晶度降低,表面积增加。本发明将H型分子筛作为粘合剂与SAPO-34复合合成纳米SAPO-34复合分子筛,该纳米复合分子筛具有较高选择性,与SAPO-34相比有较长催化寿命,成本低并能加快催化反应速度。
附图说明
图1为未处理的天然斜发沸石、H型分子筛、SAPO-34分子筛及实施例1-3制备的的纳米SAPO-34复合分子筛XRD图。
图2为在SAPO-34上,天然沸石上,天然沸石和SAPO-34的物理混合物,以及纳米SAPO-34复合分子筛上甲醇转化率。
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,但本发明的保护范围不限于此。
实施例1
一种SAPO-34复合分子筛分子筛的制备方法,包括以下步骤:
1)天然斜发沸石处理:将天然斜发沸石按固液比1g:20ml加入1mol/L硝酸溶液中混合,70℃下加热8h,离心,洗涤至pH=6,120℃干燥12h,500℃焙烧4h,即得H型分子筛;
2)SAPO-34凝胶制备:分别将异丙醇铝Al(OPri)3,二乙胺(DEA)加入去离子水中,混合搅拌2h;加入原硅酸四乙酯(TEOS),混合搅拌2.5h;加入H3PO4溶液,搅拌3h得到凝胶乳液;凝胶乳液摩尔组成为n(Al2O3): n(P2O5): n(SiO2):n(DEA): n(H2O)=1: 1 : 0.8: 8.0 : 20;
3)将步骤1)所得的H型分子筛加入步骤2)所制备的凝胶乳液中,混合搅拌1h,在24KHZ的频率下超声1h,190℃水热晶化24h;通过离心法用蒸馏水洗涤3次,120℃干燥12h,500℃焙烧4h,即得SAPO-34复合分子筛(复合分子筛中SAPO-34的含量为H型分子筛的50wt%)。
实施例2
实施例2与实施例1的不同之处在于步骤3)为:将步骤1)所得的H型分子筛加入步骤2)所制备的凝胶乳液中,混合搅拌1h,在24KHZ的频率下超声1h,190℃水热晶化24h;通过离心法用蒸馏水洗涤3次,,120℃干燥12h,500℃焙烧4h,即得SAPO-34复合分子筛(复合分子筛中SAPO-34的含量为H型分子筛的70wt%)。
实施例3
实施例3与实施例1的不同之处在于步骤3)为:将步骤1)所得的H型分子筛加入步骤2)所制备的凝胶乳液中,混合搅拌1h,在24KHZ的频率下超声1h,190℃水热晶化24h;通过离心法用蒸馏水洗涤3次,,120℃干燥12h,500℃焙烧4h,即得SAPO-34复合分子筛(复合分子筛中SAPO-34的含量为H型分子筛的90wt%)。
对比例1
SAPO-34分子筛的制备:分别将异丙醇铝Al(OPri)3,二乙胺(DEA)加入去离子水中,混合搅拌2h;加入原硅酸四乙酯(TEOS),混合搅拌2.5h;加入H3PO4溶液,搅拌3h得到凝胶乳液,摩尔组成为n(Al2O3): n(P2O5): n(SiO2):n(DEA): n(H2O)=1: 1 : 0.8: 8.0 : 20,190℃水热晶化24h;离心,洗涤,120℃干燥12h,500℃焙烧4h,即得SAPO-34分子筛。
图1为未处理的天然斜发沸石、H型分子筛、SAPO-34分子筛及实施例1-3制备的的SAPO-34复合分子筛(记为S/C)XRD图。图1中横坐标为角度,纵坐标为结晶度。在图1中标记(a)为未处理的天然斜发沸石,标记(b)为HNO3处理过的天然斜发沸石,标记(c)为SAPO-34;标记(d)为实施例1制备的SAPO-34复合分子筛,其中(SAPO-34的含量为H型分子筛的50%);标记(e)为实施例2制备的SAPO-34复合分子筛,其中(SAPO-34的含量为H型分子筛的70%);标记(f)为实施例3制备的SAPO-34复合分子筛,其中(SAPO-34的含量为H型分子筛的90%)。从图1中可以看出,经改性的天然斜发沸石结晶度降低;复合分子筛样品显示了纳米复合结构中SAPO-34与天然斜发沸石两个相的共同存在;此外,正如纳米复合材料XRD图观察到的一样,超声波在合成过程中通过声谱化导致了完全结晶产物的形成,这是由于超声能有效促进成改善核阶段,产生大量原子核,随后的水热处理使原子核生长达到完全结晶状态。
应用实验
将SAPO-34分子筛、天然沸石上、天然沸石和SAPO-34的物理混合物、实施例中制备SAPO-34复合分子筛(记为S/C)应用在催化甲醇制低碳烯烃的反应中,反应结果如图2所示。从图2中可以看出,根据这些样品的结构就失活行为来说,样品在MTO反应中转化率有很大不同,在所有这些过程,甲醇的转化随着时间推移而增加,在约60分钟后甲醇转化率几乎为100%;在60-260分钟之间在SAP0-34上甲醇的转化率是高的,之后由于积炭形成快速失活;在0-300分钟之间在物理混合物上甲醇的转化与SAPO-34是相似的,然而与SAPO-34和改性过的沸石相比,它失活的很慢,S/C纳米复合分子筛与其他样品相比显示了更好的性能,且保持这个性能很长时间,此外,当纳米复合分子筛作为催化剂时,在天然斜发沸石和SAPO-34上显示的高失活率在纳米复合分子筛上并未观察到;随着时间流动,由于甲醇分子最终在酸性位上吸附和转化,分子产物形成分散的孔结构,S/C纳米复合分子筛催化剂快速转化且活性持续时间超过420分钟。
Claims (7)
1.一种SAPO-34复合分子筛分子筛的制备方法,其特征在于包括以下步骤:
1)天然斜发沸石处理:将天然斜发沸石加入硝酸溶液中,70℃下加热8h,离心,洗涤至pH=6,120℃干燥12h,500℃焙烧4h,即得H型分子筛;
2)SAPO-34凝胶制备:分别将异丙醇铝Al(OPri)3,二乙胺(DEA)加入去离子水中,混合搅拌2h;加入原硅酸四乙酯(TEOS),混合搅拌2.5h;加入H3PO4溶液,搅拌3h得到凝胶乳液;
3)将步骤1)所得的H型分子筛加入步骤2)所制备的凝胶乳液中,混合搅拌1h,超声1h,190℃水热晶化24h;洗涤,120℃干燥12h,500℃焙烧4h,即得SAPO-34复合分子筛。
2.如权利1要求做所述的SAPO-34复合分子筛的制备方法,其特征在于步骤1)中硝酸溶液与天然斜发沸石的液固比为20:1。
3.如权利1要求做所述的SAPO-34复合分子筛的制备方法,其特征在于步骤1)中硝酸溶液浓度为1mol/L。
4. 如权利1要求做所述的SAPO-34复合分子筛的制备方法,其特征在于步骤2)中所得凝胶乳液摩尔组成为n(Al2O3): n(P2O5): n(SiO2):n(DEA): n(H2O)=1: 1 : 0.8: 8.0 :20。
5.如权利1要求做所述的SAPO-34复合分子筛的制备方法,其特征在于:步骤3)中制备的SAPO-34复合分子筛中SAPO-34的含量为H型分子筛的50~90wt%。
6.采用权利要求1-5任一方法制备的SAPO-34复合分子筛。
7.如权利要求6所述SAPO-34复合分子筛在催化甲醇制低碳烯烃的反应中应用。
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