CN114505097A - 一种轻烃裂解多产低碳烯烃复合分子筛催化剂及其制备方法 - Google Patents
一种轻烃裂解多产低碳烯烃复合分子筛催化剂及其制备方法 Download PDFInfo
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- B01J29/00—Catalysts comprising molecular sieves
- B01J29/04—Catalysts comprising molecular sieves having base-exchange properties, e.g. crystalline zeolites
- B01J29/06—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof
- B01J29/80—Mixtures of different zeolites
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Abstract
本发明公开了一种轻烃催化裂解多产低碳烯烃复合分子筛催化剂及其制备方法,主要步骤如下:将LTA分子筛预氢化后,与商业化的氢型ZSM‑5分子筛混合,借助机械搅拌和超声混合的协同作用,实现分子筛均匀复合,从而充分发挥两种分子筛特有孔道结构的优势。本方法制备的催化剂用于轻烃的催化裂解反应,借助具有十元环孔道结构的酸性ZSM‑5分子筛的催化作用,实现轻烃的高效裂解,同时利用LTA分子筛的八元环孔道结构,抑制裂解产物发生二次反应,从而提高低碳烯烃选择性,有效降低焦炭的生成催化剂的失活速率,提高催化剂使用寿命。该发明简单高效,性能优异,在石油催化裂解生产乙丙烯工艺中具有较好的应用价值。
Description
技术领域:
本发明涉及石油化工技术领域,具体涉及一种轻烃催化裂解高选择性生产低碳烯烃的催化剂及其制备方法。
背景技术:
低碳烯烃(乙烯、丙烯和丁烯)是石油化工生产最基本的原料。目前,生产低碳烯烃的主要工艺包括:蒸汽裂解工艺、催化裂化及催化裂解工艺、甲醇制烯烃技术以及烷烃脱氢工艺和烯烃易位等。其中,蒸汽裂解是应用最广泛的低碳烯烃生产工艺,经过多年发展,蒸汽裂解工艺臻于成熟,但仍存在建设成本高、产能规模小、装置能耗高、三烯收率低、碳排放量大等弊端。催化裂解技术在裂解深度、低碳烯烃产率、灵活调控产物分布、原料适用性及能耗等方面具有显著优势,可克服蒸汽裂解技术的不足,因此催化裂解技术被认为是一种极具发展潜力、能够替代蒸汽裂解生产低碳烯烃的工艺。
专利CN201811437754.8发明了一种Pt-HZSM-5复合催化剂的制备方法,采用商用Si/Al比50的HZSM-5为原料,经过碱处理扩孔后,将Pt的前驱体溶液引入到HZSM5孔内,还原得到Pt-HZSM-5复合催化剂。利用Pt-HZSM-5催化裂解性能和脱氢功能,提高催化裂解烷烃过程中低碳烯烃选择性。专利CN109806907A公开了一种负载型Pt/TiO2/ZSM-5分子筛催化剂,将TiO2负载ZSM-5分子筛后,再将Pt前驱体负载到TiO2/ZSM-5上,氢气还原后得到该类催化剂,该催化剂提高正丁烷活化能力的同时,降低Pt对烯烃的吸附能力,抑制深度脱氢等副反应和焦炭的生成,提高了催化剂的反应稳定性和乙丙烯选择性和收率。专利202110028358.5公开了一种用于催化裂解的金属掺杂HZSM-5分子筛催化剂,活性组份为金属钨元素和过渡金属元素Mn、Cr、Ti的一种,金属钨降低催化剂酸性,抑制积碳,提高催化剂稳定性,用于催化裂解重质油可以提高烯烃、芳烃等产物产率。专利CN102861604B公开了一种EU-1/ZSM-5复合分子筛负载杂多酸催化裂解轻烃制烯烃的方法,按照特定比例取适量模板剂、蒸馏水、EU-1分子筛、硅源混合后晶化、过滤、洗涤、干燥、焙烧、氨交换后,混合少量杂多酸,在粘结剂的作用下成型,焙烧后得到此类复合分子筛催化剂,用于石脑油催化裂解,提高了催化剂的稳定性和乙丙烯的选择性。
综上所述,已有报道中多数研究工作将金属甚至贵金属引入到分子筛,改变催化剂的酸量或酸类型,从而提高轻烃催化裂解过程中低碳烯烃的选择性;还有一部分研究工作,采用较为复杂的方法制备复合分子筛催化剂提高低碳烯烃的选择性。本发明从分子筛孔道结构的角度出发,采用非常简单的方式将不同孔径的两种分子筛均匀复合,无需添加金属或非金属等载体,充分利用不同孔道结构分子筛的特有属性,在催化裂解过程中发挥各自的优势,抑制烯烃二次反应的发生和焦炭的生成,提高催化剂的稳定性、低碳烯烃的选择性和收率。
发明内容:
本发明目的在于提供一种轻烃催化裂解高选择性制低碳烯烃复合分子筛催化剂及其制备方法。该催化剂用于轻烃催化裂解制低碳烯烃过程中,提高低碳烯烃选择性,抑制烯烃产物发生二次反应,降低芳烃等产物的收率,提高催化剂的使用寿命,从而提高轻烃催化裂解技术的整体经济效益。
为了实现上述目的,本发明采用如下技术方案:
一种催化裂解轻烃多产低碳烯烃催化剂,无需掺杂任何金属或非金属活性组分,其活性组分由LTA型分子筛和MFI型分子筛构成,按照重量含量计,MFI分子筛含量在10-80%之间。
LTA分子筛预氢化,采用浓度为1mol/L氯化铵溶液,在80℃下,铵离子交换三次后,去离子水洗涤,干燥后,350-400℃下焙烧6h制得。
一种催化裂解轻烃多产低碳烯烃催化剂的制备方法,制备步骤如下:
(1)取MFI分子筛、LTA分子筛按一定质量比混合后加入30倍质量的去离子水,室温(20~25℃),高速机械搅拌下,超声分散1h,实现两种分子筛在悬浮液中高度分散。
(2)通过高速离心实现固液分离,将上层水溶液倾出得到下层白色固体,用去离子水反复清洗3次,在80℃下干燥24-48h,得到所需分子筛。
(3)催化剂在投入使用之前,需在反应温度下活化2小时。
附图说明:
图1是采用实施例5得到催化剂MA-50的扫描电镜照片;
图2是实施例与对比例中催化剂的裂解性能对比。
具体实施方式:
实施例1
取LTA分子筛20g置于烧杯中,加入配置好的1mol/L氯化铵溶液160mL,混合后搅拌均匀。将混合悬浮液放入圆底烧瓶,升温至80℃,加热搅拌12h后,通过高速离心分离固体和水溶液,将上层水溶液倾出得到下层白色固体,用90mL去离子水反复清洗3次。将得到的白色固体再次加入配置好的1mol/L氯化铵溶液重复上述步骤两次,离心分离得到白色固体,在80℃下干燥24h,取出,置入马弗炉400℃焙烧24h。600℃焙烧2h,得到氢化LTA分子筛。
取氢型ZMS-5分子筛和氢型LTA分子筛,按照质量比1:9混合,加入30倍质量的去离子水,在室温(20℃~25℃)下,借助高速机械搅拌,并超声辅助分散1h,通过高速离心实现固体和水溶液的分离,将上层水溶液倾出得到下层白色固体,用去离子水反复清洗3次,在80℃下干燥24h,得到所需催化剂粉末。之后用压片机压制粉末,筛分出40-60目粒径的催化剂,记作MA-10。
实施例2
本实施例中,氢型MFI分子筛和氢型LTA分子筛质量比1:4,其它步骤同实施例1,记作MA-20。
实施例3
本实施例中,氢型MFI分子筛和氢型LTA分子筛质量比3:7,其它步骤同实施例1,记作MA-30。
实施例4
本实施例中,氢型MFI分子筛和氢型LTA分子筛质量比2:3,其它步骤同实施例1,记作MA-40。
实施例5
本实施例中,氢型MFI分子筛和氢型LTA分子筛质量比1:1,其它步骤同实施例1,记作MA-50。
实施例6
本实施例中,氢型MFI分子筛和氢型LTA分子筛质量比3:2,其它步骤同实施例1,记作MA-60。
实施例7
本实施例中,氢型MFI分子筛和氢型LTA分子筛质量比7:3,其它步骤同实施例1,记作MA-70。
实施例8
本实施例中,氢型MFI分子筛和氢型LTA分子筛质量比4:1,其它步骤同实施例1,记作MA-80。
对比例1
本对比例中,催化剂为氢型LTA分子筛,氢型LTA分子筛的制备同实施例1,记作HA。
对比例2
本对比例中,催化剂为氢型MFI分子筛,记作HM。
以正己烷为原料,在相同的催化剂粒径40-60目、装填量2g和氮气流速20mL/min下,开展连续10小时催化裂解性能评价。评价条件及10小时内间隔30分钟取样分析平均结果如表所示:
表1.催化剂固定床连续评价条件及结果
上述虽然对本发明的具体实施方式进行了描述,但并非对本发明保护范围的限制,所属领域技术人员应该明白,在本发明的技术方案基础上,本领域技术人员不需要付出创造性劳动即可做出的各种修改或变形,仍在本发明的保护范围之内。
Claims (5)
1.一种轻烃裂解多产低碳烯烃复合分子筛催化剂及其制备方法,其特征在于,所述催化剂活性组分由LTA和MFI型分子筛组成,无需掺杂任何金属或非金属活性组分,按照质量计,氢型MFI分子筛含量在10-80%之间。
2.根据权利要求1所述的制备方法,其特征在于,LTA型分子筛须预氢化,采用浓度为1mol/L氯化铵溶液,在一定温度下,铵离子交换三次后,用去离子水洗涤,干燥后,350-400℃下焙烧6h制得。
3.根据权利要求1所述催化剂的制备方法,其特征在于,制备步骤如下:
(1)取MFI分子筛和LTA分子筛按一定质量比混合后,加入30倍质量的去离子水,室温(20~25℃),高速机械搅拌下,超声分散1h,实现两种分子筛在悬浮液中高度分散。
(2)通过高速离心实现固液分离,将上层水溶液倾倒出得到下层白色固体,用去离子水清洗3次,在80℃下干燥24-48h,得到所需分子筛。
4.根据权利要求1所述催化剂的制备方法,其特征在于,催化剂在投入使用之前,需在反应温度下活化1-2h。
5.根据权利要求1所述催化剂特征在于,利用MFI分子筛的酸性裂解烷烃,结合LTA分子筛八元环孔道的吸附保护效应,可抑制裂解产物发生二次反应,提高烷烃裂解过程中低碳烯烃选择性和催化剂使用寿命。
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