CN106622345A - 一种双功能多级孔分子筛催化剂及其制备方法 - Google Patents
一种双功能多级孔分子筛催化剂及其制备方法 Download PDFInfo
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- 239000003054 catalyst Substances 0.000 title claims abstract description 34
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 title claims abstract description 26
- 239000002808 molecular sieve Substances 0.000 title claims abstract description 24
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
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- 238000006243 chemical reaction Methods 0.000 claims abstract description 13
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- 239000013078 crystal Substances 0.000 claims abstract description 4
- 239000000243 solution Substances 0.000 claims description 19
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 15
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- 239000011259 mixed solution Substances 0.000 claims description 14
- 239000007787 solid Substances 0.000 claims description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 13
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims description 12
- 238000001354 calcination Methods 0.000 claims description 10
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 9
- 238000000034 method Methods 0.000 claims description 8
- LPSKDVINWQNWFE-UHFFFAOYSA-M tetrapropylazanium;hydroxide Chemical compound [OH-].CCC[N+](CCC)(CCC)CCC LPSKDVINWQNWFE-UHFFFAOYSA-M 0.000 claims description 7
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 6
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- UFWIBTONFRDIAS-UHFFFAOYSA-N Naphthalene Chemical compound C1=CC=CC2=CC=CC=C21 UFWIBTONFRDIAS-UHFFFAOYSA-N 0.000 claims description 4
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 4
- 229910021645 metal ion Inorganic materials 0.000 claims description 4
- LRTOHSLOFCWHRF-UHFFFAOYSA-N 1-methyl-1h-indene Chemical class C1=CC=C2C(C)C=CC2=C1 LRTOHSLOFCWHRF-UHFFFAOYSA-N 0.000 claims description 2
- 235000017166 Bambusa arundinacea Nutrition 0.000 claims description 2
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- 241000345998 Calamus manan Species 0.000 claims description 2
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- 229920002488 Hemicellulose Polymers 0.000 claims description 2
- KKCBUQHMOMHUOY-UHFFFAOYSA-N Na2O Inorganic materials [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 claims description 2
- 244000082204 Phyllostachys viridis Species 0.000 claims description 2
- 235000015334 Phyllostachys viridis Nutrition 0.000 claims description 2
- 240000008042 Zea mays Species 0.000 claims description 2
- 235000002017 Zea mays subsp mays Nutrition 0.000 claims description 2
- SMZOGRDCAXLAAR-UHFFFAOYSA-N aluminium isopropoxide Chemical compound [Al+3].CC(C)[O-].CC(C)[O-].CC(C)[O-] SMZOGRDCAXLAAR-UHFFFAOYSA-N 0.000 claims description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 2
- 239000011425 bamboo Substances 0.000 claims description 2
- 150000001720 carbohydrates Chemical class 0.000 claims description 2
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- 229910052681 coesite Inorganic materials 0.000 claims description 2
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- 239000000377 silicon dioxide Substances 0.000 claims description 2
- 229910052682 stishovite Inorganic materials 0.000 claims description 2
- 229910052718 tin Inorganic materials 0.000 claims description 2
- 229910052719 titanium Inorganic materials 0.000 claims description 2
- 229910052905 tridymite Inorganic materials 0.000 claims description 2
- 239000002699 waste material Substances 0.000 claims description 2
- 239000002023 wood Substances 0.000 claims description 2
- 229910001845 yogo sapphire Inorganic materials 0.000 claims description 2
- 229910052726 zirconium Inorganic materials 0.000 claims description 2
- 206010054949 Metaplasia Diseases 0.000 claims 1
- 235000016383 Zea mays subsp huehuetenangensis Nutrition 0.000 claims 1
- 239000002253 acid Substances 0.000 claims 1
- 235000009973 maize Nutrition 0.000 claims 1
- 230000015689 metaplastic ossification Effects 0.000 claims 1
- 239000010902 straw Substances 0.000 claims 1
- 239000002028 Biomass Substances 0.000 abstract description 6
- 230000003197 catalytic effect Effects 0.000 abstract description 4
- 150000001491 aromatic compounds Chemical class 0.000 abstract description 2
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- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 3
- 239000008367 deionised water Substances 0.000 description 3
- 229910021641 deionized water Inorganic materials 0.000 description 3
- 238000001914 filtration Methods 0.000 description 3
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 3
- 239000010931 gold Substances 0.000 description 3
- 229910052737 gold Inorganic materials 0.000 description 3
- OGHBATFHNDZKSO-UHFFFAOYSA-N propan-2-olate Chemical compound CC(C)[O-] OGHBATFHNDZKSO-UHFFFAOYSA-N 0.000 description 3
- 230000035484 reaction time Effects 0.000 description 3
- 238000006555 catalytic reaction Methods 0.000 description 2
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- 235000005824 Zea mays ssp. parviglumis Nutrition 0.000 description 1
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- 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
- B01J29/40—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof of the pentasil type, e.g. types ZSM-5, ZSM-8 or ZSM-11, as exemplified by patent documents US3702886, GB1334243 and US3709979, respectively
- B01J29/405—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof of the pentasil type, e.g. types ZSM-5, ZSM-8 or ZSM-11, as exemplified by patent documents US3702886, GB1334243 and US3709979, respectively containing rare earth elements, titanium, zirconium, hafnium, zinc, cadmium, mercury, gallium, indium, thallium, tin or lead
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
- B01J35/64—Pore diameter
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
- B01J35/64—Pore diameter
- B01J35/643—Pore diameter less than 2 nm
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2229/00—Aspects of molecular sieve catalysts not covered by B01J29/00
- B01J2229/10—After treatment, characterised by the effect to be obtained
- B01J2229/18—After treatment, characterised by the effect to be obtained to introduce other elements into or onto the molecular sieve itself
- B01J2229/183—After treatment, characterised by the effect to be obtained to introduce other elements into or onto the molecular sieve itself in framework positions
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
本发明涉及一种双功能多级孔分子筛催化剂及其制备方法,属于分子筛催化材料制备领域,该催化剂由ZSM‑5分子筛颗粒在纳米尺度上并列排布,形成结构规整的晶体结构,颗粒之间的空隙形成尺寸不一的中孔,颗粒内部保持了ZSM‑5的微孔结构,催化剂含有路易斯酸点和布朗斯特酸点两种催化活性中心,具有两种催化功能,该催化剂结晶度好,未引入其它结构分子筛,微孔尺寸及形状均一,与双功能活性点配合,适合于生物质等大分子反应体系,有利于提高芳香类及烯类目标产物的选择性,该催化剂的制备方法简单,操作方便,易于工业化生产。
Description
技术领域
本发明涉及一种双功能多级孔分子筛催化剂及其制备方法,属于生物质及废弃物能源化利用领域。
背景技术
能源危机及环境污染问题日益严重,因此,将低值生物质及废弃高分子材料转化为能源及化工原料意义重大,已经成为世界各国的能源战略之一。快速催化热解技术可以将生物质及废弃高分子材料转换为高品质的生物油、燃气和生物炭,具有广阔的市场前景和重要的社会价值。
该技术的关键点之一是选用性能优良的催化剂,一方面能有效提高反应转化率和目标产物的选择性,另一方面自身稳定性要好、不易失活。ZSM-5分子筛由于其特有的晶体结构和孔隙尺寸,对芳香类化合物和烯烃类化合物有很好的选择性,是当今化学工业上使用最广泛的分子筛催化剂,但其用于大分子体系反应过程中稳定性不好,易于失活。另外,生物质快速热解过程中反应随机性强,反应过程复杂,产物众多,目标反应的催化机理不尽相同,单一的催化剂活性点位只能促进单一类型的反应过程,导致产物选择性不高。
发明内容
针对以上问题,本发明的目的是提供一种双功能多级孔分子筛催化剂及其制备方法,该催化剂具有多级孔隙结构,含有路易斯酸点和布朗斯特酸点两种催化活性中心,具有两种催化功能,适合于生物质等大分子反应体系,有利于提高芳香类及烯类目标产物的选择性,制备方法简单,操作方便,易于工业化生产。
本发明提出了一种双功能多级孔分子筛催化剂及其制备方法,其特征在于该催化剂由ZSM-5分子筛颗粒在纳米尺度上并列排布,形成结构规整的晶体结构,颗粒之间的空隙形成尺寸不一的中孔,颗粒内部保持了ZSM-5的微孔结构,形成了多级孔结构,其微孔孔径为0.55~0.65 nm,其介孔尺寸为1nm~100 nm,分子筛结构上含有路易斯酸点和布朗斯特酸点,路易斯酸点强度和布朗斯特酸点的强度比可调;所述双功能多级孔分子筛催化剂的制备按照以下步骤进行:
(1)按照各组分比例配制溶液,具体过程为:将一定量的浓度为10 M的NaOH溶液和去离子水加入浓度为1 M的TPAOH溶液中充分混合,之后将一定量的Ludox HS-40逐滴加入上述混合溶液中,并搅拌1h形成透明溶液,最后将一定量的Aluminum isopropoxide加入上述混合溶液中,并搅拌30min,最后配制的溶液中各成分的比例为:SiO2 : 0.25 TPAOH :(0.006~0.02) Al2O3 : 0.014 Na2O : 16.44 H2O;
(2)利用水热法进行结晶,具体过程为:将上述配制的混合溶液置入特氟龙内衬的金属反应器中,在90~135 oC的条件下处理48~72 h,将得到的固体物质使用蒸馏水清洗后在100oC 的温度下过夜干燥,干燥后置于管式炉内煅烧12 h,煅烧温度为550 oC;
(3)采用原子植入的方法引入路易斯酸点,具体方法是将上述得到的固体物质先进行脱铝,再在加入金属离子溶液,在水热环境下处理12~120 h,这些金属离子包括Al, Ga,Sn, Ti, Zr或它们的组合。
所述的ZSM-5分子筛催化剂颗粒是球形,颗粒粒径范围为10~100nm。
所述的路易斯酸点强度和布朗斯特酸点的强度为0.1~100。
所述的ZSM-5分子筛的Si/Al为15~300。
该催化剂应用于农林废弃物、废旧塑料、食品废物、碳水化合物或其组合物等大分子反应体系,并将其转化生成芳香类及烯烃类产物。
所述的农林废弃物包括各种木材、藤条、竹材、纤维素、半纤维素、木质素、玉米秸秆、其它农林废弃物或它们的组合。
所述的芳香类产物包括苯、甲基苯、乙基苯、萘、甲基萘、茚、甲基茚及它们的同分异构体。
所述的烯烃类产物包括乙烯、丙烯、丁烯及它们的同分异构体。
附图说明
图1是实施例1所制备的样品的XRD图;
图2是实施例1所制备的样品的SEM图;
图3是实施例1所制备的样品的孔径分布图。
具体实施方式
实施例1
将0.233mL的10M的NaOH溶液和0.163g的去离子水加入20.806mL的1M的TPAOH溶液中;将12.5g的Ludox HS-40逐滴加入上述混合溶液中,并搅拌1h;将0.566g的aluminumisopropoxide加入上述混合溶液中,并搅拌30min;将上述混合溶液置入有特氟龙内衬的金属反应器中进行水热合成反应,反应温度135 oC,反应时间48 h;将等到的固体物质使用蒸馏水清洗;将清洗后的物质在100 oC的温度下过夜干燥;将干燥后的物质煅烧12h,煅烧温度550 oC,空气流速3ml/min;将得到的固体物质脱铝,并加入0.07g 的SnCl4·5H2O,水热反应48 h,得到的固体清洗、过滤,煅烧等到最终催化剂。
实施例2
将0.233mL的10M的NaOH溶液和0.163g的去离子水加入20.806mL的1M的TPAOH溶液中;将12.5g的Ludox HS-40逐滴加入上述混合溶液中,并搅拌1h;将0.24g的aluminumisopropoxide加入上述混合溶液中,并搅拌30min;将上述混合溶液置入有特氟龙内衬的金属反应器中进行水热合成反应,反应温度120 oC,反应时间72 h;;将等到的固体物质使用蒸馏水清洗;将清洗后的物质在100 oC的温度下过夜干燥;将干燥后的物质煅烧12h,煅烧温度550 oC,空气流速3ml/min;将得到的固体物质脱铝,并加入0.07g 的SnCl4·5H2O,水热反应48 h,得到的固体清洗、过滤,煅烧等到最终催化剂。
实施例3
将0.233mL的10M的NaOH溶液和0.163g的去离子水加入20.806mL的1M的TPAOH溶液中;将12.5g的Ludox HS-40逐滴加入上述混合溶液中,并搅拌1h;将0.566g的aluminumisopropoxide加入上述混合溶液中,并搅拌30min;将上述混合溶液置入有特氟龙内衬的金属反应器中进行水热合成反应,反应温度135 oC,反应时间48 h;将等到的固体物质使用蒸馏水清洗;将清洗后的物质在100 oC的温度下过夜干燥;将干燥后的物质煅烧12h,煅烧温度550 oC,空气流速3ml/min;将得到的固体物质脱铝,并加入100 mL 浓度为0.01M的Ga(NO3)3 ,水热反应12 h,得到的固体清洗、过滤,煅烧等到最终催化剂。
以上仅为本发明的较佳实施例,但本发明实施的范围并不受其限制。
Claims (8)
1.一种双功能多级孔分子筛催化剂及其制备方法,其特征在于该催化剂由ZSM-5分子筛颗粒在纳米尺度上并列排布,形成结构规整的晶体结构,颗粒之间的空隙形成尺寸不一的中孔,颗粒内部保持了ZSM-5的微孔结构,形成了多级孔结构,其微孔孔径为0.55~0.65nm,其介孔尺寸为1~100 nm,分子筛结构上含有路易斯酸点和布朗斯特酸点,路易斯酸点强度和布朗斯特酸点的强度比可调;所述双功能多级孔分子筛催化剂的制备按照以下步骤进行:
(1)按照各组分比例配制溶液,具体过程为:将一定量的浓度为10 M的NaOH溶液和去离子水加入浓度为1 M的TPAOH溶液中充分混合,之后将一定量的Ludox HS-40逐滴加入上述混合溶液中,并搅拌1 h形成透明溶液,最后将一定量的Aluminum isopropoxide加入上述混合溶液中,并搅拌30min,最后配制的溶液中各成分的比例为:SiO2 : 0.25 TPAOH :(0.006~0.02) Al2O3 : 0.014 Na2O : 16.44 H2O;
(2)利用水热法进行结晶,具体过程为:将上述配制的混合溶液置入特氟龙内衬的金属反应器中,在90~135 oC的条件下处理48~72 h,将得到的固体物质使用蒸馏水清洗后在100oC 的温度下过夜干燥,干燥后置于管式炉内煅烧12 h,煅烧温度为550 oC;
(3)采用原子植入的方法引入路易斯酸点,具体方法是将上述得到的固体物质先进行脱铝,再在加入金属离子溶液,在水热环境下处理12~120 h,这些金属离子包括Al, Ga,Sn, Ti, Zr或它们的组合。
2.根据权利要求1所述的一种双功能多级孔分子筛催化剂,其特征在于所述的ZSM-5分子筛催化剂颗粒是球形,颗粒粒径范围为10~100 nm。
3.根据权利要求1所述的一种双功能多级孔分子筛催化剂,其特征在于所述的路易斯酸点强度和布朗斯特酸点的强度为0.1~100。
4.根据权利要求1所述的一种双功能多级孔分子筛催化剂,其特征在于所述的ZSM-5分子筛的Si/Al为15~300。
5.根据权利要求1所述的一种双功能多级孔分子筛催化剂,其特征在于该催化剂应用于农林废弃物、废旧塑料、食品废物、碳水化合物或其组合物等大分子反应体系,并将其转化生成芳香类及烯烃类产物。
6.根据权利要求5所述的一种双功能多级孔分子筛催化剂,其特征在于所述的农林废弃物包括各种木材、藤条、竹材、纤维素、半纤维素、木质素、玉米秸秆、其它农林废弃物或它们的组合。
7.根据权利要求5所述的一种双功能多级孔分子筛催化剂,其特征在于所述的芳香类产物包括苯、甲基苯、乙基苯、萘、甲基萘、茚、甲基茚及它们的同分异构体。
8.根据权利要求5所述的一种双功能多级孔分子筛催化剂,其特征在于所述的烯烃类产物包括乙烯、丙烯、丁烯及它们的同分异构体。
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