CN111760584A - 一种新型甲基吡啶催化剂的制备的方法 - Google Patents
一种新型甲基吡啶催化剂的制备的方法 Download PDFInfo
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- 239000003054 catalyst Substances 0.000 title claims abstract description 43
- BSKHPKMHTQYZBB-UHFFFAOYSA-N 2-methylpyridine Chemical compound CC1=CC=CC=N1 BSKHPKMHTQYZBB-UHFFFAOYSA-N 0.000 title claims abstract description 20
- 238000002360 preparation method Methods 0.000 title abstract description 8
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 claims abstract description 19
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 18
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229910021645 metal ion Inorganic materials 0.000 claims abstract description 14
- 238000003756 stirring Methods 0.000 claims abstract description 14
- 239000000725 suspension Substances 0.000 claims abstract description 14
- 238000000034 method Methods 0.000 claims abstract description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000006243 chemical reaction Methods 0.000 claims abstract description 8
- 244000282866 Euchlaena mexicana Species 0.000 claims abstract description 7
- 230000004913 activation Effects 0.000 claims abstract description 7
- 238000001914 filtration Methods 0.000 claims abstract description 7
- 230000003213 activating effect Effects 0.000 claims abstract description 4
- 238000001354 calcination Methods 0.000 claims abstract description 4
- -1 compound silicate Chemical class 0.000 claims abstract description 3
- 238000000643 oven drying Methods 0.000 claims abstract description 3
- YKTSYUJCYHOUJP-UHFFFAOYSA-N [O--].[Al+3].[Al+3].[O-][Si]([O-])([O-])[O-] Chemical compound [O--].[Al+3].[Al+3].[O-][Si]([O-])([O-])[O-] YKTSYUJCYHOUJP-UHFFFAOYSA-N 0.000 claims description 30
- 239000004110 Zinc silicate Substances 0.000 claims description 8
- 235000019352 zinc silicate Nutrition 0.000 claims description 8
- 238000013329 compounding Methods 0.000 claims description 6
- ASTZLJPZXLHCSM-UHFFFAOYSA-N dioxido(oxo)silane;manganese(2+) Chemical compound [Mn+2].[O-][Si]([O-])=O ASTZLJPZXLHCSM-UHFFFAOYSA-N 0.000 claims description 6
- 239000010941 cobalt Substances 0.000 claims description 5
- 229910017052 cobalt Inorganic materials 0.000 claims description 5
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 5
- HCWCAKKEBCNQJP-UHFFFAOYSA-N magnesium orthosilicate Chemical compound [Mg+2].[Mg+2].[O-][Si]([O-])([O-])[O-] HCWCAKKEBCNQJP-UHFFFAOYSA-N 0.000 claims description 5
- 239000000391 magnesium silicate Substances 0.000 claims description 5
- 229910052919 magnesium silicate Inorganic materials 0.000 claims description 5
- 235000019792 magnesium silicate Nutrition 0.000 claims description 5
- 239000002131 composite material Substances 0.000 claims description 4
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 2
- ZOIVSVWBENBHNT-UHFFFAOYSA-N dizinc;silicate Chemical compound [Zn+2].[Zn+2].[O-][Si]([O-])([O-])[O-] ZOIVSVWBENBHNT-UHFFFAOYSA-N 0.000 claims 2
- 238000009472 formulation Methods 0.000 claims 1
- 239000000203 mixture Substances 0.000 claims 1
- 150000004760 silicates Chemical class 0.000 claims 1
- 230000002194 synthesizing effect Effects 0.000 abstract description 6
- 239000002808 molecular sieve Substances 0.000 abstract description 5
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 abstract description 5
- 238000006555 catalytic reaction Methods 0.000 abstract description 3
- 238000011068 loading method Methods 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 21
- ITQTTZVARXURQS-UHFFFAOYSA-N 3-methylpyridine Chemical compound CC1=CC=CN=C1 ITQTTZVARXURQS-UHFFFAOYSA-N 0.000 description 14
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 description 6
- XSMMCTCMFDWXIX-UHFFFAOYSA-N zinc silicate Chemical compound [Zn+2].[O-][Si]([O-])=O XSMMCTCMFDWXIX-UHFFFAOYSA-N 0.000 description 6
- 239000000575 pesticide Substances 0.000 description 5
- 239000005995 Aluminium silicate Substances 0.000 description 4
- 235000012211 aluminium silicate Nutrition 0.000 description 4
- 229910000323 aluminium silicate Inorganic materials 0.000 description 4
- 238000001035 drying Methods 0.000 description 4
- 150000001875 compounds Chemical class 0.000 description 3
- 239000003814 drug Substances 0.000 description 3
- 229940079593 drug Drugs 0.000 description 3
- 238000003837 high-temperature calcination Methods 0.000 description 3
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 description 3
- 229910019142 PO4 Inorganic materials 0.000 description 2
- 239000000543 intermediate Substances 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 2
- 239000010452 phosphate Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000012266 salt solution Substances 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- SNICXCGAKADSCV-JTQLQIEISA-N (-)-Nicotine Chemical compound CN1CCC[C@H]1C1=CC=CN=C1 SNICXCGAKADSCV-JTQLQIEISA-N 0.000 description 1
- UJPKMTDFFUTLGM-UHFFFAOYSA-N 1-aminoethanol Chemical compound CC(N)O UJPKMTDFFUTLGM-UHFFFAOYSA-N 0.000 description 1
- WOXFMYVTSLAQMO-UHFFFAOYSA-N 2-Pyridinemethanamine Chemical class NCC1=CC=CC=N1 WOXFMYVTSLAQMO-UHFFFAOYSA-N 0.000 description 1
- 239000005906 Imidacloprid Substances 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 239000003899 bactericide agent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000012847 fine chemical Substances 0.000 description 1
- 235000013373 food additive Nutrition 0.000 description 1
- 239000002778 food additive Substances 0.000 description 1
- 239000004009 herbicide Substances 0.000 description 1
- 229940056881 imidacloprid Drugs 0.000 description 1
- YWTYJOPNNQFBPC-UHFFFAOYSA-N imidacloprid Chemical compound [O-][N+](=O)\N=C1/NCCN1CC1=CC=C(Cl)N=C1 YWTYJOPNNQFBPC-UHFFFAOYSA-N 0.000 description 1
- 238000005470 impregnation Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229960002715 nicotine Drugs 0.000 description 1
- SNICXCGAKADSCV-UHFFFAOYSA-N nicotine Natural products CN1CCCC1C1=CC=CN=C1 SNICXCGAKADSCV-UHFFFAOYSA-N 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 150000002910 rare earth metals Chemical class 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000009885 systemic effect Effects 0.000 description 1
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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
- B01J29/00—Catalysts comprising molecular sieves
- B01J29/03—Catalysts comprising molecular sieves not having base-exchange properties
- B01J29/0308—Mesoporous materials not having base exchange properties, e.g. Si-MCM-41
- B01J29/0341—Mesoporous materials not having base exchange properties, e.g. Si-MCM-41 containing arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
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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
- B01J29/00—Catalysts comprising molecular sieves
- B01J29/03—Catalysts comprising molecular sieves not having base-exchange properties
- B01J29/0308—Mesoporous materials not having base exchange properties, e.g. Si-MCM-41
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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
- B01J29/03—Catalysts comprising molecular sieves not having base-exchange properties
- B01J29/0308—Mesoporous materials not having base exchange properties, e.g. Si-MCM-41
- B01J29/0316—Mesoporous materials not having base exchange properties, e.g. Si-MCM-41 containing iron group metals, noble metals or copper
- B01J29/0333—Iron group metals or copper
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D213/00—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members
- C07D213/02—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members
- C07D213/04—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members having no bond between the ring nitrogen atom and a non-ring member or having only hydrogen or carbon atoms directly attached to the ring nitrogen atom
- C07D213/06—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members having no bond between the ring nitrogen atom and a non-ring member or having only hydrogen or carbon atoms directly attached to the ring nitrogen atom containing only hydrogen and carbon atoms in addition to the ring nitrogen atom
- C07D213/08—Preparation by ring-closure
- C07D213/09—Preparation by ring-closure involving the use of ammonia, amines, amine salts, or nitriles
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D213/00—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members
- C07D213/02—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members
- C07D213/04—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members having no bond between the ring nitrogen atom and a non-ring member or having only hydrogen or carbon atoms directly attached to the ring nitrogen atom
- C07D213/06—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members having no bond between the ring nitrogen atom and a non-ring member or having only hydrogen or carbon atoms directly attached to the ring nitrogen atom containing only hydrogen and carbon atoms in addition to the ring nitrogen atom
- C07D213/16—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members having no bond between the ring nitrogen atom and a non-ring member or having only hydrogen or carbon atoms directly attached to the ring nitrogen atom containing only hydrogen and carbon atoms in addition to the ring nitrogen atom containing only one pyridine ring
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Abstract
本发明公开了一种新型甲基吡啶催化剂的制备的方法，包括如下步骤：步骤1：将水、浓盐酸、P123于25‑50℃搅拌0.5‑4h；步骤2：在所得溶液中缓慢滴加TEOS，滴加时间为10‑24h，再加入含有金属离子的硅酸盐和复合硅酸盐溶液，并将上述溶液搅拌24‑48h，得到乳白色悬浊液；步骤3：将上述悬浊液转入自压釜中60‑120℃晶华24‑48h，抽滤，40‑70℃烘干；步骤4：得到含有金属离子负载的SBA‑15分子筛催化剂，并置于马沸炉内450‑650℃高温煅烧活化催化剂，活化时间为2‑6h。本发明通过一步法于SBA‑15介孔分子筛中负载金属离子，制备得到新型催化合成甲基吡啶的催化剂，催化得到甲基吡啶的选择性和转化率高，催化剂的热稳定性高以及催化有效寿命长。
Description
技术领域
本发明涉及催化剂制备技术领域，具体为一种新型甲基吡啶催化剂的制备的方法。
背景技术
甲基吡啶是三药及三药中间体的关键共性化合物，也是日用化工、饲料、食品添加剂、子午轮胎工业的重要原料。其中3-甲基吡啶及其衍生物是重要的化工原料或有机中间体，广泛应用于农药、医药等精细化工行业。以3-甲基吡啶及其衍生物开发的农药中，有超高效的杀虫剂、除草剂，还出现了高效的杀菌剂，并逐渐形成了一大类特有的农药系列。特别值得提及的是近年开发的与烟碱作用机理一致的以吡虫啉为代表的吡啶甲胺类化合物，此类化合物以其具有的内吸、广谱、高效等特点已成为国内外农药界研究开发的热点。
专利CN201410764200.4公开一种3-甲基吡啶制吡啶催化剂及其制备方法，通过ZSM11分子筛和稀土Y分子筛等制备合成吡啶以及3-甲基吡啶的催化剂；专利CN200310117024.7公开一种负载型合成甲基吡啶催化剂的制备方法，采用磷酸盐和复合磷酸盐负载于硅球载体上，用浸渍法负载金属离子的方法制备合成甲基吡啶的催化剂。上述两者中载体为ZSM11和硅球的催化剂，在催化剂的重复使用率以及催化剂的寿命均较为短暂，催化合成3-甲基吡啶的转化率以及收率均偏低。
发明内容
本发明的目的在于提供一种新型甲基吡啶催化剂的制备的方法，一步法于SBA-15介孔分子筛中负载金属离子，制备得到新型催化合成甲基吡啶的催化剂，催化得到甲基吡啶的选择性和转化率高，催化剂的热稳定性高以及催化有效寿命长，以解决上述背景技术中提出的问题。
为实现上述目的，本发明提供如下技术方案：一种新型甲基吡啶催化剂的制备的方法，包括如下步骤：
步骤1：将水、浓盐酸、P123于25-50℃搅拌0.5-4h；
步骤2：在所得溶液中缓慢滴加TEOS，滴加时间为10-24h，再加入含有金属离子的硅酸盐和复合硅酸盐溶液，并将上述溶液搅拌24-48h，得到乳白色悬浊液；
步骤3：将上述悬浊液转入自压釜中60-120℃晶华24-48h，抽滤，40-70℃烘干；
步骤4：得到含有金属离子负载的SBA-15分子筛催化剂，并置于马沸炉内450-650℃高温煅烧活化催化剂，活化时间为2-6h。
进一步地，所述硅酸盐和复合硅酸盐用量为SBA-15分子筛载体重量的1％-40％。
进一步地，所述P123、水、浓盐酸、TEOS反应质量比为2:50:25:10。
进一步地，所述硅酸盐由硅酸锰、硅酸镁、硅酸钴、硅酸锌、硅酸铝中的两种以上复合。
进一步地，所述硅酸盐是两种以上的硅酸盐复合，其配方和比例为：
硅酸锰：硅酸铝复合，其摩尔比为1:0.05-1；
硅酸镁：硅酸铝复合，其摩尔比为1:0.05-1；
硅酸钴：硅酸铝复合，其摩尔比为1:0.05-1；
硅酸锌：硅酸铝复合，其摩尔比为1:0.05-1。
与现有技术相比，本发明的有益效果是：
本发明通过一步法于SBA-15介孔分子筛中负载金属离子，制备得到新型催化合成甲基吡啶的催化剂，催化得到甲基吡啶的选择性和转化率高，催化剂的热稳定性高以及催化有效寿命长。
具体实施方式
以下将详细说明本发明实施例，然而，本发明实施例并不以此为限。基于本发明中的实施例，本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例，都属于本发明保护的范围。
实施例1
将4.0gP123、100g水、25g浓盐酸于40℃搅拌3h；在所得溶液中缓慢滴加10.0gTEOS，滴加时间为20h，将硅酸铝和硅酸锰盐溶液加入其中，并将上述溶液搅拌24h，得到乳白色悬浊液；将上述悬浊液转入自压釜中90℃晶华24h，抽滤，70℃烘干；得到含有金属离子负载的SBA-15分子筛催化剂，并置于马沸炉内450℃高温煅烧活化催化剂，活化时间为4h。其中硅酸铝和硅酸锰盐溶液摩尔比为1:1(mol)，用量为总体系质量的15％。
实施例2
将5.5gP123、120g水、30g浓盐酸于40℃搅拌2h；在所得溶液中缓慢滴加11.0gTEOS，滴加时间为24h，将硅酸铝和硅酸锌盐溶液加入其中，并将上述溶液搅拌24h，得到乳白色悬浊液；将上述悬浊液转入自压釜中90℃晶华24h，抽滤，70℃烘干；得到含有金属离子负载的SBA-15分子筛催化剂，并置于马沸炉内450℃高温煅烧活化催化剂，活化时间为4h。其中硅酸铝和硅酸锌盐溶液摩尔比为1:1(mol)，用量为总体系质量的20％。
实施例3
将5gP123、100g水、50g浓盐酸于25℃搅拌4h；在所得溶液中缓慢滴加10.0gTEOS，滴加时间为18h，将硅酸镁和硅酸铝盐溶液加入其中，并将上述溶液搅拌48h，得到乳白色悬浊液；将上述悬浊液转入自压釜中60℃晶华36h，抽滤，40℃烘干；得到含有金属离子负载的SBA-15分子筛催化剂，并置于马沸炉内550℃高温煅烧活化催化剂，活化时间为2h。其中硅酸铝和硅酸锌盐溶液摩尔比为1:1(mol)，用量为总体系质量的30％。
实施例4
将6gP123、125g水、60g浓盐酸于50℃搅拌2h；在所得溶液中缓慢滴加12.0gTEOS，滴加时间为10h，将硅酸钴和硅酸铝盐溶液加入其中，并将上述溶液搅拌24h，得到乳白色悬浊液；将上述悬浊液转入自压釜中120℃晶华48h，抽滤，70℃烘干；得到含有金属离子负载的SBA-15分子筛催化剂，并置于马沸炉内650℃高温煅烧活化催化剂，活化时间为6h。其中硅酸铝和硅酸锌盐溶液摩尔比为1:1(mol)，用量为总体系质量的40％。
本发明采用一步法将硅酸盐和复合硅酸盐负载在SBA-15分子筛载体溶胶上，催化醛氨反应生成3-甲基吡啶和吡啶，大大提高了3-甲基吡啶的转化率和收率，催化剂的稳定性和催化寿命显著提高。
尽管已经示出和描述了本发明的实施例，对于本领域的普通技术人员而言，可以理解在不脱离本发明的原理和精神的情况下可以对这些实施例进行多种变化、修改、替换和变型，本发明的范围由所附权利要求及其等同物限定。
Claims (5)
1.一种新型甲基吡啶催化剂的制备的方法，其特征在于，包括如下步骤：
步骤1：将水、浓盐酸、P123于25-50℃搅拌0.5-4h；
步骤2：在所得溶液中缓慢滴加TEOS，滴加时间为10-24h，再加入含有金属离子的硅酸盐和复合硅酸盐溶液，并将上述溶液搅拌24-48h，得到乳白色悬浊液；
步骤3：将上述悬浊液转入自压釜中60-120℃晶华24-48h，抽滤，40-70℃烘干；
步骤4：得到含有金属离子负载的SBA-15分子筛催化剂，并置于马沸炉内450-650℃高温煅烧活化催化剂，活化时间为2-6h。
2.根据权利要求1所述的新型甲基吡啶催化剂的制备的方法，其特征在于，所述硅酸盐和复合硅酸盐用量为SBA-15分子筛载体重量的1％-40％。
3.根据权利要求1所述的新型甲基吡啶催化剂的制备的方法，其特征在于，所述P123、水、浓盐酸、TEOS反应质量比为2:50:25:10。
4.根据权利要求1所述的新型甲基吡啶催化剂的制备的方法，其特征在于，所述硅酸盐由硅酸锰、硅酸镁、硅酸钴、硅酸锌、硅酸铝中的两种以上复合。
5.根据权利要求4所述的新型甲基吡啶催化剂的制备的方法，其特征在于，所述硅酸盐是两种以上的硅酸盐复合，其配方和比例为：
硅酸锰：硅酸铝复合，其摩尔比为1:0.05-1；
硅酸镁：硅酸铝复合，其摩尔比为1:0.05-1；
硅酸钴：硅酸铝复合，其摩尔比为1:0.05-1；
硅酸锌：硅酸铝复合，其摩尔比为1:0.05-1。
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102992932A (zh) * | 2012-11-28 | 2013-03-27 | 浙江工业大学 | 利用m-sba-15型介孔分子筛脱除芳烃中烯烃的方法 |
| CN103406138A (zh) * | 2013-02-06 | 2013-11-27 | 华南师范大学 | 用于臭氧氧化的高稳定性过渡金属改性sba-15催化剂的制备方法 |
| CN106927476A (zh) * | 2015-12-30 | 2017-07-07 | 中国石油天然气股份有限公司 | Mo-SBA-15分子筛及加氢催化剂的制备方法 |
| JP2018202389A (ja) * | 2017-05-31 | 2018-12-27 | 古河電気工業株式会社 | アルキレート製造用触媒構造体、該触媒構造体を有するアルキレート製造装置及びアルキレート製造用触媒構造体の製造方法 |
| CN110668458A (zh) * | 2018-07-02 | 2020-01-10 | 国家能源投资集团有限责任公司 | Al-SBA-15介孔分子筛和脱硝催化剂及各自的制备方法和应用 |
| CN111151291A (zh) * | 2020-01-21 | 2020-05-15 | 山东玉皇化工有限公司 | 一种介孔分子筛催化剂的制备方法及应用 |
-
2020
- 2020-07-10 CN CN202010662908.4A patent/CN111760584A/zh active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102992932A (zh) * | 2012-11-28 | 2013-03-27 | 浙江工业大学 | 利用m-sba-15型介孔分子筛脱除芳烃中烯烃的方法 |
| CN103406138A (zh) * | 2013-02-06 | 2013-11-27 | 华南师范大学 | 用于臭氧氧化的高稳定性过渡金属改性sba-15催化剂的制备方法 |
| CN106927476A (zh) * | 2015-12-30 | 2017-07-07 | 中国石油天然气股份有限公司 | Mo-SBA-15分子筛及加氢催化剂的制备方法 |
| JP2018202389A (ja) * | 2017-05-31 | 2018-12-27 | 古河電気工業株式会社 | アルキレート製造用触媒構造体、該触媒構造体を有するアルキレート製造装置及びアルキレート製造用触媒構造体の製造方法 |
| CN110668458A (zh) * | 2018-07-02 | 2020-01-10 | 国家能源投资集团有限责任公司 | Al-SBA-15介孔分子筛和脱硝催化剂及各自的制备方法和应用 |
| CN111151291A (zh) * | 2020-01-21 | 2020-05-15 | 山东玉皇化工有限公司 | 一种介孔分子筛催化剂的制备方法及应用 |
Non-Patent Citations (1)
| Title |
|---|
| 高闯等: "硅铝摩尔比对Al-SBA-15介孔分子筛结构和性质的影响", 《石油化工》 * |
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