WO2008019585A1 - Procédé de modification d'un tamis moléculaire à micropores de silicoaluminium phosphate au moyen d'un métal - Google Patents

Procédé de modification d'un tamis moléculaire à micropores de silicoaluminium phosphate au moyen d'un métal Download PDF

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Publication number
WO2008019585A1
WO2008019585A1 PCT/CN2007/002349 CN2007002349W WO2008019585A1 WO 2008019585 A1 WO2008019585 A1 WO 2008019585A1 CN 2007002349 W CN2007002349 W CN 2007002349W WO 2008019585 A1 WO2008019585 A1 WO 2008019585A1
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WIPO (PCT)
Prior art keywords
molecular sieve
modified
metal
sap0
sapo
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PCT/CN2007/002349
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English (en)
Chinese (zh)
Inventor
Peng Tian
Zhongmin Liu
Lei Xu
Lixin Yang
Yue Yang
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Dalian Institute Of Chemical Physics, Chinese Academy Of Sciences
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Publication of WO2008019585A1 publication Critical patent/WO2008019585A1/fr

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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
    • B01J29/82—Phosphates
    • B01J29/84—Aluminophosphates containing other elements, e.g. metals, boron
    • B01J29/85—Silicoaluminophosphates [SAPO compounds]
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B39/00—Compounds having molecular sieve and base-exchange properties, e.g. crystalline zeolites; Their preparation; After-treatment, e.g. ion-exchange or dealumination
    • C01B39/54—Phosphates, e.g. APO or SAPO compounds
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C1/00—Preparation of hydrocarbons from one or more compounds, none of them being a hydrocarbon
    • C07C1/20—Preparation of hydrocarbons from one or more compounds, none of them being a hydrocarbon starting from organic compounds containing only oxygen atoms as heteroatoms
    • 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
    • B01J2229/12—After treatment, characterised by the effect to be obtained to alter the outside of the crystallites, e.g. selectivation
    • 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
    • B01J2229/20—After treatment, characterised by the effect to be obtained to introduce other elements in the catalyst composition comprising the molecular sieve, but not specially in or on the molecular sieve itself
    • 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
    • B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/02—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the alkali- or alkaline earth metals or beryllium
    • 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
    • B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/06—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of zinc, cadmium or mercury
    • 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
    • B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
    • B01J23/72—Copper
    • 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
    • B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
    • B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
    • B01J23/78—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with alkali- or alkaline earth metals
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C2529/00—Catalysts comprising molecular sieves
    • C07C2529/82—Phosphates
    • C07C2529/84—Aluminophosphates containing other elements, e.g. metals, boron
    • C07C2529/85—Silicoaluminophosphates (SAPO compounds)

Definitions

  • the invention relates to a metal modification method of a small pore phosphorus silicon aluminum molecular sieve, and a catalytic application of a metal modified molecular sieve catalyst in the reaction of converting oxygen compounds into low carbon olefins.
  • Low-carbon olefins are the basic raw materials for petrochemicals. With the development of the world economy, its demand is increasing year by year. The main route for the production of ethylene and propylene is currently through naphtha cracking. Because petroleum is a non-renewable resource with limited reserves, research and development of new low-carbon olefin production technologies is of great significance. Natural gas or coal by methanol The production of low-carbon olefins such as ethylene and propylene is the most promising alternative to the naphtha route to olefins.
  • SAPO-n phosphosilicate series molecular sieve
  • SAPO molecular sieves are a class of crystalline silicoaluminophosphates composed of tetrahedrons of P0 4 +, A10 4 — and Si0 4 .
  • SAPO molecular sieves with small pores and moderate acidity have been used for MTO reactions such as SAPO-17, SAPO-18, SAPO-34, SAPO-44, etc.
  • US4499327 their pore sizes are approximately It is a good type of shape-selective catalyst with 0.43nm.
  • SAPO-34 molecular sieve has become a hot spot in MTO reaction due to its suitable acidity and pore structure.
  • CN1167654A discloses the modification of SAPO-34 by using Cu, Co, Ni, Ca, Ba or Sr, and adding a binder and a pore former to prepare a catalyst for converting methanol or dimethyl ether into a lower olefin.
  • the metal is introduced into the SAPO-34 molecular sieve by direct in situ synthesis or impregnation, and the mass of the metal in the molecular sieve is 0.01-0.15%.
  • CN1216941A reports the use of calcium, strontium and barium and mixtures thereof to modify small pore molecular sieves and their use in the conversion of oxygenates.
  • the modification method of the molecular sieve of the patent is divided into two types, one is direct in-situ synthesis, and the other is to modify the synthesized molecular sieve raw powder by the impregnation method.
  • US4752651 Non-zeolite small pore molecular sieves have been reported to be modified with alkaline earth metals strontium and magnesium.
  • JP 940 74 134 discloses a process for alkaline earth metal modified molecular sieves which refers to a molecular sieve pore size between macroporous zeolites such as X and Y zeolites and small pore molecular sieves such as erionite and chabazite.
  • US2004224839 reports a process for modifying calcined SAPO molecular sieves such as SAPO-34 using organometallic reagents. Summary of the invention
  • the technical solution of the present invention is to provide a metal modification method for a small-porous phosphosilica molecular sieve, which comprises impregnating or mechanically grinding a compound containing an alkali metal and/or a transition metal with a small hole.
  • the original powder of the phosphorus silicon aluminum molecular sieve is mixed to prepare a modified molecular sieve.
  • the small pore phosphosilica molecular sieve is one or a mixture of SAPO-17, SAPO-18, SAPO-34, SAPO-44, SAPO-35, and SAPO-56.
  • the alkali metal-containing source is one or a mixture of oxides, inorganic salts or organic salts of calcium, barium or strontium; the source of the transition metal is copper or zinc.
  • the modified molecular sieve prepared by the high-temperature calcination removal of the template has a mass content of 0.1-5 %.
  • the modified molecular sieve prepared by the high-temperature calcination removal of the templating agent has a metal content of 0.5-3%.
  • the preparation method is as follows: a) hydrothermal synthesis of small pores SAPO molecular sieve, drying at 100-120 ° C, to obtain molecular sieve raw powder;
  • modified small pore SAPO molecular sieve obtained in the step b) is dried at 120 ° C, and calcined in air at 500-700 ° C for 3-8 hours to obtain a modified SAPO molecular sieve catalyst.
  • the modified molecular sieve catalyst obtained by the method of the invention can be applied to the conversion of oxygenates to olefins, and the modified molecular sieves exhibit higher initial selectivity of lower olefins than unmodified molecular sieves.
  • the method of the invention adopts a method of impregnation or mechanical grinding to mix a compound containing an alkali metal (calcium, barium or strontium) and/or a transition metal (copper or zinc) with a small-porous phosphosilica molecular sieve raw powder (such as SAPO-34). Mixing, preparing modified molecular sieves.
  • a compound containing an alkali metal calcium, barium or strontium
  • a transition metal copper or zinc
  • the invention is characterized in that the small pore silicon aluminum molecular sieve used is one or a mixture of any one of SAPO-17, SAPO-18, SAPO-34, SAPO-44, SAPO-35, SAPO-56.
  • step b) The modified pores obtained in step b) are dried at 120 ° C and calcined in air at 500-700 ° C.
  • the modified SAPO molecular sieve catalyst was obtained in 3-8 hours.
  • the present invention is characterized in that the source of the metal used is one or a mixture of oxides, inorganic salts or organic salts of calcium, barium, strontium, copper or zinc. After the modified molecular sieve is calcined at a high temperature to remove the templating agent, the metal content thereof is 0.1-5%.
  • the invention is described in detail below by way of examples.
  • the modified SAPO-34 molecular sieve catalyst obtained in Example 1-4 was used for methanol to olefin catalytic reaction, and the unmodified SAPO-34 molecular sieve raw powder was calcined and the template was also calcined to evaluate the reaction.
  • Reaction conditions 2.5 g of a sample of 20-40 mesh granule catalyst was charged into a reactor, activated by nitrogen at 550 ° C for 1 hour, and then cooled to 50 (TC was carried out. The nitrogen was used as a diluent gas to carry the raw material methanol, nitrogen flow rate The molecular weight of the methanol was 2.01 ⁇ at 40 ml/min.
  • the composition of the reaction product was analyzed by on-line gas chromatography, and the results are shown in Table 1.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Materials Engineering (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Geology (AREA)
  • Inorganic Chemistry (AREA)
  • Catalysts (AREA)
  • Silicates, Zeolites, And Molecular Sieves (AREA)

Abstract

Procédé de modification d'un tamis moléculaire à micropores de silicoaluminium phosphate au moyen d'un métal. Ce procédé consiste à mélanger une poudre de tamis moléculaires de silicoaluminium phosphate, tel que SAPO-34, avec un composé alcalino-terreux (CA, Sr ou Ba) et/ou un métal de transition (Cu iz Zn) par un procédé d'immersion ou par broyage. Ainsi modifié, le tamis moléculaire peut s'utiliser comme catalyseur pour transformer des charges de produits oxygénées en oléfines et présente pour les oléfines à faible teneur en carbone une séléctivité initiale plus élevée que des tamis moléculaires non modifiés.
PCT/CN2007/002349 2006-08-08 2007-08-06 Procédé de modification d'un tamis moléculaire à micropores de silicoaluminium phosphate au moyen d'un métal WO2008019585A1 (fr)

Applications Claiming Priority (4)

Application Number Priority Date Filing Date Title
CN200610089170 2006-08-08
CN200610089170.7 2006-08-08
CN200610160685.1 2006-12-04
CNA2006101606851A CN101121532A (zh) 2006-08-08 2006-12-04 一种小孔磷硅铝分子筛的金属改性方法

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US7601662B2 (en) 2007-02-27 2009-10-13 Basf Catalysts Llc Copper CHA zeolite catalysts
US7998423B2 (en) 2007-02-27 2011-08-16 Basf Corporation SCR on low thermal mass filter substrates
US8293199B2 (en) 2009-12-18 2012-10-23 Basf Corporation Process for preparation of copper containing molecular sieves with the CHA structure, catalysts, systems and methods
US8293198B2 (en) 2009-12-18 2012-10-23 Basf Corporation Process of direct copper exchange into Na+-form of chabazite molecular sieve, and catalysts, systems and methods
US8603432B2 (en) 2007-04-26 2013-12-10 Paul Joseph Andersen Transition metal/zeolite SCR catalysts
US8617474B2 (en) 2008-01-31 2013-12-31 Basf Corporation Systems utilizing non-zeolitic metal-containing molecular sieves having the CHA crystal structure
CN108262068A (zh) * 2017-01-04 2018-07-10 中国石油化工股份有限公司 含氧物制低碳烯烃的方法
US10583424B2 (en) 2008-11-06 2020-03-10 Basf Corporation Chabazite zeolite catalysts having low silica to alumina ratios
CN112250087A (zh) * 2020-11-08 2021-01-22 江西苏克尔新材料有限公司 一种金属改性的sapo-34分子筛的制备方法及应用
CN115672393A (zh) * 2021-07-28 2023-02-03 国家能源投资集团有限责任公司 甲醇转化制低碳烯烃用催化剂及其制备方法、甲醇转化制备低碳烯烃的方法
CN116493041A (zh) * 2023-05-30 2023-07-28 天津大沽化工股份有限公司 一种用于1,2-二氯乙烷制氯乙烯的复合催化剂及其制备方法
CN115672393B (zh) * 2021-07-28 2024-06-04 国家能源投资集团有限责任公司 甲醇转化制低碳烯烃用催化剂及其制备方法、甲醇转化制备低碳烯烃的方法

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CN101632939B (zh) * 2008-07-24 2015-07-29 中国石油化工股份有限公司 一种含磷酸硅铝分子筛的组合物、制备方法及其应用
CN105984876B (zh) * 2015-01-30 2018-06-29 中国科学院大连化学物理研究所 一种金属改性sapo分子筛的制备方法
CN106984364B (zh) * 2016-01-20 2020-03-17 中国科学院大连化学物理研究所 磷酸硅铝类分子筛原粉在分离/提取金属离子中的应用
CN106064823A (zh) * 2016-05-30 2016-11-02 中国天辰工程有限公司 一种改性sapo‑34分子筛的方法
CN107661776B (zh) * 2016-07-28 2020-06-09 中国科学院大连化学物理研究所 制备含铜和银双金属的sapo分子筛的方法及其应用
CN109926033B (zh) * 2019-04-15 2020-12-01 清华大学 改性小孔分子筛吸附剂及其制备方法和用途
CN110354874A (zh) * 2019-08-13 2019-10-22 南开大学 多孔结构的硅铝磷载体加氢催化剂的制备方法及在制备生物燃料中的应用
CN113751066B (zh) * 2020-06-05 2023-08-29 中国石油化工股份有限公司 合成气直接制备乙烯和丙烯的催化剂组合物及其用途
CN114713282B (zh) * 2021-01-05 2023-08-04 中国石油化工股份有限公司 一种甲醇制烯烃催化剂的改性方法
CN115228430B (zh) * 2021-04-23 2024-05-07 中国科学院大连化学物理研究所 一种丙烯吸附剂及其在丙烯/丙烷分离中的应用

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US9839905B2 (en) 2007-02-27 2017-12-12 Basf Corporation Copper CHA zeolite catalysts
US7998423B2 (en) 2007-02-27 2011-08-16 Basf Corporation SCR on low thermal mass filter substrates
US8119088B2 (en) 2007-02-27 2012-02-21 Basf Corporation SCR on low thermal mass filter substrates
US11845067B2 (en) 2007-02-27 2023-12-19 Basf Corporation Copper CHA zeolite catalysts
US11529619B2 (en) 2007-02-27 2022-12-20 Basf Corporation Copper CHA zeolite catalysts
US8404203B2 (en) 2007-02-27 2013-03-26 Basf Corporation Processes for reducing nitrogen oxides using copper CHA zeolite catalysts
US7601662B2 (en) 2007-02-27 2009-10-13 Basf Catalysts Llc Copper CHA zeolite catalysts
US10654031B2 (en) 2007-02-27 2020-05-19 Basf Corporation Copper CHA zeolite catalysts
US8735311B2 (en) 2007-02-27 2014-05-27 Basf Corporation Copper CHA zeolite catalysts
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US9656254B2 (en) 2007-02-27 2017-05-23 Basf Corporation Copper CHA zeolite catalysts
US8603432B2 (en) 2007-04-26 2013-12-10 Paul Joseph Andersen Transition metal/zeolite SCR catalysts
US11478748B2 (en) 2007-04-26 2022-10-25 Johnson Matthey Public Limited Company Transition metal/zeolite SCR catalysts
US10105649B2 (en) 2008-01-31 2018-10-23 Basf Corporation Methods utilizing non-zeolitic metal-containing molecular sieves having the CHA crystal structure
US8617474B2 (en) 2008-01-31 2013-12-31 Basf Corporation Systems utilizing non-zeolitic metal-containing molecular sieves having the CHA crystal structure
US10583424B2 (en) 2008-11-06 2020-03-10 Basf Corporation Chabazite zeolite catalysts having low silica to alumina ratios
US11660585B2 (en) 2008-11-06 2023-05-30 Basf Corporation Chabazite zeolite catalysts having low silica to alumina ratios
US8293198B2 (en) 2009-12-18 2012-10-23 Basf Corporation Process of direct copper exchange into Na+-form of chabazite molecular sieve, and catalysts, systems and methods
US8293199B2 (en) 2009-12-18 2012-10-23 Basf Corporation Process for preparation of copper containing molecular sieves with the CHA structure, catalysts, systems and methods
CN108262068A (zh) * 2017-01-04 2018-07-10 中国石油化工股份有限公司 含氧物制低碳烯烃的方法
CN112250087A (zh) * 2020-11-08 2021-01-22 江西苏克尔新材料有限公司 一种金属改性的sapo-34分子筛的制备方法及应用
CN115672393A (zh) * 2021-07-28 2023-02-03 国家能源投资集团有限责任公司 甲醇转化制低碳烯烃用催化剂及其制备方法、甲醇转化制备低碳烯烃的方法
CN115672393B (zh) * 2021-07-28 2024-06-04 国家能源投资集团有限责任公司 甲醇转化制低碳烯烃用催化剂及其制备方法、甲醇转化制备低碳烯烃的方法
CN116493041A (zh) * 2023-05-30 2023-07-28 天津大沽化工股份有限公司 一种用于1,2-二氯乙烷制氯乙烯的复合催化剂及其制备方法

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