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公开(公告)号：US09061954B2
公开(公告)日：2015-06-23
申请号：US12864966
申请日：2009-02-05
CPC分类号： C07C1/24 , B01J29/40 , B01J2229/16 , B01J2229/36 , B01J2229/37 , B01J2229/42 , C07C2529/40 , Y02P20/52 , C07C11/04
摘要： The present invention relates to a process for the dehydration of at least an alcohol to make at least an olefin, comprising: introducing in a reactor a stream (A) comprising at least an alcohol, optionally water, optionally an inert component, contacting said stream with a catalyst in said reactor at conditions effective to dehydrate at least a portion of the alcohol to make an olefin, recovering from said reactor an olefin containing stream (B), Wherein the catalyst is: a crystalline silicate having a ratio Si/Al of at least about 100, or a dealuminated crystalline silicate, or a phosphorus modified zeolite, the WHSV of the alcohols is at least 2 h−1, the temperature ranges from 280° C. to 500° C. It relates also to the same process as above but wherein the catalyst is a phosphorus modified zeolite and at any WHSV.The partial pressure of the alcohol in the dehydration reactor advantageously ranges from 1.2 to 4 bars absolute (0.12 MPa to 0.4 MPa), the temperature of the dehydration reactor ranges advantageously from 300° C. to 400° C. and the alcohol is selected among ethanol, propanol, butanol and phenylethanol.
摘要翻译： 本发明涉及一种使至少一种醇脱水以制备至少一种烯烃的方法，其包括：在反应器中引入至少包含醇，任选的水，任选的惰性组分的物流（A） 在有效使至少一部分醇脱水以制备烯烃的条件下在所述反应器中的催化剂，从所述反应器回收含烯烃的料流（B），其中所述催化剂是：具有Si / Al比率的结晶硅酸盐 至少约100个，或脱铝的结晶硅酸盐或磷改性沸石，醇的WHSV为至少2h -1，温度范围为280℃至500℃。它还涉及相同的方法 如上所述，但是其中催化剂是磷改性沸石并且在任何WHSV。 脱水反应器中的醇的分压有利地为1.2至4巴绝对压力（0.12MPa至0.4MPa），脱水反应器的温度有利地为300℃至400℃，醇选自 乙醇，丙醇，丁醇和苯乙醇。
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2.发明授权Use of phosphorus modified molecular sieves in conversion of organics to olefins 有权使用磷改性分子筛将有机物转化为烯烃公开(公告)号：US09035120B2
公开(公告)日：2015-05-19
申请号：US12671220
申请日：2008-07-28
CPC分类号： C07C1/20 , B01J29/40 , B01J37/28 , B01J2229/18 , B01J2229/37 , C07C1/322 , C07C4/06 , C07C2529/85 , C10G2400/20 , Y02P30/42 , C07C11/02
摘要： A method of making light olefins in a combined XTO (organics to olefins) and OCP (olefins cracking) process, from an oxygen-containing, halogenide-containing, or sulphur-containing organic feedstock contacted with a catalyst in a first reactor to convert the feedstock into a reactor effluent comprising light olefins and a heavy hydrocarbon fraction; separating the light olefins from the heavy hydrocarbon fraction, then contacting the heavy hydrocarbon fraction in a second reactor with a catalyst to convert a portion of the heavy hydrocarbons into light olefins; wherein the catalyst is a zeolite selected among a H+ or NH4+—form of MFI, MEL, FER, MOR, or clinoptilolite; modifying the zeolite by adding from 0.05 to 7 wt % of phosphorous to the zeolite, and an optional washing and/or drying in either order, then calcination. In an embodiment, the initial zeolite Si:Al atomic ratio of at least one catalyst is 100 or less.
摘要翻译： 在第一反应器中与含催化剂接触的含氧卤化物或含硫有机原料的组合XTO（有机物至烯烃）和OCP（烯烃裂解）方法中制备轻质烯烃的方法，以将 原料进入包含轻质烯烃和重质烃馏分的反应器流出物; 将轻质烯烃与重质烃馏分分离，然后使第二反应器中的重质烃馏分与催化剂接触，将一部分重质烃转化成轻质烯烃; 其中所述催化剂是选自MFI，MEL，FER，MOR或斜发沸石的H +或NH4 +形式的沸石; 通过向沸石添加0.05至7重量％的磷，并且任选地洗涤和/或干燥，然后煅烧来改性沸石。 在一个实施方案中，至少一种催化剂的初始沸石Si：Al原子比为100以下。
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公开(公告)号：US08957273B2
公开(公告)日：2015-02-17
申请号：US13000387
申请日：2009-06-24
IPC分类号： C07C1/20 , C07C1/24 , C07C1/26 , B01J21/08 , B01J21/16 , B01J27/14 , B01J29/18 , B01J29/40 , B01J29/65 , B01J29/90 , B01J38/12 , C07C1/32
CPC分类号： C07C1/20 , B01J21/08 , B01J21/16 , B01J27/14 , B01J29/18 , B01J29/40 , B01J29/65 , B01J29/90 , B01J38/12 , B01J2229/16 , B01J2229/18 , B01J2229/36 , B01J2229/37 , C07C1/26 , C07C1/322 , C07C4/06 , C07C2529/40 , Y02P20/584 , Y02P30/42 , C07C11/02
摘要： The present invention relates to a process to make light olefins, in a combined XTO-OC process, from an oxygen-containing, halogenide-containing or sulphur-containing organic feedstock comprising: a0) providing a first portion and a second portion of said oxygen-containing, halogenide-containing or sulphur-containing organic feedstock, a) providing a catalyst comprising zeolitic molecular sieves containing at least 10 membered ring pore openings or larger in their microporous structure, b) providing an XTO reaction zone, an OC reaction zone and a catalyst regeneration zone, said catalyst circulating in the three zones, such that at least a portion of the regenerated catalyst is passed to the OC reaction zone, optionally at least a portion of the catalyst in the OC reaction zone is passed to the XTO reaction zone and at least a portion of the catalyst in the XTO reaction zone is passed to the regeneration zone; c) contacting the first portion of said oxygen-containing, halogenide-containing or sulphur-containing organic feedstock in the XTO reactor with the catalyst at conditions effective to convert at least a portion of the feedstock to form a XTO reactor effluent comprising light olefins and a heavy hydrocarbon fraction; d) separating said light olefins from said heavy hydrocarbon fraction; e) contacting said heavy hydrocarbon fraction and the second portion of said oxygen-containing, halogenide-containing or sulphur-containing organic feedstock in the OC reactor with the catalyst at conditions effective to convert at least a portion of said heavy hydrocarbon fraction and oxygen-containing, halogenide-containing or sulphur-containing organic feedstock to light olefins.
摘要翻译： 本发明涉及一种在组合的XTO-OC方法中由含氧，含卤素或含硫有机原料制备轻质烯烃的方法，包括：a）提供所述氧气的第一部分和第二部分 a）提供包含在其微孔结构中含有至少10元环孔或更大孔沸石分子筛的催化剂，b）提供XTO反应区，OC反应区和 催化剂再生区，所述催化剂在三个区域中循环，使得至少一部分再生催化剂通入OC反应区，任选地将OC反应区中的至少一部分催化剂通入XTO反应 区域，并且XTO反应区中的至少一部分催化剂被传送到再生区; c）在有效地转化至少一部分原料以形成包含轻质烯烃的XTO反应器流出物的条件下，将XTO反应器中的含氧卤化物或含硫有机原料的第一部分与催化剂接触， 重质烃馏分; d）从所述重质烃馏分中分离出所述轻质烯烃; e）在OC反应器中将所述重质烃部分和第二部分所述含氧卤化物或含硫有机原料与所述催化剂接触，所述条件有效地将至少一部分所述重质烃部分和氧 - 含卤素或含硫有机原料转化成轻质烯烃。
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公开(公告)号：US08957272B2
公开(公告)日：2015-02-17
申请号：US13000368
申请日：2009-06-24
IPC分类号： C07C1/20 , C07C1/24 , B01J21/08 , B01J21/16 , B01J27/14 , B01J29/18 , B01J29/40 , B01J29/65 , B01J29/90 , B01J38/02 , B01J38/12 , C07C1/26 , C07C1/32
CPC分类号： C07C1/20 , B01J21/08 , B01J21/16 , B01J27/14 , B01J29/18 , B01J29/40 , B01J29/65 , B01J29/90 , B01J38/02 , B01J38/12 , B01J2229/16 , B01J2229/18 , B01J2229/36 , B01J2229/37 , C07C1/26 , C07C1/322 , C07C4/06 , C07C2529/40 , Y02P20/584 , Y02P30/42 , C07C11/02
摘要： The present invention relates to a process to make light olefins, in a combined XTO-OC process, from an oxygen-containing, halogenide-containing or sulphur-containing organic feedstock comprising: a0) providing a first portion and a second portion of said oxygen-containing, halogenide-containing or sulphur-containing organic feedstock, a) providing a catalyst comprising zeolitic molecular sieves containing at least 10 membered ring pore openings or larger in their microporous structure, b) providing an XTO reaction zone, an OC reaction zone and a catalyst regeneration zone, said catalyst circulating in the three zones, such that at least a portion of the regenerated catalyst is passed to the OC reaction zone, at least a portion of the catalyst in the OC reaction zone is passed to the XTO reaction zone and at least a portion of the catalyst in the XTO reaction zone is passed to the regeneration zone; c) contacting the first portion of said oxygen-containing, halogenide-containing or sulphur-containing organic feedstock in the XTO reactor with the catalyst at conditions effective to convert at least a portion of the feedstock to form a XTO reactor effluent comprising light olefins and a heavy hydrocarbon fraction; d) separating said light olefins from said heavy hydrocarbon fraction; e) contacting said heavy hydrocarbon fraction and the second portion of said oxygen-containing, halogenide-containing or sulphur-containing organic feedstock in the OC reactor with the catalyst at conditions effective to convert at least a portion of said heavy hydrocarbon fraction and oxygen-containing, halogenide-containing or sulphur-containing organic feedstock to light olefins.
摘要翻译： 本发明涉及一种在组合的XTO-OC方法中由含氧，含卤素或含硫有机原料制备轻质烯烃的方法，包括：a）提供所述氧气的第一部分和第二部分 a）提供包含在其微孔结构中含有至少10元环孔或更大孔沸石分子筛的催化剂，b）提供XTO反应区，OC反应区和 催化剂再生区，所述催化剂在三个区域中循环，使得至少一部分再生催化剂通过OC反应区，OC反应区中的至少一部分催化剂通入XTO反应区 并且将XTO反应区中的至少一部分催化剂送入再生区; c）在有效地转化至少一部分原料以形成包含轻质烯烃的XTO反应器流出物的条件下，将XTO反应器中的含氧卤化物或含硫有机原料的第一部分与催化剂接触， 重质烃馏分; d）从所述重质烃馏分中分离出所述轻质烯烃; e）在OC反应器中将所述重质烃部分和第二部分所述含氧卤化物或含硫有机原料与所述催化剂接触，所述条件有效地将至少一部分所述重质烃部分和氧 - 含卤素或含硫有机原料转化成轻质烯烃。
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公开(公告)号：US08883668B2
公开(公告)日：2014-11-11
申请号：US12671217
申请日：2008-07-28
IPC分类号： B01J29/06 , C01B33/24 , C07C1/32 , C07C1/26 , C01B39/02 , C07C1/20 , B01J29/85 , C10G3/00 , B01J29/40
CPC分类号： C07C1/322 , B01J29/40 , B01J29/85 , B01J2229/36 , B01J2229/37 , C01B39/026 , C07C1/20 , C07C1/22 , C07C1/26 , C07C2/06 , C07C4/06 , C07C7/04 , C07C2529/85 , C10G3/00 , C10G2300/202 , C10G2300/4081 , C10G2400/20 , Y02P20/52 , Y02P30/20 , Y02P30/42 , C07C11/02 , C07C11/06
摘要： The present invention is a phosphorous modified zeolite (A) made by a process comprising in that order: selecting a zeolite with low Si/Al ratio (advantageously lower than 30) among H+ or NH4+-form of MFI, MEL, FER, MOR, clinoptilolite, said zeolite having been made preferably without direct addition of organic template; steaming at a temperature ranging from 400 to 870° C. for 0.01-200 h; leaching with an aqueous acid solution containing the source of P at conditions effective to remove a substantial part of Al from the zeolite and to introduce at least 0.3 wt % of P; separation of the solid from the liquid; an optional washing step or an optional drying step or an optional drying step followed by a washing step; a calcination step. The present invention also relates to a process (hereunder referred as “XTO process”) for making an olefin product from an oxygen-containing, halogenide-containing or sulphur-containing organic feedstock wherein said oxygen-containing, halogenide-containing or sulphur-containing organic feedstock is contacted with the above catalyst (in the XTO reactor) under conditions effective to convert at least a portion of the oxygen-containing, halogenide-containing or sulphur-containing organic feedstock to olefin products (the XTO reactor effluent).The present invention also relates to a process (hereunder referred as “combined XTO and OCP process”) to make light olefins from an oxygen-containing, halogenide-containing or sulphur-containing organic feedstock comprising : contacting said oxygen-containing, halogenide-containing or sulphur-containing organic feedstock in the XTO reactor with the above catalyst at conditions effective to convert at least a portion of the feedstock to form an XTO reactor effluent comprising light olefins and a heavy hydrocarbon fraction; separating said light olefins from said heavy hydrocarbon fraction; contacting said heavy hydrocarbon fraction in the OCP reactor at conditions effective to convert at least a portion of said heavy hydrocarbon fraction to light olefins.
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6.发明授权Process to make propylene from ethylene and either dimethyl ether, or methanol and dimethyl ether 有权从乙烯和二甲醚或甲醇和二甲醚制备丙烯的方法公开(公告)号：US08716543B2
公开(公告)日：2014-05-06
申请号：US13581817
申请日：2011-03-15
申请人： Pieter Struelens , Pierre Jacobs , Nikolai Nesterenko , Delphine Minoux , Sander Van Donk , Jean-Pierre Dath
发明人： Pieter Struelens , Pierre Jacobs , Nikolai Nesterenko , Delphine Minoux , Sander Van Donk , Jean-Pierre Dath
IPC分类号： C07C1/20
摘要： A process to make propylene can include providing a reaction zone containing a catalyst and introducing a feedstock into the reaction zone. The catalyst can be an acid. The feedstock can include ethylene, dimethyl ether or methanol and dimethyl ether with at least 1000 wppm of dimethyl ether, and optionally steam. The feedstock can be contacted with the catalyst at temperature and pressure conditions to produce an effluent, including propylene, hydrocarbons, steam, optionally unconverted methanol and/or unconverted dimethyl ether and optionally unconverted ethylene. The temperature at the inlet of the reaction zone can be under 280° C., such as from 50 to 280° C. The effluent can be sent to a fractionation zone to recover propylene, optionally methanol, dimethyl ether and optionally ethylene. At least a part of methanol, dimethyl ether, and ethylene can be recycled to the reaction zone at step b).
摘要翻译： 制备丙烯的方法可以包括提供含有催化剂并将原料引入反应区的反应区。 催化剂可以是酸。 原料可以包括具有至少1000wppm二甲醚的乙烯，二甲醚或甲醇和二甲醚，以及任选的蒸汽。 原料可以在温度和压力条件下与催化剂接触以产生流出物，包括丙烯，烃，蒸气，任选未转化的甲醇和/或未转化的二甲醚和任选的未转化的乙烯。 反应区入口处的温度可以在280℃，例如50-280℃。流出物可以送到分馏区以回收丙烯，任选的甲醇，二甲醚和任选的乙烯。 甲醇，二甲醚和乙烯的至少一部分可以在步骤b）循环到反应区。
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7.发明申请SIMULTANEOUS DEHYDRATION AND SKELETAL ISOMERISATION OF ISOBUTANOL ON ACID CATALYSTS 有权ISOBUTANOL在酸性催化剂上的同时脱水和同位素同位素公开(公告)号：US20130204057A1
公开(公告)日：2013-08-08
申请号：US13582759
申请日：2011-03-15
CPC分类号： C07C1/24 , B01J29/85 , C07C5/2518 , C07C5/2775 , C07C11/08 , C07C11/09 , C07C2521/04 , C07C2529/40 , C07C2529/65 , C07C2529/70 , Y02P20/127
摘要： The present invention (in a first embodiment) relates to a process for the simultaneous dehydration and skeletal isomerisation of isobutanol to make substantially corresponding olefins, having the same number of carbons and consisting essentially of a mixture of n-butenes and iso-butene, said process comprising: a) introducing in a reactor a stream (A) comprising isobutanol, optionally water, optionally an inert component, b) contacting said stream with a catalyst in said reactor at conditions effective to dehydrate and skeletal isomerise at least a portion of the isobutanol to make a mixture of n- butenes and iso-butene, c) recovering from said reactor a stream (B), removing water, the inert component if any and unconverted isobutanol if any to get a mixture of n-butenes and iso-butene, Wherein, the WHSV of the isobutanol is at least 1 h−1 or the temperature is from 200° C. to 600° C. and the catalyst is capable to make simultaneously the dehydration and skeletal isomerization of butene. The catalyst is a crystalline silicate of the group FER, MWW, EUO, MFS, ZSM-48, MTT, MFI, MEL or TON having Si/Al higher than 10, or a dealuminated crystalline silicate of the group FER, MWW, EUO, MFS, ZSM-48, MTT, MFI, MEL or TON having Si/Al higher than 10, or a phosphorus modified crystalline silicate of the group FER, MWW, EUO, MFS, ZSM-48, MTT, MFI, MEL or TON having Si/Al higher than 10, or a silicoaluminaphosphate molecular sieve of the group AEL, or a silicated, zirconated or titanated or fluorinated alumina. Advantageously the stream (B) is fractionated in a step d) to produce a n-butenes stream (N) and to remove the essential part of isobutene optionally recycled with stream (A) to the dehydration/isomerization reactor of step b).
摘要翻译： 本发明（在第一个实施方案中）涉及同时脱水和骨架异构化异丁醇以制备具有相同数目的碳并基本上由正丁烯和异丁烯组成的基本相应的烯烃的方法，所述方法 方法包括：a）在反应器中引入包含异丁醇，任选的水，任选的惰性组分的物流（A），b）在所述反应器中使所述物流与催化剂接触，所述条件有效地脱水和骨架异构化至少部分 异丁醇以制备正丁烯和异丁烯的混合物，c）从所述反应器回收流（B），除去水，惰性组分（如果有的话）和未转化的异丁醇（如果有的话）以得到正丁烯和异丁烯的混合物， 丁烯，其中异丁醇的WHSV为至少1h-1或温度为200℃至600℃，并且催化剂能够同时进行bu的脱水和骨架异构化 泰恩 该催化剂是具有Si / Al大于10的FER，MWW，EUO，MFS，ZSM-48，MTT，MFI，MEL或TON的结晶硅酸盐，或FER，MWW，EUO等的脱铝结晶硅酸盐， 具有Si / Al大于10的MFS，ZSM-48，MTT，MFI，MEL或TON，或FER，MWW，EUO，MFS，ZSM-48，MTT，MFI，MEL或TON的磷改性结晶硅酸盐，其具有 Si / Al高于10，或AEL的硅铝磷酸盐分子筛，或硅化，锆酸化或钛酸化或氟化氧化铝。 有利地，在步骤d）中将流（B）分馏以产生正丁烯料流（N），并除去任选与料流（A）一起循环的异丁烯的主要部分至步骤b）的脱水/异构化反应器。
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8.发明授权Process for obtaining catalyst composites comprising MeAPO and their use in conversion of organics to olefins 失效用于获得包含MeAPO的催化剂复合物的方法及其在将有机物转化为烯烃中的用途公开(公告)号：US08450233B2
公开(公告)日：2013-05-28
申请号：US12811218
申请日：2009-01-23
CPC分类号： C07C1/32 , B01J29/005 , B01J29/40 , B01J29/85 , B01J2229/186 , B01J2229/42 , C07C1/20 , C07C1/22 , C07C1/26 , Y02P30/42 , C07C11/02
摘要： The present invention relates to a mixture comprising 0.01 to 30% by weight of at least one medium or large pore crystalline silicoaluminate, silicoaluminophosphate materials or silicoaluminate mesoporous molecular sieves (co-catalyst) (A) and respectively 99.99 to 70% by weight of at least a MeAPO molecular sieve. The present invention also relates to catalysts consisting of the above mixture or comprising the above mixture. The present invention also relates to a process (hereunder referred as “XTO process”) for making an olefin product from an oxygen-containing, halogenide-containing or sulphur-containing organic feedstock, wherein said oxygen-containing, halogenide-containing or sulphur-containing organic feedstock is contacted with the above catalyst (in the XTO reactor) under conditions effective to convert the oxygen-containing, halogenide-containing or sulphur-containing organic feedstock to olefin products (the XTO reactor effluent). The present invention also relates to a process (hereunder referred as “combined XTO and OCP process”) to make light olefins from an oxygen-containing, halogenide-containing or sulphur-containing organic feedstock comprising: contacting said oxygen-containing, halogenide-containing or sulphur-containing organic feedstock in the XTO reactor with the above catalyst at conditions effective to convert at least a portion of the feedstock to form an XTO reactor effluent comprising light olefins and a heavy hydrocarbon fraction; separating said light olefins from said heavy hydrocarbon fraction; and contacting said heavy hydrocarbon fraction in the OCP reactor at conditions effective to convert at least a portion of said heavy hydrocarbon fraction to light olefins.
摘要翻译： 本发明涉及包含0.01至30重量％的至少一种中等或大孔结晶硅铝酸盐，硅铝磷酸盐材料或硅铝酸盐介孔分子筛（助催化剂）（A）和分别为99.99至70重量％ 至少一种MeAPO分子筛。 本发明还涉及由上述混合物组成或包含上述混合物的催化剂。 本发明还涉及从含氧卤化物或含硫有机原料制备烯烃产物的方法（以下称为“XTO法”），其中所述含氧卤化物或含硫化合物的含硫或含硫有机原料， 含有有机原料的有机原料在有效将含氧卤化物或含硫有机原料转化为烯烃产物（XTO反应器流出物）的条件下与上述催化剂（在XTO反应器中）接触。 本发明还涉及从含氧的含卤化物或含硫有机原料制备轻质烯烃的方法（以下称为“组合的XTO和OCP方法”），包括：使含有氧的含卤素的 或含硫有机原料在具有上述催化剂的XTO反应器中，在有效地转化至少一部分原料以形成包含轻质烯烃和重质烃馏分的XTO反应器流出物的条件下; 将所述轻质烯烃与所述重质烃馏分分离; 并在有效将至少一部分所述重质烃馏分转化成轻质烯烃的条件下使OCP反应器中的所述重质烃馏分接触。
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9.发明申请METHOD FOR DISTILLATE PRODUCTION BY MEANS OF CATALYTIC OLIGOMERIZATION OF OLEFINS IN THE PRESENCE OF METHANOL AND/OR DIMETHYL ETHER 审中-公开通过在甲醇和/或二甲醚存在下烯烃催化低聚制备蒸馏法的方法公开(公告)号：US20120264989A1
公开(公告)日：2012-10-18
申请号：US13501413
申请日：2010-10-13
IPC分类号： C07C2/02
CPC分类号： C10G50/00 , C10G2300/1014 , C10G2300/1088 , C10G2300/4018 , C10G2300/4081 , C10G2400/22 , Y02P30/20
摘要： The invention relates to a process for producing distillate by oligomerization starting with a hydrocarbon-based charge in the presence of methanol and/or dimethyl ether, which may especially be of plant origin. By addition of an oxygenated compound, this process makes it possible to reduce the amounts of olefins whose chain length is too short to be exploited (typically C10, or even less) and to increase the yields of C10+ olefins.
摘要翻译： 本发明涉及一种通过在甲醇和/或二甲醚存在下由烃类电荷开始的低聚制备馏出物的方法，其可以特别是植物来源。 通过加入含氧化合物，该方法可以减少链长太短而不能开发（通常为C10或甚至更少）的烯烃的量，并提高C10 +烯烃的产率。
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公开(公告)号：US20110201861A1
公开(公告)日：2011-08-18
申请号：US12994567
申请日：2009-02-24
申请人： Metin Bulut , Pierre Jacobs , Delphine Minoux , Nikolai Nesterenko , Jean-Pierre Dath , Sander Van Donk
发明人： Metin Bulut , Pierre Jacobs , Delphine Minoux , Nikolai Nesterenko , Jean-Pierre Dath , Sander Van Donk
CPC分类号： B01J29/40 , B01J2229/62 , C01B37/005 , C01B39/02 , C01B39/023 , C01B39/38 , C01B39/40 , C07C2/864 , C07C2529/70 , C10G29/205 , C10G2300/70 , Y02P20/52 , C07C15/08
摘要： The present invention relates to a process for making a crystalline metallosilicate composition and comprising crystallites having an inner part (the core) and an outer part (the outer layer or shell) such that:the ratio Si/Metal is higher in the outer part than in the inner part, the crystallites have a continuous distribution of metal and silicon over the crystalline cross-section, said process comprising: a) providing an aqueous medium comprising OH− anions and a metal source, b) providing an aqueous medium comprising an inorganic source of silicon and optionally a templating agent, c) optionally providing a non aqueous liquid medium comprising optionally an organic source of silica, d) mixing the medium a), b) and the optional c) at conditions effective to partly crystallize the desired metallosilicate, e) cooling down the reaction mixture a)+b)+c) to about room temperature, f) decreasing the pH of the reaction mixture by at least 0.1 preferably by 0.3 to 4, more preferably by 0.5 to 3, g) subjecting the resulting mixture of step f) at conditions effective to continue the crystallization of the desired metallosilicate, h) recovering the desired metallosilicate, wherein at step d) in the mixture a)+b)+c), before crystallization, the ratio Si org/Si inorganic is
摘要翻译： 本发明涉及一种制备结晶金属硅酸盐组合物的方法，其包括具有内部（芯）和外部（外层或外壳）的微晶，使得外部部分的Si /金属比高于 在内部，微晶在结晶横截面上具有金属和硅的连续分布，所述方法包括：a）提供包含OH-阴离子和金属源的水性介质，b）提供包含无机的水性介质 硅源和任选的模板剂，c）任选地提供包含任选的二氧化硅有机源的非水性液体介质，d）在有效地使所需金属硅酸盐部分结晶的条件下，将介质a），b）和任选的c） e）将反应混合物a）+ b）+ c）冷却至约室温，f）将反应混合物的pH降低至少0.1，优选0.3至4，更优选0 g）使所得到的步骤f）的混合物在有效继续所需金属硅酸盐结晶的条件下进行; h）回收所需的金属硅酸盐，其中在混合物中的步骤d）a）+ b）+ c） 在结晶之前，Si org / Si无机的比例<0.3，有利地<0.2，优选为0，OH- / SiO 2的摩尔比为至少0.3，有利地为0.3至0.62，优选为0.31至0.61，更优选为0.32 至0.61，非常优选为0.33至0.6。
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