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1. 发明授权

US10464053B2 Method for making a catalyst comprising a phosphorous modified zeolite and use of said zeolite 有权
公开(公告)号：US10464053B2
公开(公告)日：2019-11-05
申请号：US14236750
申请日：2012-07-25
申请人： Nikolai Nesterenko , Delphine Minoux , Cindy Adam , Jean-Pierre Dath
发明人： Nikolai Nesterenko , Delphine Minoux , Cindy Adam , Jean-Pierre Dath
IPC分类号： B01J29/06 , B01J29/85 , B01J29/40 , B01J37/02 , B01J29/70 , B01J29/65 , B01J37/10 , B01J37/28 , C07C1/20 , C07C1/24 , C07C2/66 , C07C2/86 , C07C4/06 , C10G29/20 , C10G29/22 , C10G3/00 , B01J37/00 , C07C1/22 , C07C2/08
摘要： A method to make a phosphorus modified zeolite can include providing a zeolite having at least one ten member ring, making an ion-exchange, steaming the zeolite, and introducing phosphorus on the zeolite. The zeolite can be mixed with one or more binders and shaping additives, and then shaped. A metal can be introduced, and the catalyst can be washed, calcined, and steamed in an equilibration step. The steaming can be at performed at a steam severity (X) of at least about 2. The steaming can be performed at a temperature above 625° C. The catalyst can be used in alcohol dehydration, olefin cracking, MTO processes, and alkylation of aromatics by alcohols with olefins and/or alcohols.

2. 发明授权

US09056806B2 Process to make olefins from isobutanol 有权
标题翻译：从异丁醇制备烯烃的方法
公开(公告)号：US09056806B2
公开(公告)日：2015-06-16
申请号：US13813115
申请日：2011-07-08
申请人： Cindy Adam , Delphine Minoux , Nikolai Nesterenko , Sander Van Donk , Jean-Pierre Dath
发明人： Cindy Adam , Delphine Minoux , Nikolai Nesterenko , Sander Van Donk , Jean-Pierre Dath
IPC分类号： C07C1/22 , C07C1/20 , C07C4/06 , C07C11/06 , C07C2/12
CPC分类号： C07C1/24 , C07C1/20 , C07C1/22 , C07C2/12 , C07C4/06 , C07C11/06 , C07C29/00 , C07C2529/40 , C07C2529/85 , C08F210/02 , C08F210/06 , C12P7/16 , Y02P30/42
摘要： The present invention relates to a process for the conversion of an alcohols mixture (A) comprising about 20 w % to 100% isobutanol to make essentially propylene, comprising: a) introducing in a reactor (A) a stream comprising the mixture (A), mixed with a stream (D1) comprising olefins having 4 carbon atoms or more (C4+ olefins), optionally water, optionally an inert component, b) contacting said stream with a catalyst (A1) at a temperature above 500° C. in said reactor (A) at conditions effective to dehydrate at least a part of the isobutanol and other alcohols, if any, and make a cracking, c) recovering from said reactor (A) an effluent comprising: ethylene, propylene, water, optionally unconverted alcohols of the mixture (A), various hydrocarbons, and the optional inert component of step a), d) fractionating said effluent of step c) to produce at least an ethylene stream, a propylene stream, a fraction consisting essentially of hydrocarbons having 4 carbon atoms or more, water and the optional inert component of step a), optionally recycling ethylene in whole or in part at the inlet of the reactor (A), optionally recycling the fraction consisting essentially of hydrocarbons having 4 carbon atoms or more at the inlet of the reactor (A).
摘要翻译：本发明涉及一种将包含约20％至100％异丁醇的醇混合物（A）转化成基本上丙烯的方法，其包括：a）在反应器（A）中引入包含混合物（A）的料流，与包含具有4个或更多碳原子的烯烃（C 4 +烯烃），任选的水，任选的惰性组分的流（D1）混合，b）在所述的温度高于500℃的温度下使所述料流与催化剂（A1）接触反应器（A）在有效使至少一部分异丁醇和其它醇脱水的条件下（如果有的话）并且产生裂化，c）从所述反应器（A）回收包含乙烯，丙烯，水，任选未转化的醇混合物（A），各种烃和步骤a）的任选的惰性组分，d）将步骤c）的所述流出物分馏以产生至少一种乙烯流，丙烯料流，基本上由具有4碳原子的烃组成的馏分原子或更多，水和步骤a）的任选的惰性组分，任选地在反应器（A）的入口处全部或部分地循环乙烯，任选地在反应器（A）的入口处循环基本上由具有4个或更多碳原子的烃组成的馏分，。

3. 发明授权

US08981173B2 Method for making a catalyst comprising a phosphorus modified zeolite to be used in a MTO process 有权
标题翻译：制备催化剂的方法，该催化剂包含用于MTO工艺中的磷改性沸石
公开(公告)号：US08981173B2
公开(公告)日：2015-03-17
申请号：US13522623
申请日：2011-01-25
申请人： Nikolai Nesterenko , Sander Van Donk , Delphine Minoux , Jean-Pierre Dath
发明人： Nikolai Nesterenko , Sander Van Donk , Delphine Minoux , Jean-Pierre Dath
IPC分类号： C07C1/24 , B01J29/85 , B01J29/06 , B01J29/40 , B01J37/28 , C07C1/20 , B01J27/16 , B01J37/00
CPC分类号： C07C1/24 , B01J27/16 , B01J29/06 , B01J29/40 , B01J29/85 , B01J37/0009 , B01J37/0045 , B01J37/06 , B01J37/08 , B01J37/28 , B01J2229/18 , B01J2229/36 , B01J2229/37 , B01J2229/42 , C07C1/20 , C07C2529/40 , C07C2529/85 , C07C11/02
摘要： The present invention is the use of a catalyst in a MTO process to convert an alcohol or an ether into light olefins wherein said catalyst comprises a phosphorus modified zeolite and is made by a method comprising the following steps in this order, a) the essential portion of the phosphorus is introduced into a zeolite comprising at least one ten members ring in the structure, b) the phosphorus modified zeolite of step a) is mixed with at least a component selected among one or more binders, salts of alkali-earth metals, salts of rare-earth metals, clays and shaping additives, b)* making a catalyst body from mixture b), c) an optional drying step or an optional drying step followed by a washing step, d) a calcination step, d*) an optional washing step followed by drying, e) optionally a small portion of phosphorus is introduced in the course of step b) or b)* or at end of step b) or b)*.
摘要翻译：本发明是在MTO方法中使用催化剂将醇或醚转化为轻质烯烃，其中所述催化剂包含磷改性沸石，并通过包括以下步骤的方法制备：a）主要部分的磷被引入到在结构中包含至少一个十元环的沸石中，b）步骤a）的磷改性沸石与至少一种选自一种或多种粘合剂，碱土金属盐，稀土金属盐，粘土和成型添加剂，b）*从混合物b）制备催化剂体，c）任选的干燥步骤或任选的干燥步骤，然后洗涤步骤，d）煅烧步骤d *）任选的洗涤步骤然后干燥，e）在步骤b）或b）*或步骤b）或b）*的末端引入任选的少量磷。

4. 发明申请

US20140296599A1 Catalyst Comprising a Phosphorous Modified Zeolite and Having Partly an Alpo Structure 有权
标题翻译：包含磷改性沸石和部分Alpo结构的催化剂
公开(公告)号：US20140296599A1
公开(公告)日：2014-10-02
申请号：US14236765
申请日：2012-07-25
申请人： Nikolai Nesterenko , Delphine Minoux , Cindy Adam , Jean-Pierre Dath
发明人： Nikolai Nesterenko , Delphine Minoux , Cindy Adam , Jean-Pierre Dath
IPC分类号： B01J29/85 , C07C2/86 , C07C2/66 , C07C1/24 , C07C4/06
CPC分类号： C07C2/66 , B01J29/40 , B01J29/405 , B01J29/7049 , B01J29/85 , B01J35/1038 , B01J35/1061 , B01J35/1066 , B01J37/0009 , B01J37/10 , B01J37/28 , B01J2229/16 , B01J2229/183 , B01J2229/186 , B01J2229/36 , B01J2229/37 , B01J2229/40 , B01J2229/42 , C07C1/24 , C07C2/864 , C07C4/06 , C07C2529/40 , C07C2529/70 , C07C2529/80 , C07C2529/83 , C07C2529/85 , Y02P20/52 , Y02P30/42 , C07C11/04
摘要： A catalyst can include a phosphorus modified zeolite having partly an ALPO structure. The ALPO structure can be determined by a signal between 35-45 ppm in 27Al MAS NMR spectrum. The zeolite can include at least one ten member ring in the structure thereof. The catalyst can also include a binder and one or more metal oxides. The catalyst can be used in processes in the presence of steam at high temperatures, such as temperatures that are above 300° C. and up to 800° C. The catalyst can be used in alcohol dehydration, olefin cracking, MTO processes, and alkylation of aromatic compounds with olefins and/or alcohols.
摘要翻译：催化剂可以包括部分具有ALPO结构的磷改性沸石。 ALPO结构可以通过27Al MAS NMR光谱中35-45ppm之间的信号来确定。沸石可以在其结构中包括至少一个十元环。催化剂还可以包括粘合剂和一种或多种金属氧化物。该催化剂可以在高温存在下的工艺中使用，例如高于300℃和高达800℃的温度。催化剂可用于醇脱水，烯烃裂解，MTO工艺和烷基化的芳族化合物与烯烃和/或醇。

5. 发明申请

US20140243568A1 Method for Making a Catalyst Comprising a Phosphorous Modified Zeolite and Use of Said Zeolite 审中-公开
标题翻译：制备包含磷改性沸石的催化剂的方法和所述沸石的用途
公开(公告)号：US20140243568A1
公开(公告)日：2014-08-28
申请号：US14236736
申请日：2012-07-25
申请人： Nikolai Nesterenko , Delphine Minoux , Cindy Adam , Jean-Pierre Dath
发明人： Nikolai Nesterenko , Delphine Minoux , Cindy Adam , Jean-Pierre Dath
IPC分类号： B01J29/85 , C07C4/06 , C07C2/08 , C07C2/86 , C07C1/22
CPC分类号： B01J29/85 , B01J29/40 , B01J29/65 , B01J29/7023 , B01J29/7026 , B01J29/7038 , B01J29/7042 , B01J29/7046 , B01J37/0009 , B01J37/10 , B01J37/28 , B01J2229/36 , B01J2229/37 , B01J2229/42 , C07C1/20 , C07C1/22 , C07C1/24 , C07C2/08 , C07C2/66 , C07C2/864 , C07C4/06 , C07C2521/08 , C07C2527/14 , C07C2529/40 , C07C2529/65 , C10G3/49 , C10G29/205 , C10G29/22 , Y02P20/52 , Y02P30/42 , C07C11/04 , C07C11/06 , C07C11/08 , C07C15/46 , C07C15/08
摘要： A method to make a phosphorus modified zeolite can include providing a zeolite including at least one ten member ring in the structure steaming the zeolite, mixing the zeolite with one or more binders and shaping additives, and then shaping the mixture. The method can include making a ion-exchange. The shaped mixture can be steamed. Phosphorous can be introduced on the catalyst to introduce at least 0.1 wt % of phosphorus, such as be dry impregnation or chemical vapor deposition. A metal, such as calcium, can be introduced. The catalyst can be washed, calcinated, and then steamed. The steaming severity (X) can be at least about 2. The catalyst can be steamed at a temperature above 625° C., such as a temperature ranging from 700 to 800° C. The catalyst can be used in alcohol dehydration, olefin cracking, MTO processes, and alkylation of aromatics by alcohols with olefins and/or alcohols.
摘要翻译：制备磷改性沸石的方法可以包括提供在蒸汽沸石的结构中包括至少一个十元环的沸石，将沸石与一种或多种粘合剂和成型添加剂混合，然后使混合物成型。该方法可以包括进行离子交换。成型的混合物可以蒸。可以在催化剂上引入磷以引入至少0.1重量％的磷，例如干浸渍或化学气相沉积。可以引入金属，如钙。催化剂可以洗涤，煅烧，然后蒸。蒸汽浓度（X）可以至少约为2.催化剂可以在高于625℃的温度下蒸煮，例如700-800℃的温度。催化剂可用于醇脱水，烯烃裂解，MTO方法，以及通过醇与烯烃和/或醇烷基化芳族化合物。

6. 发明申请

US20140194662A1 Method for Making a Catalyst Comprising a Phosphorous Modified Zeolite and Use of Said Zeolite 审中-公开
标题翻译：制备包含磷改性沸石的催化剂的方法和所述沸石的用途
公开(公告)号：US20140194662A1
公开(公告)日：2014-07-10
申请号：US14236750
申请日：2012-07-25
申请人： Nikolai Nesterenko , Delphine Minoux , Cindy Adam , Jean-Pierre Dath
发明人： Nikolai Nesterenko , Delphine Minoux , Cindy Adam , Jean-Pierre Dath
IPC分类号： B01J29/85 , C07C2/66 , C07C2/86 , C07C1/24 , C07C4/06
CPC分类号： B01J29/85 , B01J29/40 , B01J29/405 , B01J29/65 , B01J29/655 , B01J29/70 , B01J29/7023 , B01J29/7026 , B01J29/7038 , B01J29/7042 , B01J29/7046 , B01J29/7049 , B01J29/7088 , B01J29/7096 , B01J37/0009 , B01J37/0201 , B01J37/0209 , B01J37/10 , B01J37/28 , B01J2229/186 , B01J2229/36 , B01J2229/37 , B01J2229/42 , C07C1/20 , C07C1/22 , C07C1/24 , C07C2/08 , C07C2/66 , C07C2/864 , C07C4/06 , C07C2521/08 , C07C2527/14 , C07C2529/40 , C07C2529/65 , C10G3/49 , C10G29/205 , C10G29/22 , Y02P20/52 , Y02P30/42 , C07C11/04 , C07C11/06 , C07C11/08 , C07C15/46 , C07C15/08
摘要： A method to make a phosphorus modified zeolite can include providing a zeolite having at least one ten member ring, making an ion-exchange, steaming the zeolite, and introducing phosphorus on the zeolite. The zeolite can be mixed with one or more binders and shaping additives, and then shaped. A metal can be introduced, and the catalyst can be washed, calcined, and steamed in an equilibration step. The steaming can be at performed at a steam severity (X) of at least about 2. The steaming can be performed at a temperature above 625° C. The catalyst can be used in alcohol dehydration, olefin cracking, MTO processes, and alkylation of aromatics by alcohols with olefins and/or alcohols.
摘要翻译：制备磷改性沸石的方法可以包括提供具有至少一个十元环的沸石，进行离子交换，蒸煮沸石，并在沸石上引入磷。沸石可以与一种或多种粘合剂和成型添加剂混合，然后成型。可以引入金属，并且可以在平衡步骤中对催化剂进行洗涤，煅烧和蒸煮。蒸汽可以在至少约2的蒸汽苛刻度（X）下进行。蒸汽可以在高于625℃的温度下进行。催化剂可用于醇脱水，烯烃裂解，MTO方法和烷基化醇与烯烃和/或醇的芳族化合物。

7. 发明申请

US20140148630A1 PROCESS TO MAKE OLEFINS FROM ISOBUTANOL 有权
标题翻译：从ISOBUTANOL制造OLEFINS的过程
公开(公告)号：US20140148630A1
公开(公告)日：2014-05-29
申请号：US13813168
申请日：2011-07-08
申请人： Cindy Adam , Delphine Minoux , Nikolai Nesterenko , Sander Van Donk , Jean-Pierre Dath
发明人： Cindy Adam , Delphine Minoux , Nikolai Nesterenko , Sander Van Donk , Jean-Pierre Dath
IPC分类号： C07C1/22
CPC分类号： C07C1/24 , B01J29/40 , B01J2229/42 , C07C1/22 , C07C4/06 , C07C6/04 , C07C2529/40 , C08F10/02 , C10G3/42 , C10G3/44 , C10G3/49 , C10G2300/1014 , C10G2300/1022 , C10G2300/201 , C10G2300/4081 , C10G2400/20 , C10G2400/22 , C12P5/026 , C12P7/16 , Y02E50/10 , Y02P20/52 , Y02P30/20 , Y02P30/42 , C07C11/08 , C07C11/06
摘要： The present invention relates to a process for the conversion of an alcohol mixture (A) comprising about 20 w % to 100% isobutanol to make essentially propylene, comprising: a) introducing in a reactor (A) a stream comprising the mixture (A), optionally water, optionally an inert component, b) contacting said stream with a catalyst (A1) at a temperature above 450° C. in said reactor (A) at conditions effective to dehydrate at least a part of the isobutanol and other alcohols, if any, and make a cracking, c) recovering from said reactor (A) an effluent comprising: ethylene, propylene, water, optionally unconverted alcohols of the mixture (A), various hydrocarbons, and the optional inert component of step a), d) fractionating said effluent of step c) to produce at least an ethylene stream, a propylene stream, a fraction consisting essentially of hydrocarbons having 4 carbon atoms or more, water and the optional inert component of step a), optionally recycling ethylene in whole or in part at the inlet of the reactor (A), optionally recycling the fraction consisting essentially of hydrocarbons having 4 carbon atoms or more at the inlet of the reactor (A).
摘要翻译：本发明涉及一种将包含约20％至100％异丁醇的醇混合物（A）转化成基本上丙烯的方法，其包括：a）在反应器（A）中引入包含混合物（A）的料流，任选的水，任选的惰性组分，b）在有效使至少一部分异丁醇和其它醇脱水的条件下，使所述物流与催化剂（A1）在高于450℃的温度下在所述反应器（A）中接触， c）从所述反应器（A）回收包含乙烯，丙烯，水，任选未转化的混合物（A）的醇，各种烃和步骤a）的任选的惰性组分的流出物， d）将步骤c）的所述流出物分馏以产生至少一种乙烯流，丙烯流，基本上由具有4个碳原子或更多的烃组成的级分，水和步骤a）的任选的惰性组分，任选地将乙烯全部回收或在par 在反应器（A）的入口处，任选地在反应器（A）的入口处循环基本上由具有4个或更多个碳原子的烃组成的馏分。

8. 发明授权

US08535515B2 Hydrotreating and/or hydrocracking catalyst of hydrocarbons and preparation thereof 有权
标题翻译：烃的加氢处理和/或加氢裂化催化剂及其制备
公开(公告)号：US08535515B2
公开(公告)日：2013-09-17
申请号：US10567564
申请日：2004-08-04
申请人： Thierry Cholley , Jean-Pierre Dath
发明人： Thierry Cholley , Jean-Pierre Dath
IPC分类号： B01J23/882
CPC分类号： B01J31/0254 , B01J23/85 , B01J23/88 , B01J23/882 , B01J37/0203 , B01J37/0236 , B01J37/20 , C10G45/08 , C10G47/12 , C10G2300/70
摘要： The invention relates to a hydroconversion catalyst, which comprises a refractory oxide support, at least one metal selected from group VIII and at least one metal selected from group VIB and which is characterized in that it has at least one organic compound containing at least one oxime group of formula (I)>C═NOR1, in which R1 is selected among hydrogen and alkyl, allyl, aryl, alkylene or cycloaliphatic groups, and combinations thereof, these groups being able to be substituted by at least one electron donor group.
摘要翻译：本发明涉及一种加氢转化催化剂，其包含难熔氧化物载体，至少一种选自VIII族的金属和至少一种选自VIB族的金属，其特征在于其具有至少一种含有至少一个肟的有机化合物式（I）的基团C = NOR1，其中R 1选自氢和烷基，烯丙基，芳基，亚烷基或脂环族基团，及其组合，这些基团能够被至少一个电子给体基团取代。

9. 发明申请

US20130204058A1 COMBINED PROCESS TO MAKE OLEFINS FROM ISOBUTANOL 有权
公开(公告)号：US20130204058A1
公开(公告)日：2013-08-08
申请号：US13813107
申请日：2011-07-08
申请人： Cindy Adam , Delphine Minoux , Nikolai Nesterenko , Sander Van Donk , Jean-Pierre Dath
发明人： Cindy Adam , Delphine Minoux , Nikolai Nesterenko , Sander Van Donk , Jean-Pierre Dath
IPC分类号： C07C1/24 , C07C4/06
CPC分类号： C07C1/24 , B01J21/04 , B01J29/40 , B01J29/65 , C07C4/06 , C07C2521/04 , C07C2529/40 , C07C2529/65 , C07C2529/85 , C10G3/44 , C10G3/49 , C10G2300/1014 , C10G2300/201 , C10G2300/4081 , C10G2400/20 , C10G2400/22 , C12P5/026 , C12P7/16 , Y02E50/10 , Y02P20/52 , Y02P30/20 , Y02P30/42 , C07C11/08 , C07C11/06
摘要： The present invention relates to a process for the conversion of an alcohols mixture (A) comprising about 20 w % to 100% isobutanol to make essentially propylene, comprising: a) introducing in a reactor (A) (also called the first reaction zone or low temperature reaction zone) a stream comprising the mixture (A), optionally water, optionally an inert component, b) contacting said stream with a catalyst (A1) in said reactor (A) at conditions effective to dehydrate: at least a portion of the isobutanol to essentially butenes, at least a portion of other alcohols, if any, to essentially olefins other than butene having the same carbon number as the alcohol precursor, c) recovering from said reactor (A) an effluent comprising: butenes, optionally olefins other than butene, water, optionally unconverted alcohols of the mixture (A), various hydrocarbons, and the optional inert component of step a), d) fractionating said effluent of step c) to remove a portion or all the water, unconverted alcohols, optionally the inert component, and optionally the whole or a part of the various hydrocarbons to get a stream (D) comprising essentially olefins and optionally the inert component, e) introducing at least a part of said stream (D) in an OCP reactor (also called the second reaction zone or high temperature zone), f) contacting said stream comprising at least a part of (D), optionally in combination with a stream (D1) comprising olefins having 4 carbon atoms or more (C4+ olefins), in said OCP reactor with a catalyst which is selective towards light olefins in the effluent, to produce an effluent with an olefin content of lower molecular weight than that of the feedstock, g) fractionating said effluent of step f) to produce at least an ethylene stream, a propylene stream and a fraction consisting essentially of hydrocarbons having 4 carbon atoms or more, optionally recycling ethylene in whole or in part at the inlet of the OCP reactor of step f), or at the inlet of the reactor (A) or at the inlet of both the OCP reactor of step f) and the reactor (A), optionally recycling the fraction consisting essentially of hydrocarbons having 4 carbon atoms or more at the inlet of the OCP reactor.

10. 发明申请

US20110190561A1 Process for Making Crystalline Metallosilicates 审中-公开
标题翻译：制备结晶金属硅酸盐的方法
公开(公告)号：US20110190561A1
公开(公告)日：2011-08-04
申请号：US12994561
申请日：2009-02-24
申请人： Metin Bulut , Pierre Jacobs , Delphine Minoux , Nikolai Nesternko , Jean-Pierre Dath , Sander Van Donk
发明人： Metin Bulut , Pierre Jacobs , Delphine Minoux , Nikolai Nesternko , Jean-Pierre Dath , Sander Van Donk
IPC分类号： C07C1/20 , C01B39/00 , C01B39/02
CPC分类号： B01J29/40 , B01J2229/62 , C01B37/005 , C01B39/02 , C01B39/04 , C01B39/38 , C01B39/40 , C07C2/864 , C07C2529/70 , C10G29/205 , Y02P20/52 , C07C15/08
摘要： The present invention relates to a process for making a crystalline metallosilicate composition 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 crystallyze the desired metallosilicate, e) recovering the desired metallosilicate, wherein 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，其包含具有内部部分（芯部）和外部部分（外层或外壳）的微晶，使得：外部部分的Si /金属比例高于所述内部部分，所述微晶在结晶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）提供包含无机源的水性介质的硅和任选的模板剂，c）任选地提供包含任选的二氧化硅有机源的非水性液体培养基，d）在有效地使所需的金属硅酸盐水解的条件下，将培养基a），b）和任选的c））回收所需的金属硅酸盐，其中在混合物a）+ b）+ c）中，在结晶之前，Si org / Si无机物的比例<0.3，有利地<0.2，优选为0，摩尔浓度 tio OH- / SiO 2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，混合物a）+ b）+ c），在结晶之前，高于13，优选高于13.1，更优选高于13.2，还更优选高于13.3，最优选高于13.4。

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