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1. 发明申请

WO2009146954A1 PROCESS FOR MAKING CRYSTALLINE METALLOSILICATES 审中-公开
标题翻译：制备晶体金属硅酸盐的方法
公开(公告)号：WO2009146954A1
公开(公告)日：2009-12-10
申请号：PCT/EP2009/052169
申请日：2009-02-24
申请人： TOTAL PETROCHEMICALS RESEARCH FELUY , BULUT, Metin , JACOBS, Pierre , MINOUX, Delphine , NESTERENKO, Nikolai , DATH, Jean-Pierre , VAN DONK, Sander
发明人： BULUT, Metin , JACOBS, Pierre , MINOUX, Delphine , NESTERENKO, Nikolai , DATH, Jean-Pierre , VAN DONK, Sander
IPC分类号： B01J29/40 , C01B39/36 , C10G11/05 , C01B39/40
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 - /SiO 2 is at least 0.3, advantageously from 0.3 to 0.62, preferably from 0.31 to 0.61, more preferably from 0.32 to 0.61, very preferably from 0.33 to 0.6.
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，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无机物的比率为 - / 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。

2. 发明申请

WO2009146955A1 PROCESS FOR MAKING CRYSTALLINE METALLOSILICATES 审中-公开
标题翻译：制备晶体金属硅酸盐的方法
公开(公告)号：WO2009146955A1
公开(公告)日：2009-12-10
申请号：PCT/EP2009/052170
申请日：2009-02-24
申请人： TOTAL PETROCHEMICALS RESEARCH FELUY , BULUT, Metin , JACOBS, Pierre , MINOUX, Delphine , NESTERENKO, Nikolai , DATH, Jean-Pierre , VAN DONK, Sander
发明人： BULUT, Metin , JACOBS, Pierre , MINOUX, Delphine , NESTERENKO, Nikolai , DATH, Jean-Pierre , VAN DONK, Sander
IPC分类号： B01J29/40 , C01B39/36 , C10G11/05
CPC分类号： C01B37/005 , B01J29/40 , B01J29/42 , B01J29/48 , C01B39/02 , C01B39/38 , C01P2002/72
摘要： The present invention provides a method for preparing a metallosilicate of MFI type, wherein organic templates, seeding techniques, using low aliphatic alcohols miscible with water or homogeneous starting solutions are not required. The present invention relates to a process for making a crystalline metallosilicate with high Si/Metal ratio comprising: a) providing an aqueous medium comprising OH− anions and a metal source, b) providing an aqueous medium comprising an inorganic water insoluble source of silicon, 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 crystallize the desired metallosilicate, e) recovering the desired metallosilicate, wherein in the mixture a)+b)+c), before crystallization, the ratio Si org/Si inorganic is 2 is at least 0.3, advantageously from 0.3 to 0.62, preferably from 0.31 to 0.61, more preferably from 0.32 to 0.61, very preferably from 0.33 to 0.6 and there is essentially no template. In another embodiment steps e), f) and g) are inserted before recovering 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.
摘要翻译：本发明提供了一种制备MFI型金属硅酸盐的方法，其中不需要使用与水混合的低脂肪醇或均相起始溶液的有机模板，接种技术。本发明涉及一种制备具有高Si /金属比的结晶金属硅酸盐的方法，其包括：a）提供包含OH-阴离子和金属源的水性介质，b）提供包含无机水不溶性硅源的水性介质， c）任选地提供包含任选的二氧化硅有机源的非水液体培养基，d）在有效使结晶期望的金属硅酸盐的条件下混合培养基a），b）和任选的c），e）回收所需的金属硅酸盐，其中混合物a）+ b）+ c），在结晶之前，Si org / Si无机物的比率为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 0.33〜0.6，基本上没有模板。在另一个实施方案中，在回收期望的金属硅酸盐之前，插入步骤e），f）和g）步骤：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0.5至3，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。

3. 发明申请

WO2009146953A1 PROCESS FOR MAKING CRYSTALLINE METALLOSILICATES 审中-公开
标题翻译：制备晶体金属硅酸盐的方法
公开(公告)号：WO2009146953A1
公开(公告)日：2009-12-10
申请号：PCT/EP2009/052168
申请日：2009-02-24
申请人： TOTAL PETROCHEMICALS RESEARCH FELUY , BULUT, Metin , JACOBS, Pierre , MINOUX, Delphine , NESTERENKO, Nikolai , DATH, Jean-Pierre , VAN DONK, Sander
发明人： BULUT, Metin , JACOBS, Pierre , MINOUX, Delphine , NESTERENKO, Nikolai , DATH, Jean-Pierre , VAN DONK, Sander
IPC分类号： B01J29/40 , C01B39/40 , C10G11/05 , C01B39/36
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 - /SiO 2 is at least 0.3, advantageously from 0.3 to 0.62, preferably from 0.31 to 0.61, more preferably from 0.32 to 0.61, very preferably from 0.33 to 0.6 and the pH of the mixture a)+b)+c), before crystallization, is higher than 13, preferably higher than 13.1, more preferably higher than 13.2, still more preferably higher than 13.3 and most preferred higher than 13.4.
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无机物的比率为至少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，结晶前混合物a）+ b）+ c）的pH高于13，优选高于13.1，更优选高于超过13.2，还更优选高于13.3，最优选高于13.4。

4. 发明申请

WO2011113837A1 PROCESS TO MAKE PROPYLENE FROM ETHYLENE AND EITHER DIMETHYL ETHER, OR METHANOL AND DIMETHYL ETHER 审中-公开
标题翻译：从乙烯和二甲基醚，或甲醇和二甲醚制得丙烯的方法
公开(公告)号：WO2011113837A1
公开(公告)日：2011-09-22
申请号：PCT/EP2011/053906
申请日：2011-03-15
申请人： TOTAL PETROCHEMICALS RESEARCH FELUY , STRUELENS, Pieter , JACOBS, Pierre , NESTERENKO, Nikolai , MINOUX, Delphine , VAN DONK, Sander , DATH, Jean-Pierre
发明人： STRUELENS, Pieter , JACOBS, Pierre , NESTERENKO, Nikolai , MINOUX, Delphine , VAN DONK, Sander , DATH, Jean-Pierre
IPC分类号： C07C2/86 , C07C11/06
CPC分类号： C07C2/862 , C07C2/864 , C07C2/865 , C07C11/06
摘要： The present invention is a process to make propylene comprising : a)providing a reaction zone containing a catalyst; b) introducing a feedstock comprising ethylene, dimethyl ether or methanol and dimethyl ether comprising at least 1000 wppm of dimethyl ether, optionally steam into said reaction zone and into contact with said catalyst; c) operating said reaction zone at temperature and pressure conditions to produce an effluent comprising propylene, hydrocarbons, steam, optionally unconverted methanol and /or unconverted dimethyl ether and optionally unconverted ethylene; d) sending the effluent of step c) to a fractionation zone to recover propylene optionally methanol and /or dimethyl ether and optionally ethylene; e)optionally recycling at least a part of methanol and /or dimethyl ether and optionally recycling at least a part of ethylene to the reaction zone at step b); wherein the catalyst is an acid and the temperature at the inlet of the reaction zone is under 280°C and advantageously from 50 to 280°C.
摘要翻译：本发明是制备丙烯的方法，包括：a）提供含有催化剂的反应区; b）将包含至少1000wppm二甲醚的乙烯，二甲醚或甲醇和二甲醚的原料引入所述反应区并与所述催化剂接触; c）在温度和压力条件下操作所述反应区以产生包含丙烯，烃，蒸汽，任选未转化的甲醇和/或未转化的二甲醚和任选未转化的乙烯的流出物; d）将步骤c）的流出物送入分馏区以回收丙烯任选的甲醇和/或二甲醚和任选的乙烯; e）任选地在步骤b）将至少一部分甲醇和/或二甲醚再循环至反应区中任选地将至少一部分乙烯循环; 其中催化剂是酸，并且反应区入口处的温度低于280℃，有利地为50-280℃。

5. 发明申请

WO2009010407A1 PROCESS FOR THE SELECTIVE OXIDATION OF METHANE 审中-公开
标题翻译：甲烷选择性氧化方法
公开(公告)号：WO2009010407A1
公开(公告)日：2009-01-22
申请号：PCT/EP2008/058690
申请日：2008-07-04
申请人： TOTAL PETROCHEMICALS RESEARCH FELUY , DE WINNE, Hendrik , JACOBS, Pierre , SELS, Bert , VERMEIREN, Walter
发明人： DE WINNE, Hendrik , JACOBS, Pierre , SELS, Bert , VERMEIREN, Walter
IPC分类号： C07C29/50 , C07C31/04 , B01J19/00 , B01J19/24
CPC分类号： C07C29/50 , B01J19/0093 , B01J19/02 , B01J19/242 , B01J19/249 , B01J2219/00085 , B01J2219/00159 , B01J2219/00826 , B01J2219/00873 , B01J2219/024 , B01J2219/0281 , B01J2219/2461 , B01J2219/2487 , C07C31/04
摘要： The present invention is a process for converting methane to methanol, comprising: feeding methane and gaseous air or oxygen or gaseous air enriched with oxygen to a reactor under an elevated pressure; said reactor having an internal surface, made of silica or coated with silica, surrounding a zone in which said gases react; and reacting said gases in said reaction zone at an elevated temperature at conditions effective to produce methanol and /or valuable oxygenates. Advantageously the internal surface is made of quartz or coated with quartz Advantageously the internal surface, made of silica (advantageously quartz) or coated with silica (advantageously quartz), is treated with HF before the conversion of methane to methanol. Advantageously the reaction is carried out in the absence in said reaction zone of any added material which measurably affects the rate of the reaction or the yield of the product. Advantageously the reactor is operated under a pressure from 1 to 7.5 MPa. Advantageously the reactor is operated at a temperature from 300°C to 600°C. Advantageously the reactor is operated at a residence time from 0.1 to 100s. Advantageously the reactor is operated at a methane to oxygen molar ratio from 1 to 50. The present invention also relates to a reactor having an internal surface made of silica (advantageously quartz) or coated with silica (advantageously quartz)
摘要翻译：本发明是一种将甲烷转化成甲醇的方法，包括：在升高的压力下将甲烷和气态空气或富含氧气的氧气或气态空气送入反应器; 所述反应器具有由二氧化硅制成或涂覆有二氧化硅的内表面，所述内表面围绕所述气体反应的区域; 并在有效产生甲醇和/或有价值的含氧化合物的条件下，在升高的温度下使所述反应区中的所述气体反应。有利地，内表面由石英制成或用石英涂覆。有利的是，在将甲烷转化成甲醇之前，用HF处理由二氧化硅（有利的是石英）或用二氧化硅（有利的是石英）制成的内表面。有利地，反应在所述反应区中不存在可测量地影响反应速率或产物收率的任何添加物质。有利地，反应器在1至7.5MPa的压力下操作。有利地，反应器在300℃至600℃的温度下操作。有利地，反应器在0.1至100s的停留时间下运行。有利地，反应器以甲烷与氧的摩尔比为1至50进行操作。本发明还涉及具有由二氧化硅（有利地为石英）或用二氧化硅（有利地为石英）涂覆的内表面的反应器，

6. 发明公开

EP2300160A1 PROCESS FOR MAKING CRYSTALLINE METALLOSILICATES 有权
标题翻译：制造结晶金属硅酸盐的方法
公开(公告)号：EP2300160A1
公开(公告)日：2011-03-30
申请号：EP09757337.2
申请日：2009-02-24
申请人： Total Petrochemicals Research Feluy
发明人： BULUT, Metin , JACOBS, Pierre , MINOUX, Delphine , NESTERENKO, Nikolai , DATH, Jean-Pierre , VAN DONK, Sander
IPC分类号： B01J29/40 , C01B39/36 , C10G11/05 , C01B39/40
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 - /SiO
2 is at least 0.3, advantageously from 0.3 to 0.62, preferably from 0.31 to 0.61, more preferably from 0.32 to 0.61, very preferably from 0.33 to 0.6.
摘要翻译：本发明涉及一种制造结晶金属硅酸盐组合物的方法，该方法包括具有内部部分（芯部）和外部部分（外层或外壳）的微晶，使得：外部部分中Si /金属的比率高于在内部部分中，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）提供包含无机物硅源和任选的模板剂，c）任选地提供包含任选有机二氧化硅源的非水性液体介质，d）在有效部分结晶所需金属硅酸盐的条件下混合介质a），b）和任选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 g）使得到的步骤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，其中在步骤d）中在混合物a）+ b）+ c）中，在结晶之前，Si org / Si无机物的比率<0.3，有利地<0.2且优选0，OH- / SiO 2的摩尔比至少为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 到0.61，非常优选从0.33到0.6。

7. 发明公开

EP2300161A1 PROCESS FOR MAKING CRYSTALLINE METALLOSILICATES 审中-公开
标题翻译：用于生产结晶金属
公开(公告)号：EP2300161A1
公开(公告)日：2011-03-30
申请号：EP09757338.0
申请日：2009-02-24
申请人： Total Petrochemicals Research Feluy
发明人： BULUT, Metin , JACOBS, Pierre , MINOUX, Delphine , NESTERENKO, Nikolai , DATH, Jean-Pierre , VAN DONK, Sander
IPC分类号： B01J29/40 , C01B39/36 , C10G11/05
CPC分类号： C01B37/005 , B01J29/40 , B01J29/42 , B01J29/48 , C01B39/02 , C01B39/38 , C01P2002/72
摘要： The present invention provides a method for preparing a metallosilicate of MFI type, wherein organic templates, seeding techniques, using low aliphatic alcohols miscible with water or homogeneous starting solutions are not required. The present invention relates to a process for making a crystalline metallosilicate with high Si/Metal ratio comprising: a) providing an aqueous medium comprising OH− anions and a metal source, b) providing an aqueous medium comprising an inorganic water insoluble source of silicon, 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 crystallize the desired metallosilicate, e) recovering the desired metallosilicate, wherein in the mixture a)+b)+c), before crystallization, the ratio Si org/Si inorganic is 2 is at least 0.3, advantageously from 0.3 to 0.62, preferably from 0.31 to 0.61, more preferably from 0.32 to 0.61, very preferably from 0.33 to 0.6 and there is essentially no template. In another embodiment steps e), f) and g) are inserted before recovering 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.

8. 发明公开

EP2300159A1 PROCESS FOR MAKING CRYSTALLINE METALLOSILICATES 审中-公开
标题翻译：用于生产结晶金属
公开(公告)号：EP2300159A1
公开(公告)日：2011-03-30
申请号：EP09757336.4
申请日：2009-02-24
申请人： Total Petrochemicals Research Feluy
发明人： BULUT, Metin , JACOBS, Pierre , MINOUX, Delphine , NESTERENKO, Nikolai , DATH, Jean-Pierre , VAN DONK, Sander
IPC分类号： B01J29/40 , C01B39/40 , C10G11/05 , C01B39/36
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 - /SiO
2 is at least 0.3, advantageously from 0.3 to 0.62, preferably from 0.31 to 0.61, more preferably from 0.32 to 0.61, very preferably from 0.33 to 0.6 and the pH of the mixture a)+b)+c), before crystallization, is higher than 13, preferably higher than 13.1, more preferably higher than 13.2, still more preferably higher than 13.3 and most preferred higher than 13.4.

9. 发明公开

EP2170792A1 PROCESS FOR THE SELECTIVE OXIDATION OF METHANE 有权
标题翻译：过程甲烷选择性氧化
公开(公告)号：EP2170792A1
公开(公告)日：2010-04-07
申请号：EP08785929.4
申请日：2008-07-04
申请人： Total Petrochemicals Research Feluy
发明人： DE WINNE, Hendrik , JACOBS, Pierre , SELS, Bert , VERMEIREN, Walter
IPC分类号： C07C29/50 , C07C31/04 , B01J19/00 , B01J19/24
CPC分类号： C07C29/50 , B01J19/0093 , B01J19/02 , B01J19/242 , B01J19/249 , B01J2219/00085 , B01J2219/00159 , B01J2219/00826 , B01J2219/00873 , B01J2219/024 , B01J2219/0281 , B01J2219/2461 , B01J2219/2487 , C07C31/04
摘要： The present invention is a process for converting methane to methanol, comprising: feeding methane and gaseous air or oxygen or gaseous air enriched with oxygen to a reactor under an elevated pressure; said reactor having an internal surface, made of silica or coated with silica, surrounding a zone in which said gases react; and reacting said gases in said reaction zone at an elevated temperature at conditions effective to produce methanol and /or valuable oxygenates. Advantageously the internal surface is made of quartz or coated with quartz Advantageously the internal surface, made of silica (advantageously quartz) or coated with silica (advantageously quartz), is treated with HF before the conversion of methane to methanol. Advantageously the reaction is carried out in the absence in said reaction zone of any added material which measurably affects the rate of the reaction or the yield of the product. Advantageously the reactor is operated under a pressure from 1 to 7.5 MPa. Advantageously the reactor is operated at a temperature from 300°C to 600°C. Advantageously the reactor is operated at a residence time from 0.1 to 100s. Advantageously the reactor is operated at a methane to oxygen molar ratio from 1 to 50. The present invention also relates to a reactor having an internal surface made of silica (advantageously quartz) or coated with silica (advantageously quartz)

10. 发明公开

EP2130586A1 Process for making crystalline metallosilicates 审中-公开
标题翻译：制造结晶金属硅酸盐的方法
公开(公告)号：EP2130586A1
公开(公告)日：2009-12-09
申请号：EP08157770.2
申请日：2008-06-06
申请人： Total Petrochemicals Research Feluy
发明人： BULUT, Metin , JACOBS, Pierre , MINOUX, Delphine , NESTERENKO, Nikolai , DATH, Jean-Pierre , VAN DONK, Sander
IPC分类号： B01J29/40 , C01B39/36 , C10G11/05
CPC分类号： B01J29/40 , C01B39/38 , C10G11/05 , C10G29/205 , C10G47/04 , C10G50/00 , C10G50/02
摘要： The present invention provides a method for preparing a metallosilicate of MFI type, wherein organic templates, seeding techniques, using low aliphatic alcohols miscible with water or homogeneous starting solutions are not required.
The present invention relates to a process for making a crystalline metallosilicate with high Si/Metal ratio comprising:
a) providing an aqueous medium comprising OH - anions and a metal source,
b) providing an aqueous medium comprising an inorganic water insoluble source of silicon,
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 crystallize the desired metallosilicate,
e) recovering the desired metallosilicate,

wherein in the mixture a)+b)+c), before crystallization,
the ratio Si org/Si inorganic is
the molar ratio OH - /SiO 2 is at least 0.3, preferably from 0.3 to 0.6 more preferably from 0.33 to 0.6 .
In another embodiment steps e), f) and g) are inserted before recovering 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.
摘要翻译：本发明提供了制备MFI型金属硅酸盐的方法，其中不需要使用可与水混溶的低级脂族醇或均相起始溶液的有机模板，接种技术。本发明涉及制备具有高Si /金属比率的结晶金属硅酸盐的方法，其包括：a）提供包含OH-阴离子和金属源的水性介质，b）提供包含无机水不溶性硅源的水性介质， c）任选地提供包含任选有机二氧化硅源的非水性液体介质，d）在有效使所需金属硅酸盐结晶的条件下混合介质a），b）和任选c），e）回收所需金属硅酸盐，其中在在结晶之前，混合物a）+ b）+ c）的比例Si org / Si无机物<0.3，有利地<0.2且优选0，OH- / SiO 2的摩尔比至少为0.3，优选为0.3至0.6以上优选从0.33至0.6。在另一个实施方案中，在回收所需的金属硅酸盐之前插入步骤e），f）和g）：e）将反应混合物a）+ b）+ c）冷却至室温，f）通过以下方式降低反应混合物的pH： g）至少0.1，优选0.3至4，更优选0.5至3，g）使得到的步骤f）的混合物在有效继续期望的金属硅酸盐结晶的条件下进行。

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