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ZEOLITE ITQ-1CM Patents

Índice de la ficha

Updated at
24/07/2026
Numero publicacion
EP.0818417.A1
Fecha publicacion
14/01/1998
Numero solicitud
EP19960939937

En detalle

Resumen

PCT No. PCT/ES96/00218 Sec. 371 Date Oct. 7, 1997 Sec. 102(e) Date Oct. 7, 1997 PCT Filed Nov. 19, 1996 PCT Pub. No. WO97/19021 PCT Pub. Date May 29, 1997The present invention relates to a microporous crystalline material of zeolitic nature, called ITQ-1A, to the process for its preparation and its use in processes of separation and transformation of organic compounds. In the roasted and anhydrous stage, the chemical composition of the material corresponds to the empirical formula: x(M1/nXO2):yYO2:SiO2, wherein x has a value smaller than 0.02 and may equal 0: y has a value smaller than 0.04 and may equal 0: m is H+ or an inorganic cation with the charge +n: X is a chemical element with an oxidation status +3 (Al, Ga, B, Cr) and Y is a chemical element with an oxidation status +4 (Ti, Ge, V). When x=0 and y=0, the material may be described as a new polymorphe form of microporous silica. The material of this invention is characterized also by its X ray diffraction pattern. The process for the preparation of said zeolite is characterized by the use of one or a plurality of organic additives in a reaction mixture which is crystallized through heating.

Reivindicaciones

1. A microporous crystalline material of zeolitic nature with an X ray diffraction pattern which is substantially concordant with that established in Tables I (figure 1) and II (figure 2) for the material, such as is synthesized, and after roasting, respectively and with a chemical composition in roasted and anhydrous stage which may be represented by the following empirical formula x(M<1/n>XO<2>):YO<2>:SiO<2> wherein x has a value smaller than 0.02, and may equal zero; y has a value smaller than 0.04, and may likewise equal zero; M is H+ or an inorganic cation with charge +n; X is a chemical element with oxidation status of +3 (as, for example, Al, Ga, B, Cr) and Y is a chemical element with oxidation status +4 (as, for example, Ti, Ge, V). 2. A zeolite according to claim 1, the chemical composition of which, in roasted and anhydrous stage may be represented by the following empirical formula x(HXO<2>):yYO<2>:SiO<2> wherein X is a trivalent element (Al, B, Ga, Cr, ...), Y is a tetravalent element different from Si (Ti, Ge, V,...), x has a value smaller than 0.02, and may equal zero, y has a value smaller than 0.04, and may likewise equal zero, and where the H+ cation may be interchanged by other mono-, di- or trivalent, organic or inorganic cations. 3. A method for synthesizing the zeolite of the previous claims, in which a reaction mixture which contains a source of SiO<2>, hydroxide of a R+ organic cation, (preferably N, N, N trimethyl-1-adamantammonium or N, N, N-trimethyl-2-adamantammonium or a mixture of both), a source of one or various tetravalent elements and different to Si, a source of one or various trivalent X elements and water is subjected to heating with or without agitation at temperatures between 80 and 200°C, preferably between 130 and 180°C, until its crystalliztion is obtained, and in which the reaction mixture has a composition, in terms of oxide molar relations, comprised between the ranges. X<2>O<3>/SiO<2>=0-0,033 ROH/SiO<2>=0,1-0,5, preferably 0,2-0,4 YO<2>/SiO<2>=0-0,05 H<2>O/SiO<2>=4-100, preferably 5-50, more preferably 25-50 . 4. A method for the synthesizing of zeolite of the previous claims, in which a reaction mixture which contains a source of SiO<2>, hydroxide of an organic cation R+, (preferably N,N, N-trimethyl-1-adamantammonium or N, N, N -trimethyl-2-adamantammonium, or mixtures of both), a source of one or various trivalent elements X and water, is subjected to heating with or without agitation, at temperatures between 80 and 200°C, preferably between 130 and 180°C, until its crystallization is obtained, and in which the reaction mixture has a composition, in terms of the molar relations of oxides, comprised between the ranges X<2>O<3>/SiO<2>=0-0,03 ROH/SiO<2>=0,1-0,5, preferably 0,2 - 0,4 H<2>O/SiO<2>=4-100, preferably 5-50, more preferably 25-50. 5. A method for synthetizing the zeolite of the previous claims, in which a reaction mixture which contains a source of Si0<2>, hydroxide of an organic cation R+ (preferably N,N, N trimethyl-1-adamantammonium or N, N, N-trimethyl-2-adamantammonium, or a mixture of both), a source of one or various tetravalent elements Y different to Si, and water, are subjected to heating with or without agitation at temperatures between 80 and 200°C, preferably between 130 and 180°C, until its cristallization is obtained, and in which the reaction mixture has a composition, in terms of the molar relations of oxides, comprised between the ranges ROH/SiO<2>=0,1-0,5, preferably 0,2-0,4 YO<2>/SiO<2>=0-0,05 H<2>O/SiO<2>=4-100, preferably 5 - 50, more preferably 25 - 50. 6. A method of synthesis of a microporous crystalline material according to claims 3, 4 and 5, in which to the reaction mixture is added a primary or secondary RN amine (preferably hexamethylenimine, heptamethylenimine, homopiperazine, cyclopenthylamine, cyclohexylamine, cyclohepthylamine or a mixture of the same), in a relation RN/R+ comprised in the range 0-20, preferably 0-5, and in which the quaternary R+ ammonium cation (preferably N, N, N -1-trimethyladamantammonium or N, N, N-2-trimethyladamantammonium, or a mixture of both) may be added as hydroxide or as another salt (preferably Halide) or a mixture of both. 7. A method of synthesis of a microporous crystalline material according to claim 6 and preceding ones, in which said crystalline material has an x ray diffraction pattern which is substancially concordant with the one established in Tables I and II for the material, such as is synthesized and after roasting respectively, and with a chemical composition in roasted and anhydrous stage which may be represented by the following empirical formula: x(M<1/n>XO<2>)yYO<2>:SiO<2> wherein x has a value smaller than 0,1, and may equal Zero; y has a value smaller than 0.04, and may likewise equal Zero; M is H+ or an inorganic cation with the charge +n; X is a chemical element with oxidation status +3 (as, for example, AL, Ga, B, Cr) and Y is a chemical element with oxidation status +4 (as for example, Ti, Ge, V). 8. A method for synthesizing the zeolite of claims 1, 2 and 7 according to the procedure of claims 3, 4, 5, and 6 where a quantity of crystalline material (preferably with the characteristicas of the material of claims 1, 2 and 7) is added to the reaction mixture as promotor of the crystallization, said quantity being comprised within the range 0.01 to 15 % in weight as regards the total added silica, preferably 0.05 to 5% . 9. A method for synthesizing the zeolite of claims 1, 2 and 7 according to the procedure of claims 3, 4, 5, 6 and 8, where the reaction mixture is essentially free of alkaline cations, the only limitation to this condition being the possible contents in alkaline impurities of the used reactives. 10. A method for synthesizing the zeolite of claims 1, 2 and 7 according to the proc edure of claims 3, 4, 5, 6 and 8, where a source of a tetravalent elements is introduced which is different to Si or to a trivalent element in an intermediate stage during the heating of the reaction mixture. 11. Use of the microporous crystalline material of claims 1, 2 and 7 in separation processes of hydrocarbides and as catalyst in processes of cracking, hydrocracking, light hydrocracking, olefins isomerization (for example, butene isomerization to isobutene and pentene to isopentene) and in selective catalytic oxidation processes using organic or inorganic hydroperoxides (as, for example, aromatic hydroxilation, olefin epoxidation, alkane oxidation and alcohols, ketone amoximation, sulfide oxidation and organic sulfoxides).

Etiquetas

Inventores
Diaz Maria JoseCamblor Fernandez Miguel AngelCorell Martinez CatalinaCorma Canos AvelinoDiaz Cabanas M JoseCorell Martires CatalinaCorma Camos AvelinoDiaz Cabanas Maria JoseDiaz CabanasMaria JoseCamblor FernandezMiguel AngelCorell MartiresCatalinaCorma CanosAvelinoDiaz Cabanas Ma Jose
Solicitantes
Consejo Superior de Investigaciones CientíficasUniv Valencia PolitecnicaUniversitat Politècnica de ValènciaUniv Politecnica de Valencia VConsejo Superior de Investigaciones Cientificas, MadridUniversidad Politecnica de Valencia, ValenciaConsejo Superior de Br InvestiConsejo Superior deConsejo Superior De<Br>Investigaciones CientificasDiaz Cabanas Ma JoseCamblor Fernandez Miguel AngelCorell Martires CatalinaCorma Camos Avelino
Clasificacion ipc
B01J 29/ 035 A IB01J 29/ 04 A IB01J 29/ 70 A IC01B 37/ 00 A IC01B 37/ 02 A IC01B 39/ 48 A IC07C 4/ 06 A IC07C 5/ 27 A IC07C 7/ 13 A IC10G 11/ 05 A IC10G 45/ 64 A IC10G 47/ 16 A I
Clasificacion cpc
423/702423/705423/706423/707423/709423/718
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