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Method for synthesis of beta-zeolite

A synthesis method and beta zeolite technology, applied in the field of beta zeolite synthesis, can solve problems such as difficulty in obtaining a silicon-alumina ratio, and achieve the effects of low water consumption, fewer defects and stable structure

Active Publication Date: 2009-01-28
RES INST OF PETROLEUM PROCESSING SINOPEC
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0011] It is difficult to obtain nano-beta zeolite with a silicon-aluminum ratio of not less than 300 and a grain size of not more than 100nm in the existing methods for preparing zeolite beta

Method used

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  • Method for synthesis of beta-zeolite

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] (1) Ethyl silicate (Beijing Chemical Reagent Company, analytically pure, SiO 2 content 28% by weight) is mixed with aluminum isopropoxide (produced by Beijing Donghuan United Chemical Factory, analytically pure), wherein ethyl silicate (as SiO 2 In terms of) and aluminum isopropoxide (in terms of Al 2 o 3 The molar ratio of SiO 2 :Al 2 o 3=350, then mix the above mixture with hydrolyzing agent NH under stirring 4 F (Chengde Yinhe Optical Material Co., Ltd., analytically pure), water (deionized water, the same below) according to the silicon source (using SiO 2 Count): NH 4 F: water = 1.0:0.015:5.0 molar ratio mixed, aged at -10°C for 12 hours to obtain silica-alumina gel.

[0031] (2) Dry the silica-alumina gel obtained in step (1) at 60° C. for 24 hours, then dry at 110° C. for 24 hours, and grind it into 40-200 mesh silica-alumina gel particles.

[0032] (3) the silica-alumina colloid particle (with SiO2) gained in step (2) 2 meter), template agent TEAF (prod...

Embodiment 2

[0034] (1) Methyl silicate (Beijing Chemical Reagent Company, analytically pure, SiO 2 Content 28% by weight) and aluminum nitrate (Beijing Chemical Reagent Company, analytically pure) aqueous solution according to SiO 2 :Al 2 o 3 =550 molar ratio mixing, then add hydrolysis agent ammonia (NH 3 ·H 2 O, Beijing Chemical Reagent Company, analytically pure), the consumption of each component makes methyl silicate (as SiO 2 Count): NH 3 ·H 2 O: water = 1.0: 0.045: 8.0 (molar ratio), stirred, and then aged at 20° C. for 6 hours to obtain a silica-alumina gel.

[0035] (2) The silica-alumina gel obtained in step (1) was first dried at 60° C. for 24 hours, then dried at 110° C. for 24 hours, and ground into 40-200 mesh silica-alumina gel particles.

[0036] (3) The silica-alumina colloidal particle of step (2) gained is mixed with TEAOH (Beijing Xingfu Institute of Fine Chemistry, analytically pure, content 20% by weight), HF (Sinopharm Chemical Reagent Company, excellent grad...

Embodiment 3

[0038] (1) Ethyl silicate (Beijing Chemical Reagent Company, analytically pure, SiO 2 Content 28% by weight), the aqueous solution of aluminum sulfate (Tianjin Dengfeng Chemical Reagent Factory) is fully mixed, wherein the consumption of ethyl silicate and aluminum sulfate makes SiO in the mixture 2 : Al 2 o 3 The mol ratio is 1050, then add hydrolyzing agent oxalic acid (Beijing Xingfu Institute of Fine Chemistry, analytically pure, concentration 40% by weight), stir well, wherein ethyl silicate (as SiO 2 The molar ratio of : oxalic acid: water is 1.0:0.050:10.5, and then aged at 40° C. for 6 hours to obtain a silica-alumina gel.

[0039] (2) The silica-alumina gel obtained in step (1) was first dried at 80° C. for 24 hours, then dried at 120° C. for 24 hours, and ground into 40-200 mesh silica-alumina gel particles.

[0040] (3) the silica-alumina colloid particles obtained in step (2), TEAOH (Beijing Xingfu Institute of Fine Chemistry, analytically pure, content 20% by w...

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Abstract

A synthetic method of beta-zeolite comprises the step of mixing and crystallizing alumino silica gel particles, a tetraethylammonium ion template agent, fluoride and water for 1-5 days at the temperature of 100-190 DEG C. Amounts of components in the mixture are that: the mol ratio of TEA<+> to SiO2 is 0.05-0.5, the mol ratio of TEA<+> to F<-> is 1-2, and the mol ratio of H2O to SiO2 is 2-10. The method can be used for synthesizing nano beta-zeolite with the ratio of silicon to aluminium ratio being not less than 300.

Description

technical field [0001] The invention relates to a synthesis method of zeolite beta. Background technique [0002] Beta zeolite is a high-silica zeolite with crossed twelve-membered ring channel system. It has good thermal stability, hydrothermal stability, acidity and good hydrophobicity. Its silicon-aluminum ratio can range from tens to all-silicon modulation. After modification, it is not easy to coke and have a long service life when used to catalyze hydrocarbon reactions. It has excellent catalytic performance in oxidation and transalkylation reactions. [0003] In 1967, Mobil Corporation of the United States first synthesized zeolite beta by the classic hydrothermal crystallization method (Wadlinger R.L, Kerr G.T, Rosinski E.J., USP 3,308,069). The synthetic method announced by US 3308069 comprises: will contain Na 2 O, Al 2 o 3 , TEAOH, SiO 2 The mixture with water is made into a slurry, and the crystallization reaction is carried out in an autoclave at 75-200°C...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/04
Inventor 王志光吴佳宋家庆何鸣元
Owner RES INST OF PETROLEUM PROCESSING SINOPEC