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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, stable structure and high acid strength

Active Publication Date: 2011-03-30
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, analytical pure, SiO 2 Content 28% by weight) mixed with aluminum isopropoxide (produced by Beijing Donghuan United Chemical Plant, analytically pure), and ethyl silicate (with SiO 2 Meter) and aluminum isopropoxide (in Al 2 O 3 Calculate the molar ratio of SiO 2 :Al 2 O 3 =350, then under stirring the above mixture and hydrolyzing agent NH 4 F (Chengde Yinhe Optical Materials Co., Ltd., analytically pure), water (deionized water, the same below) according to the silicon source (with SiO 2 Meter): NH 4 F: water = 1.0:0.015:5.0 in a molar ratio, and aging for 12 hours at a temperature of -10°C to obtain a silica-alumina gel.

[0031] (2) The silica-alumina gel obtained in step (1) is dried at 60° C. for 24 hours, and then dried at a temperature of 110° C. for 24 hours, and ground into silica-alumina gel particles with 40-200 mesh.

[0032] (3) The silica-alumina particles obtained in step (2) (with SiO 2 Meter), template TEA...

Embodiment 2

[0034] (1) Methyl silicate (Beijing Chemical Reagent Company, analytical pure, SiO 2 The content of 28% by weight) and aluminum nitrate (Beijing Chemical Reagent Company, analytical pure) aqueous solution according to SiO 2 :Al 2 O 3 =550 mol ratio and mix, then add the hydrolysis agent ammonia (NH 3 ·H 2 O, Beijing Chemical Reagent Company, analytical grade), the dosage of each component is such that methyl silicate (with SiO 2 Meter): NH 3 ·H 2 O:water=1.0:0.045:8.0 (molar ratio), stirring, and then aging for 6 hours at a temperature of 20°C to obtain a silica-alumina gel.

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

[0036] (3) Combine the silica-alumina gel particles obtained in step (2) with TEAOH (Beijing Xingfu Fine Chemical Research Institute, analytically pure, content 20% by weight), HF (Chemical Reagent Company ...

Embodiment 3

[0038] (1) Ethyl silicate (Beijing Chemical Reagent Company, analytical pure, SiO 2 The content of 28% by weight), aluminum sulfate (Tianjin Dengfeng Chemical Reagent Factory) aqueous solution is fully mixed, wherein the amount of ethyl silicate and aluminum sulfate in the mixture is SiO 2 :Al 2 O 3 The molar ratio is 1050, and then add the hydrolyzing agent oxalic acid (Beijing Xingfu Fine Chemical Research Institute, analytically pure, concentration 40% by weight), stir evenly, in which ethyl silicate (with SiO 2 The molar ratio of oxalic acid: water is 1.0:0.050:10.5, and then the silica-alumina gel is obtained by aging for 6 hours at a temperature of 40°C.

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

[0040] (3) The silica-alumina gel particles obtained in step (2), TEAOH (Beijing Xingfu Institute of Fine Chemistry, an...

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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. Themethod 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 method for synthesizing beta zeolite. Background technique [0002] Beta zeolite is a high-silica zeolite with a cross-twelve-membered ring channel system. It has good thermal stability, hydrothermal stability, acidity and good hydrophobicity. Its silicon-to-aluminum ratio can be in the range of tens to full silicon. Modulation. After its modification, it is used to catalyze the hydrocarbon reaction and shows the characteristics of not easy to coke and long service life. It is used in hydrocracking, hydrorefining, hydrodewaxing, diesel pour point depressing, catalytic cracking, isomerization, alkyl It has excellent catalytic performance in chemical and transalkylation reactions. [0003] In 1967, the American Mobil Company used the classic hydrothermal crystallization method to synthesize β zeolite for the first time (Wadlinger R.L, Kerr G.T, Rosinski E.J., USP3,308,069). The synthesis method published by US 3308069 includes: wil...

Claims

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Application Information

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Patent Type & Authority Patents(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
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