Synthesis method for nanometer Beta zeolite

A technology of beta zeolite and synthesis method, which is applied in the direction of crystalline aluminosilicate zeolite, etc., can solve the problems of low yield of nano-scale zeolite, large crystal grains of Beta zeolite, etc., to avoid loss, improve reactivity and stability, The effect of good technical effects

Active Publication Date: 2012-05-23
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The technical problem to be solved by the present invention is that the crystal grains of Beta zeolite synthesized in the prior art are large, and the recovery of nano-scale zeolite by conventional filtration or centrifugal separation method is low. A new synthesis method of nano-Beta zeolite is provided

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0013] 600g 40% silica sol, 38.9g sodium aluminate (alumina content 42%), 70.6g 25% tetraethylammonium hydroxide (TEAOH), 5.0g diethylamine (DEA), 168.0g tetraethyl bromide Ammonium (TEABr), 16.0 g of sodium hydroxide, 136.0 g of 25% ammonium hydroxide, and 925.1 g of water were mixed and stirred evenly at room temperature. Then, transfer to a stainless steel autoclave, the crystallization temperature is 140° C., and react for 72 hours. After the reaction, add oxalic acid and adjust the pH value to less than 11. Filter through a filter cloth, wash the crystalline product with deionized water, and dry. Among them, SiO in molar ratio in the reaction mixture 2 / Al 2 o 3 =25, TEAOH / SiO 2 =0.03, DEA / SiO 2 =0.03, TEABr / SiO 2 =0.2, NaOH / SiO 2 =0.1, NH 4 OH / SiO 2 =0.5,H 2 O / SiO 2 = 20, R1 / R2 = 0.3.

[0014] The crystalline product obtained by XRD powder diffraction analysis of the product is Beta zeolite, and the recovery rate of the product is 100% based on silicon oxide...

Embodiment 2

[0016] Synthetic method is the same as [Example 1], but SiO is calculated in molar ratio in the reaction mixture 2 / Al 2 o 3 =15, TEAOH / SiO 2 =0.05, TEABr / SiO 2 =0.20, NaOH / SiO 2 =0.02, NH 4 OH / SiO 2 =0.8,H 2 O / SiO 2 =12, R1 / R2==0.25. The crystallization temperature was 150°C, and the reaction was 55 hours. After the reaction, firstly add hydrochloric acid to adjust the pH value to 11, and then use ethylenediaminetetraacetic acid to adjust the pH value to less than 9.

[0017] The crystalline product obtained by XRD powder diffraction analysis of the product is Beta zeolite, and the recovery rate of the product is 99% based on silicon oxide, and the crystal grain size is 10-40nm according to transmission electron microscope TEM analysis.

Embodiment 3

[0019] Synthetic method is the same as [Example 1], just replace diethylamine (DEA) with triethylamine (TrEA), and SiO is counted in molar ratio in the reaction mixture 2 / Al 2 o 3 =40, TEAOH / SiO 2 =0.02, TrEA / SiO 2 = 0.1, TEABr / SiO 2 =0.20, NaOH / SiO 2 =0.00, NH 4 OH / SiO 2 = 1.0, H 2 O / SiO 2 = 15, R1 / R2 = 0.6. The crystallization temperature was 155°C, and the reaction was 45 hours. After the reaction, first add phosphoric acid to adjust the pH value to 11, and then use citric acid to adjust the pH value to less than 9.

[0020] The crystalline product obtained by XRD powder diffraction analysis of the product is Beta zeolite, and the recovery rate of the product is 99% based on silicon oxide, and the crystal grain size is 10-40nm according to transmission electron microscope TEM analysis.

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Abstract

The invention relates to a synthesis method for nanometer Beta zeolite, which mainly solves the problems in the prior art that the synthesized Beta zeolite has big crystal particle, and the efficiency is low when the nanometer zeolite is recovered with a common filtering or centrifugal separation method. The synthesis method for the nanometer Beta zeolite comprises the following steps: a) mixing a silicon source, an aluminum source, alkali MOH and compound template agent RN with water, wherein reaction mixture is calculated at the following molar ratio: SiO2 / Al2O3 is equal to 5-100, MOH / SiO2 is equal to 0.1-2.0, H2O / SiO2 is equal to 5-80, RN / SiO2 is equal to 0.01-1.0; crystallizing the mixture at the temperature of 110-200DEG C for 5-100hours to obtain crystallization liquid, wherein the compound template agent RN is the mixture of R1 and R2, R1 is selected from at least one of tetraethylammonium hydroxide and triethylamine or diethylamine, R2 is selected from tetraethyl ammonium halide, and the molar ratio of R1 to R2 is 0.05-2.0; and b) adding acid compound into the crystallization liquid, regulating the pH value of the crystallization liquid to be less than 11, and separating, washing and drying to obtain the nanometer Beta zeolite, wherein the acid compound is selected from at least one of inorganic acid, organic acid or ammonium chloride. According to the technical scheme, the problem is better solved. The synthesis method for the nanometer Beta zeolite can be used for the industrial production of the Beta zeolite.

Description

technical field [0001] The invention relates to a synthesis method of nano Beta zeolite. Background technique [0002] Nano Beta zeolite can be used as catalyst. As early as 1967, US Patent No. 3,308,069 introduced the synthesis of conventional Beta zeolite using tetraethylammonium hydroxide as a template. The crystal grain of Beta zeolite synthesized by this method is larger than 1 micron; in addition, because tetraethylammonium hydroxide is completely used as template agent, the cost is relatively high. U.S. Patent No. 5,672,799 describes a synthesis method of Beta zeolite for the alkylation of propylene and benzene, which is modified by introducing metal ions. Microporous and Mesoporous Materials, 2003, Vol 6, P21 introduced the synthesis method of Beta zeolite with mesoporous features. Acta Catalytica Sinica (2000, Vol21 No1, P75) introduced a method for synthesizing Beta zeolite in a F-containing system, but the crystal grains of the synthesized Beta zeolite are also...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/04
Inventor 高焕新周斌魏一伦顾瑞芳方华季树芳姚晖
Owner CHINA PETROLEUM & CHEM CORP
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