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Preparation method of microcrystal mordenites

A mordenite and small-grain technology, which is applied in the field of synthesis of small-grain mordenite, can solve the problems of large amount of template agent, high production cost, high sodium content, etc., and achieve high activity and isomerization selectivity, wide silicon Effect of Al Ratio Variation Range

Active Publication Date: 2009-09-02
CHINA PETROLEUM & CHEM CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

T.Sano et al. (Microporous and Mesoporous Materials 95 (2006) 141-145) reported that using silica gel as a silicon source, AlCl 3 As the aluminum source, tetraethylammonium hydroxide (TEAOH) was used as the template, and the SiO 2 / Al 2 o 3 =20~40 high silica mordenite, but TEAOH / SiO 2 0.23, the amount of template agent is large, the production cost is high, the grain size of synthetic zeolite is large, and the grain range is 2.5-14.3 μm
T.Sano et al. (J.Mater.Chem., 2003, 13, 1173-1179) reported that SiO was prepared by adding NaF as a mineralizer in the crystallization system 2 / Al 2 o 3 The method for the high-silica mordenite of 50, the particle size of the obtained mordenite is 10 μm, but the F- of the zeolite bulk phase is not easy to remove, which seriously affects the thermal stability of the zeolite
K.Itabashi etc. reported the synthesis and characteristics of silicon-containing mordenite in Zeolites, 1986, Vol 6, January, 30-34, using benzyltrimethylamine as template agent, amorphous silica, aluminate Sodium solution and sodium hydroxide are used as raw materials, stirred and crystallized at 150-200°C for 20-72 hours, and mordenite with a silicon-aluminum ratio of 10.2-19.1 can be directly synthesized, but the sodium content in the synthesis system is still high

Method used

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  • Preparation method of microcrystal mordenites
  • Preparation method of microcrystal mordenites
  • Preparation method of microcrystal mordenites

Examples

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example 1

[0030] Add sodium metaaluminate solution containing 139.5 g / L of sodium oxide, 100.0 g / L of aluminum oxide, and tetraethylammonium hydroxide solution with a concentration of 2.03 mol / L (produced by Daxing Xingfu Fine Chemical Research Institute) into deionized water , stir evenly to make a mixed solution, add coarse-porous silica gel (7.8% by mass on ignition, produced by Qingdao Ocean Chemical Factory) with a particle size of 150 to 225 μm into the above mixed solution, so that the surface of the silica gel is wetted by the mixed solution to obtain a reaction The mixture, wherein the molar ratio of each raw material is shown in Table 1, and then the reaction mixture was aged in an autoclave at 60°C for 24 hours, crystallized at 120°C for 24 hours, crystallized at 148°C for 48 hours, and cooled to 25°C The solid product was isolated, washed with deionized water and dried at 80° C. for 12 hours to obtain the mordenite of the present invention. Its XRD was as follows: figure 1 A...

example 2

[0032] Add the sodium metaaluminate solution and tetraethylammonium hydroxide solution used in Example 1 into deionized water, stir evenly to make a mixed solution, and then add coarse-pored silica gel to the above mixed solution, so that the surface of the silica gel is wetted by the mixed solution , to obtain the reaction mixture, the mol ratio of each raw material is shown in Table 1. Transfer the reaction mixture to a high-pressure reactor for crystallization, crystallize at 70°C for 24 hours, crystallize at 135°C for 24 hours, separate the solid after cooling, wash with deionized water and dry at 80°C for 12 hours to obtain mordenite. Its properties are shown in Table 1.

example 3

[0034] Add the sodium metaaluminate solution and tetraethylammonium hydroxide solution used in Example 1 into deionized water, stir evenly to make a mixed solution, and then add coarse-pored silica gel to the above mixed solution, so that the surface of the silica gel is wetted by the mixed solution , to obtain the reaction mixture, the mol ratio of each raw material is shown in Table 1. Transfer the reaction mixture into a high-pressure reactor, add mordenite with a silicon-aluminum ratio of 20, accounting for 5% of the total mass of the mixture on a dry basis, as a seed crystal, carry out two-stage crystallization at 120°C and 140°C, and separate the solid after cooling , the mordenite prepared by washing with deionized water and drying at 80°C for 12 hours, its properties are shown in Table 1, and the TEM photos are shown in Figure 4 . Figure 4 It shows that the mordenite synthesized by adding seeds is spherical.

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Abstract

The invention discloses a preparation method of microcrystal mordenites, which comprises the following steps of: blending an aluminum resource, a sodium resource, a template agent and water to obtain a mixed solution; applying the mixed solution to moisten the surface of silica gel so as to form a synthetic system with the mole ratio as follows: the mole ratio of SiO2 to A12O3 is 10 to 100, the mole ratio of template agent to SiO2 is 0.01 to 0.10, the mole ratio of Na2O to SiO2 is 0.01 to 0.10 and the mole ratio of H2O to SiO2 is 4.0 to 8.0; and conducting two-segment crystallization over the synthetic system at different temperatures and then collecting, washing and drying the solid substances. The mordenites synthesized by the method has small grain and high silica alumina ratio, and has rather high isomerized selectivity when being applied to the isomerization reaction of C5 / C6 light hydrocarbon.

Description

technical field [0001] The invention is a method for synthesizing silica-alumina zeolite, in particular, a method for synthesizing small-grain mordenite. Background technique [0002] Mordenite is a molecular sieve with a high silica-to-alumina ratio, that is, a high molar ratio of silica / alumina. It has a large number of five-membered rings, which are interrelated in pairs. Ellipse, the size is 0.65nm×0.68nm. Mordenite is widely used as a catalyst in chemical and petrochemical industries and as an adsorbent for separating gas or liquid mixtures. [0003] Mordenite, no matter it is natural mordenite or artificially synthesized mordenite, its silicon-alumina ratio is generally 10-12, and its catalytic activity is low. Usually, multiple ammonium exchanges and acid exchanges are required to convert mordenite into one with higher silicon-aluminum ratio. Only hydrogen-type mordenite can be used for catalytically active components. In each exchange process, steps such as washin...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/26
Inventor 贾晓梅王永睿慕旭宏舒兴田
Owner CHINA PETROLEUM & CHEM CORP
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