Preparation method of EUO structural nano silica-alumina molecular sieves

A technology of molecular sieve and nano-silicon, which is applied in the field of preparation of silicon-aluminum molecular sieve, can solve the problems of crystal phase impurity, low yield, large particle size of EUO structure molecular sieve, etc., and achieve short synthesis time, good repeatability and excellent isomerism The effects of chemical activity and selectivity

Inactive Publication Date: 2013-05-29
CHINA PETROLEUM & CHEM CORP +1
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0013] The technical problem to be solved by the present invention is that the EUO structure molecular sieve synthesized in the prior art has large particle size, impure crystal phase and low yield, and provides a new preparation method of nano-EUO structure silicon-aluminum molecular sieve

Method used

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  • Preparation method of EUO structural nano silica-alumina molecular sieves
  • Preparation method of EUO structural nano silica-alumina molecular sieves
  • Preparation method of EUO structural nano silica-alumina molecular sieves

Examples

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Embodiment 1

[0037] Weighed 1.41g of sodium metaaluminate (chemically pure, with mass content of aluminum oxide ≥ 41%, mass content of sodium oxide ≥ 31%, the same below) and dissolved in 30 g of deionized water to obtain solution A. In addition, 50g of silica sol (ammonium type, produced by Foshan Lianjie Silicon Material Co., Ltd., with a mass content of silicon dioxide of 40%, the same below) was dissolved in 20g of deionized water to obtain solution B, and solution B was slowly added dropwise under stirring Add 6g of hexamethylammonium bromide to the solution A to react into a gel, add 6g of hexamethylammonium bromide after the dropwise addition, stir vigorously for a period of time, then use an appropriate amount of sodium hydroxide (analytically pure, >96%) to adjust the pH value of the gel to 12 to control the molar composition of the gel. Ratio: SiO 2 / Al 2 o 3 =60,H 2 O / Al 2 o 3 =730,OH - / Al 2 o 3 =4.5, R / Al 2 o 3 =2.99, Na 2 O / Al 2 o 3 = 3.77, then add 6g of hexamet...

Embodiment 2～6

[0039] Molecular sieves were prepared according to the method of Example 1, the difference being that the initial gel silica-alumina ratio was different, and the amounts of raw materials and crystallization conditions used in each example were listed in Table 1.

[0040] Table 1

[0041]

Embodiment 7

[0043] (1) Preparation of template precursor N1

[0044] 180g of dibromohexane, 90g of trimethylamine (40%) and 180g of deionized water were mixed at room temperature, and fully stirred to obtain template precursor N1.

[0045] (2) Synthetic molecular sieve

[0046] Stir and dissolve quantitative sodium aluminate (A.R, alumina mass content > 41%, sodium oxide mass content 31%) and mineralizer in a certain amount of deionized water to obtain acid solution A, mix silica sol with a certain amount of deionized water Evenly obtain lye B, add solution B dropwise to solution A at room temperature ~ 80°C under stirring, then add the calculated amount of template agent, stir well to obtain the initial gel mixture, and move the mixture into a stainless steel crystallization kettle React at 180°C for 48 hours, and the reaction product is cooled, filtered, washed, and dried to obtain EUO structure nano-silicon-aluminum molecular sieve raw powder.

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Abstract

The invention relates to a preparation method of EUO structural nano silica-alumina molecular sieves, and mainly solves problems of large particle size, low yield, and impure crystalline phase of EUO structural sial zeolites prepared by existing technology. The preparation method includes evenly mixing an aluminum source, an silicon source, a template R, seed crystals and water to obtain an initial gel mixture with a molar ratio of (1 - 150) Na2O: (15 - 300) SiO2: Al2O3: (1 - 20) R: (200 - 3500) H2O; adjusting the hydrogen by inorganic acid or inorganic base, placing the mixture in a reactor to crystallize for 12 hours to 7 days on a condition of 140-200 DEG C temperature, and recycling solid productions to prepare so as to obtain pure phase EUO structural nano silica-alumina molecular sieves. According to the technical scheme, the preparation method solves the problems effectively and can be used in industrial production of the EUO structural nano silica-alumina molecular sieves.

Description

technical field [0001] The invention relates to a preparation method of a silicon-aluminum molecular sieve, in particular to a preparation method of a nano-silicon-aluminum molecular sieve with an EUO structure. Background technique [0002] The EUO structure molecular sieve is a unique type of medium-porous high-silicon molecular sieve, which was first released by John L. Casci et al. in the European patent EP42226 in 1981. It has a one-dimensional microporous structure, and its skeleton is composed of silicon-oxygen and aluminum-oxygen tetrahedrons. The composed ten-membered ring channel has an elliptical opening with a diameter of 0.41nm×0.57nm. There is a cage structure on the side of the main channel of the molecular sieve, the depth of the cage is 0.81nm, and the diameter of the cage opening is 0.68nm×0.58nm. The grain size of the molecular sieve is about 1-3 μm, and the aggregated size of the grains is about 425-1000 μm. The catalyst with EUO type molecular sieve as...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/04
Inventor 姜向东郑均林孔德金钱斌
Owner CHINA PETROLEUM & CHEM CORP
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