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Preparation method of nanometer hierarchical porous zsm-11/zsm-5 eutectic zeolite

The technology of ZSM-11 and ZSM-5 is applied in the field of preparation of nano-hierarchical porous ZSM-11/ZSM-5 eutectic zeolite, which can solve the problems of short single-pass service cycle and easy deactivation of catalysts, and achieve good technical results Effect

Active Publication Date: 2015-11-18
CHINA PETROLEUM & CHEM CORP +1
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The technical problem to be solved by the present invention is that there are problems in the prior art that the catalyst is easily deactivated and the one-way service life is short, and a new preparation method of nanometer hierarchical porous ZSM-11 / ZSM-5 eutectic zeolite is provided

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  • Preparation method of nanometer hierarchical porous zsm-11/zsm-5 eutectic zeolite

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Embodiment 1

[0020] The preparation method of nanometer hierarchical porous ZSM-11 / ZSM-5 eutectic zeolite comprises the following steps:

[0021] a) step, the raw material mixture is SiO on a molar basis 2 / Al 2 o 3 =100, Na 2 O / SiO 2 =0.14,H 2 O / SiO 2 =40, organic ammonium / SiO 2 =0.15, organic polymer / SiO 2 =0.0002, the organic ammonium is tetrabutylammonium bromide, the alkali source is sodium hydroxide, the silicon source is silica sol, the aluminum source is sodium metaaluminate, and the organic polymer is polyethylene glycol alcohol.

[0022] In step b), the hydrothermal crystallization temperature is 145° C., and the crystallization time is 168 hours. The product is washed with distilled water until neutral, centrifuged, dried and then roasted in air at 550°C. The product XRD spectrum shows that the product is a ZSM-11 / ZSM-5 eutectic zeolite, and the baseline is straight, indicating that it does not contain amorphous substances substantially, see figure 1 . The SEM photo ...

Embodiment 2

[0028] The preparation and evaluation of the catalyst were the same as in Example 1, except that the crystallization time was 192 hours when the catalyst was prepared, and the XRD diffraction peak intensity of the product increased slightly after 192 hours of crystallization, indicating that the crystallinity increased. The SEM photo of the product shows the particle size of the nano-hierarchical ZSM-11 / ZSM-5 eutectic zeolite, the pore structure parameters and the mass percentage of ZSM-11 in the nano-hierarchical ZSM-11 / ZSM-5 eutectic zeolite. Table 1. The evaluation results after 168 hours of continuous reaction are shown in Table 2.

Embodiment 3

[0030] The preparation and evaluation of the catalyst were the same as in Example 1, except that the crystallization time was 216 hours, and the XRD pattern of the product after crystallization for 216 hours had no obvious change compared with that in Example 2. The SEM photo of the product shows the particle size of the nano-hierarchical ZSM-11 / ZSM-5 eutectic zeolite, the pore structure parameters and the mass percentage of ZSM-11 in the nano-hierarchical ZSM-11 / ZSM-5 eutectic zeolite. Table 1. The evaluation results after 168 hours of continuous reaction are shown in Table 2.

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Abstract

The invention relates to a preparation method of hierarchical-pore nano ZSM-11 / ZSM-5 eutectic zeolite, which mainly solves the problems of small pore size and large crystal grain particle size of the ZSM-11 / ZSM-5 eutectic zeolite obtained in the prior art. The method comprises the following steps: preparing an aluminum source, a silicon source, organic ammonium, organic high polymer, alkali and deionized water into a raw material mixture, and carrying out hydrothermal crystallization on the raw material mixture at 60-200 DEG C for 24-480 hours to obtain the nano hierarchical-pore ZSM-11 / ZSM-5 eutectic zeolite. The raw material mixture is composed of organic ammonium, Na2O, SiO2, Al2O3, organic high polymer and H2O in a mol ratio of (0.03-0.3):(0.05-0.2):1:(0.005-0.025):(0.0001-0.1):(8-50). The technical scheme provided by the invention well solves the problems, and can be used for industrial preparation of nano hierarchical-pore ZSM-11 / ZSM-5 eutectic zeolite.

Description

technical field [0001] The invention relates to a preparation method of nanometer hierarchical hole ZSM-11 / ZSM-5 eutectic zeolite. Background technique [0002] ZSM-11 zeolite is a member of the high-silicon ZSM series, which was first synthesized by the Mobil Company of the United States in the early 1970s [US3709979]. Both ZSM-11 and ZSM-5 are Pentasil zeolites. The silicon-oxygen tetrahedrons in the Pentasil molecular sieve framework are connected to form a special structural unit, which consists of 8 five-membered rings. Into pieces. The sheet structure adopts different connection methods (symmetry center correlation and mirror correlation), and two structural configurations of MFI and MEL can be obtained respectively. Both ZSM-11 (MEL) and ZSM-5 (MFI) are two-dimensional channel systems, but the channel structures of the two are different. ZSM-11 is formed by the intersection of two-dimensional straight channels (0.51×0.55nm) of elliptical ten-membered rings. . ZSM-...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B39/36
Inventor 刘师前李亚男金照生顾龙勤
Owner CHINA PETROLEUM & CHEM CORP
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